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Pressure-Sensitive Conducting and Antibacterial Materials Obtained by in Situ Dispersion Coating of Macroporous Melamine Sponges with Polypyrrole

  • Jaroslav Stejskal*
    Jaroslav Stejskal
    Institute of Macromolecular Chemistry, Academy of Sciences of the Czech Republic, 162 06 Prague 6, Czech Republic
    *Email: [email protected]
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    Orcidhttps://orcid.org/0000-0001-9350-9647
  • , 
  • Miroslava Trchová
    Miroslava Trchová
    University of Chemistry and Technology, Prague, 166 28 Prague 6, Czech Republic
    More by Miroslava Trchová
    Orcidhttps://orcid.org/0000-0001-6105-7578
  • , 
  • Hayk Kasparyan
    Hayk Kasparyan
    University of Chemistry and Technology, Prague, 166 28 Prague 6, Czech Republic
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  • , 
  • Dušan Kopecký
    Dušan Kopecký
    University of Chemistry and Technology, Prague, 166 28 Prague 6, Czech Republic
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  • , 
  • Zdeňka Kolská
    Zdeňka Kolská
    Faculty of Science, J.E. Purkyně University, 400 96 Ústí nad Labem, Czech Republic
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  • , 
  • Jan Prokeš
    Jan Prokeš
    Faculty of Mathematics and Physics, Charles University, 180 00 Prague 8, Czech Republic
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  • Ivo Křivka
    Ivo Křivka
    Faculty of Mathematics and Physics, Charles University, 180 00 Prague 8, Czech Republic
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  • Jan Vajďák
    Jan Vajďák
    Centre of Polymer Systems, Tomas Bata University in Zlín, 760 01 Zlín, Czech Republic
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  • , and 
  • Petr Humpolíček
    Petr Humpolíček
    Centre of Polymer Systems, Tomas Bata University in Zlín, 760 01 Zlín, Czech Republic
    More by Petr Humpolíček
    Orcidhttps://orcid.org/0000-0002-6837-6878
Cite this: ACS Omega 2021, 6, 32, 20895–20901
Publication Date (Web):August 6, 2021
https://doi.org/10.1021/acsomega.1c02330

Copyright © 2021 The Authors. Published by American Chemical Society. This publication is licensed under

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Abstract

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Melamine sponges were coated with polypyrrole during the in situ polymerization of pyrrole. The precipitation polymerization was compared with the dispersion mode, that is, with the preparation in the presence of poly(N-vinylpyrrolidone) and nanosilica as colloidal stabilizers. The coating of sponges during the dispersion polymerization leads to the elimination of the undesired polypyrrole precipitate, improved conductivity, and increased specific surface area. The sponges were tested with respect to their conductivity and as pressure-sensitive conducting materials with antibacterial performance.

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1. Introduction

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Conducting polymers, (1,2) such as polypyrrole, (3) are currently prepared by the oxidation of respective monomers in aqueous medium, iron(III) chloride being an oxidant of choice in the oxidation of pyrrole. (4,5) The oxidation takes place in aqueous medium, and any object in contact with the reaction mixture becomes coated with a thin polymer film. This is so-called surface polymerization. (6) After the interface is coated and reactants are still present in the reaction mixture, the precipitation polymerization continues in the aqueous medium and macroscopic polymer aggregates are produced and isolated as a powder.
The conducting polymers alone are intractable. For this reason, their deposition on suitable materials is a solution for most applications. Polymer sponges are attractive substrates for the coating with conducting polymers due to their low weight, open-cell macroporosity, high specific surface area, chemical stability, and elasticity. This makes them good candidates for sorbents applicable in biomedicine, (7) analytical chemistry, (8) solar steam generation, (9) energy storage, (10) and especially in environmental issues, such as water-pollution treatment. (11−14) Melamine/formaldehyde sponges are commercially available, and they are used as flame-retardant sound-proofing and thermal insulation or as abrasive cleaners. The coating with polypyrrole endows them with additional properties, such as the conductivity, (15) electroactivity, and ability to sense humidity (16) or to adsorb organic dyes (12,13) and various pollutants, including oil spills (17) and heavy-metal ions. (18) The conducting and electroactive coating enables to control the properties by applying or recording an electric potential, for example, in stimulation or monitoring of biological objects, (2,19) the heating of sponges by passing electric current being another example. (17)
When applied to the coating of macroporous melamine sponges by surface polymerization of pyrrole, (15) the precipitated polymer produced at the same time remains entrapped in the macroporous template. The precipitate cannot be removed even by excessive washing. For various applications, this may be inconvenient because the polymer leaves the sponge during the processing, for example, cutting or squeezing of the sponge, and contaminates the surrounding space (Figure 1a). The presence of a fine polypyrrole precipitate can be eliminated by the addition of a water-soluble polymer stabilizer, for example, poly(N-vinylpyrrolidone) (PVP) (Figure 1b), or nanocolloidal silica. Its presence converts a macroscopic polypyrrole precipitate to a colloidal dispersion that is easily washed out from the sponge. This approach, the coating of sponges in the course of dispersion polymerization of pyrrole, is demonstrated in the present report.

Figure 1

Figure 1. Melamine sponges after being compressed with hand and released: (a) polypyrrole coating and (b) reduced polypyrrole content deposited in the presence of PVP.

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2. Results and Discussion

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2.1. Polypyrrole Coating

Pyrrole is oxidized in aqueous medium to polypyrrole. Any surface in contact with this medium, here the threads of melamine sponge, becomes coated with a thin conducting polymer film (20−22) (Figure 2). The typical thickness of films produced in in situ precipitation polymerization is 100–200 nm. (21) In the absence of any additive, globular polypyrrole particles are produced in the medium surrounding the sponge, that is, inside the macropores, and they are also incorporated into the growing film or adhere to its surface (Figure 2a). The macroscopic precipitate is not observed within the macropores by microscopy due to the way of the sample preparation for microscopy, but the incorporation of globular polypyrrole into coating is clearly visible (Figure 3a). The presence of the free polypyrrole is only revealed when the sponges are compressed or cut as an emanating “smoke” and the surrounding area gets “dirty” (Figure 1a). No changes in the melamine skeleton associated with the coating have been detected (Figure 3).

Figure 2

Figure 2. Polypyrrole coating produced on the threads of melamine sponge during (a) precipitation polymerization and in the dispersion mode stabilized (b) with PVP or (c) colloidal nanosilica.

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Figure 3

Figure 3. Micrographs of melamine sponge coated with polypyrrole (a) in the absence of any stabilizer, (b) in the presence of PVP, or (c) colloidal nanosilica taken at lower (left) and higher magnification (right).

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If the same experiment is carried out instead of water in the solution of PVP, the conducting polymer is produced as colloidal dispersion stabilized with this water-soluble polymer (21,23−25) (Figure 2b). The typical size of colloidal particles is about 100 nm (Figure 4a). They are easily removed from open-cell pores with the size of tens of micrometres (Figure 3b). Also, outside the sponge, a stable colloid, a “soluble” polypyrrole, is produced. Such preparation is referred to proceed in the dispersion mode. The polypyrrole films are produced on immersed substrates also in this case. Compared to the previous case, they are thinner and smoother, (24) with some colloidal particles occasionally attached to the film surface (Figure 3b). The analogous studies on polyaniline demonstrated that PVP does not become incorporated into the conducting polymer film. (24) There is no free polypyrrole precipitate which would later contaminate the surroundings during sponge processing (Figure 1b).

Figure 4

Figure 4. Transmission electron micrograph of (a) polypyrrole dispersion particles stabilized with PVP and (b) aggregates produced in the presence of colloidal nanosilica.

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The water-soluble PVP can also be replaced with an inorganic stabilizer (Figure 2c), colloidal nanosilica, here with a 35 nm particle size. In the case of polyaniline, colloidal dispersions of spherical nanoparticles are produced too. (26−28) The presence of nanosilica prevents the formation of a macroscopic polypyrrole precipitate, but the dispersions have not been stable and sedimented (Figure 4b). Electron microscopy reveals polypyrrole/nanosilica aggregates (Figure 3c), but the underlying polypyrrole films are of good quality (Figure 3c). At closer inspection and in contrast to PVP, silica nanoparticles are uniformly incorporated onto the polypyrrole film surface. (27)
The content of the conducting polymer was calculated from the increase in mass after polypyrrole deposition as 21.1 wt % for the sponge prepared in the absence of additives, 6.9 wt % in the presence of PVP, and 9.2 wt % with nanosilica. In the coating during the precipitation polymerization of pyrrole, an additional part of polypyrrole is present in the macropores as free powder (Figure 1a). This is absent in the dispersion coating, and the content of polypyrrole in sponges is reduced correspondingly. It has also been demonstrated that the coatings in the presence of steric stabilizers, PVP (24) and nanosilica, (27) are thinner than those prepared in their absence. This is additional reason for the reduction in conducting polymer content. The increase in mass after the coating procedure may be, in principle, due to the incorporation of the stabilizers to the polypyrrole coating. This was proved to be absent at least in the case of PVP, (24) but it is present, to some extent, in the case of nanosilica (Figure 3c); (27) the residue in the thermogravimetric analysis performed in air allows us to estimate the silica content in the sponge to 2 wt %.

2.2. FTIR Spectra

The Fourier transform infrared (FTIR) spectrum of the melamine sponge coated with polypyrrole is very close to the spectrum of PPy powder (5) (Figure 5). This is due to the similar chemical bonding in the molecular structure of both nitrogen-containing entities (Figure 6). Melamine sponge manifests itself by the characteristic peak at 812 cm–1 (spectrum M). (15) This peak is present even after the coating with polypyrrole, but its contribution becomes reduced (spectra PPy, +PVP, and +silica). This reflects the fact that the coatings in the presence of the colloidal stabilizer are thinner than those in their absence (24) but still penetrable to the infrared radiation. The peaks of poly(N-vinylpyrrolidone) are absent (spectrum +PVP) because this polymer is not incorporated into polypyrrole coatings. (24) Silica, on the other hand, is present, but its content is low, limited to a few percent, and silica does not display any sharp absorption peaks. For this reason, the presence of silica manifests itself only as a modest broad-band shift of a baseline.

Figure 5

Figure 5. ATR FTIR spectra of the melamine sponge coated with polypyrrole in the absence (PPy) and in the presence of PVP (+PVP) or colloidal nanosilica (+silica). The spectra of melamine (M), PVP, and nanosilica are shown for the comparison.

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Figure 6

Figure 6. Molecular structure of (a) polypyrrole salt (hydrochloride) and (b) melamine incorporated in melamine/formaldehyde sponge. R = H or a linkage to another melamine unit.

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2.3. Surface Properties

The specific surface area and pore volume of the sponges coated with polypyrrole in the dispersion mode are higher compared to the standard coating (Figure 7, Table 1). This is positive news for most applications. In the standard coating, the macropores seem to be blocked by the polypyrrole precipitate. Almost the third of sample weight was lost at degassing before and in the course of surface area determination due to the free polypyrrole particles, which are not attached to the sponge skeleton and easily leave the macroporous interior (Figure 1a). Such a mass decrease has not been observed when the coating took place in the dispersion mode (Figure 1b). Mass reduction was taken into account when evaluating the specific surface area.

Figure 7

Figure 7. (a) Adsorption isotherms and (b) pore size distribution of the melamine sponge coated with polypyrrole (squares) compared with the coating in the presence of PVP (circles) or colloidal nanosilica (triangles).

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Table 1. Specific Surface Area and Pore Volume of Melamine Sponge Coated with Polypyrrole Compared with the Coating in the Presence of PVP or Colloidal Nanosilica
sampleS, m2 g–1V, cm3 g–1
melamine spongea39.2 ± 0.50.071 ± 0.001
polypyrrole-coated sponge75.2 ± 0.60.081 ± 0.002
+PVP158 ± 5.10.233 ± 0.015
+silica172 ± 110.241 ± 0.012
a

Taken from ref (15).

2.4. Conductivity

The conductivity is an intensive electrical characteristic of the material that does not depend on the size and shape of the samples. Its determination by the four-point van der Pauw method as a function of pressure is not trivial, and the reader is referred to the Experimental Section for details. The conductivity of the sponges coated with polypyrrole increases by about two orders of magnitude during the compression as expected (Figure 8) because the number of conducting pathways per infinitesimal sample cross-section increases. The sponge coated with polypyrrole in the dispersion mode in the presence of PVP or colloidal nanosilica has a comparable conductivity. After compression, the conductivity reaches the order of 10–1 S cm–1 and approaches the conductivity of globular polypyrrole, which is of the same order of magnitude. (5) The coating of sponges with polypyrrole in the precipitation mode, despite the higher polypyrrole content, is lower by about 1 order of magnitude. We can speculate that, in this case, free polypyrrole particles that are not attached to the sponge threads do not contribute to the conduction.

Figure 8

Figure 8. Conductivity of the melamine sponges coated with polypyrrole in the absence and in the presence of PVP or colloidal nanosilica.

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2.5. Resistance

For the practical applications, for example, in pressure sensing, the change in the sample resistance (extensive quantity), rather than the conductivity (intensive quantity), is of prime interest. In this case, the resistance of the sample decreases when the pressure is applied (Figure 9). The change in resistance is the result of the increasing conductivity (Figure 8) along with the reduced length of the cylindrical sample during compression. The results of conductivity and resistance determination cannot be directly compared. The former method uses a direct current and pressures approaching 10 MPa, while the latter exploits the alternating current of 1 kHz frequency at pressures of up to ≈0.1 MPa. In the last case, a parallel resistance of the Rp – Cp equivalent electrical circuit of the sponge (circuit selected based on the inner sample shape) is evaluated along with the compression or expansion.

Figure 9

Figure 9. Resistance of the melamine sponge coated with polypyrrole in the absence (squares) and in the presence of PVP (circles) or colloidal nanosilica (triangles) during compression (full symbols) and pressure release (open symbols).

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The resistance Rp of the sponge coated with polypyrrole in the absence of any stabilizer increases more than four orders of magnitude at full compression (Figure 9). By 100% compression, we mean the state at the maximum applied pressure 170 kPa. From the practical point of view, the use of the sponge at low compression (up to 40%) is limited as the resistance Rp is in the order of MΩ. This brings problems associated with electrical noise added to the measured signal. Hence, the sponge coated with polypyrrole only can be considered as insensitive to low pressures equal up to approx. 40% of compression. We assume that at low pressures, the free polypyrrole is distributed within the macropores, and only later, at higher pressure, it becomes squeezed between polypyrrole-coated threads and starts to participate in the conduction. There is a marked memory effect, that is, the length of the sponge does not completely recover after the pressure is released.
The sponge coated in the presence of PVP is less sensitive to the small pressure changes, and the resistance Rp decreases only by two orders of magnitude, but the resistance Rp is generally lower than in the preceding case (Figure 9). This may be of benefit in compressible and flexible supercapacitor electrodes. The memory effect is less pronounced compared with the polypyrrole coating in the absence of the stabilizer. The introductory experiment proves that the memory effect can be eliminated using pressures below ≈10 kPa. Finally, sponges coated by polypyrrole and in the presence of nanosilica exhibit the lowest resistance Rp (Figure 9). This sponge is again almost insensitive to initial compression up to approximately 40%. Moreover, a similar memory effect can be also observed here.
In conclusion, the addition of PVP to the synthesis protocol brings the benefits in the form of a moderate decrease in resistance which allows us to use the sponge in the whole compression range along with a modest memory effect, which allows the sponge to expand back to the initial length.

2.6. Antibacterial Properties

Antibacterial properties are welcome for materials planned to be applied in many fields of industry and in biomedicine, and water-pollution treatment may serve as an example. The melamine-formaldehyde/poly(vinyl alcohol) composite was reported to have bactericidal effects, (11) and such a behavior thus might be expected from the melamine-formaldehydemelamine-formaldehyde sponge alone. Another study on neat melamine sponges, however, has not revealed any antibacterial properties. (29) On the other hand, polypyrrole was found to display marked antibacterial properties, (30) which could be still enhanced by incorporation of silver nanoparticles. (31)
The results indicate that the presence of polypyrrole-coated sponges in the bacterial broth significantly reduces the number of colony-forming units (Table 2). The effect of melamine sponge alone is only marginal, but the coating with polypyrrole reduced the number of bacterial units by 3–4 orders of magnitude. Especially, the polypyrrole coating with incorporated nanosilica is efficient in antibacterial performance (Table 2), possibly due to the expected higher hydrophilicity and closer interaction with bacteria. In the present case, this can be assigned not only to the restricted bacterial growth but, alternatively or in the combination, also due to the adsorption and subsequent deactivation of bacteria on the sponge. (30) Regardless of the mechanism, the sponges can be considered as materials with good antibacterial performance.
Table 2. Concentration of Colony-Forming Units (CFU mL–1) in Bacterial Suspensions in the Presence of Melamine Sponges Coated in Various Ways with Polypyrrole
coatingStaphylococcus aureusEscherichia coli
reference8.4 × 1061.3 × 108
no coating1.5 × 1061.3 × 107
PPy coating1.5 × 1053.8 × 106
+PVP7.5 × 1046.8 × 105
+silica3.7 × 1021.1 × 105

3. Conclusions

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The dispersion coating of melamine sponges with polypyrrole produced in the course of dispersion polymerization of pyrrole in the presence of PVP or colloidal nanosilica has several positive effects compared to the coating in the absence of stabilizers: (1) no contaminating polypyrrole precipitate produced inside the sponge, (2) the improved conductivity by 1 order of magnitude, (3) reduced memory effect upon compression and release, and (4) enhanced specific surface area. These polypyrrole-coated sponges can be applied as pressure-sensitive materials applicable in biomedicine with the benefit of antimicrobial performance.

4. Experimental Section

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4.1. Preparation

Commercial open-cell macroporous melamine-formaldehyde sponges of the Basotect type (BASF AG, Germany) advertised as miraculous sponges were delivered in 105 × 62 × 25 mm3 blocks from a local distributor Drogerie ZDE (Czech Republic). They were coated with polypyrrole in an aqueous reaction mixture containing 0.05 M pyrrole and 0.125 M iron(III) chloride hexahydrate (Sigma-Aldrich). (15) For the preparation of polypyrrole in 1 L of the reaction mixture, pyrrole (3.35 g) and iron(III) chloride hexahydrate (33.8 g) were dissolved separately in water. The volume of solutions was adjusted to 0.5 L. Both solutions were precooled to 4 °C, mixed, and poured quickly over the melamine sponge. The sponge was gently squeezed to assure the penetration of the reaction mixture into the sponge. The precipitation polymerization of pyrrole was left to proceed for 1 h. The sponge was removed and transferred repeatedly to 0.1 M hydrochloric acid until no colored byproducts were observed. The sponge was then immersed several times in ethanol to remove water and then left to dry in air at room temperature.
The coating with polypyrrole in the dispersion mode was carried out in a similar manner, and only water was replaced with a 2 wt % aqueous solution of PVP (molecular weight 360,000; Fluka, Switzerland) or 5 wt % colloidal nanosilica Ludox AS-40 (Du Pont product distributed by Aldrich).

4.2. Characterization

Morphology of sponges was observed with a scanning ultrahigh-resolution electron microscope MAIA3 Tescan (Brno, Czech Republic) and that of colloidal particles was observed with a transmission electron microscope Tecnai G2 Spirit (FEI).
FTIR spectra were recorded with a Thermo Nicolet 6700 FTIR spectrometer equipped with a GladiATR (PIKE Technologies, USA) using an attenuated total reflection (ATR) monolithic diamond in the wavenumber range 2000–400 cm–1, 64 scans at 4 cm–1 resolution. The spectra were corrected for carbon dioxide and humidity in the optical path.
The specific surface area and pore volume were determined with a NOVA3200 (Quantachrome Instruments). Sponges were degassed for 24 h at 100 °C. The adsorption and desorption isotherms were recorded with nitrogen (Linde, 99.999%). Brunauer–Emmett–Teller analysis has been used to determine the total surface area, and the Barrett–Joyner–Halenda model was used for pore volume. Each sample was characterized four times, and the results were averaged. The experimental error was 5%.
For the electrical characterization, cylinders 10 mm in diameter were cut with a circular cork-cutter knife from the sponge and trimmed to ca 8 mm length. The conductivity was determined by the four-point van der Pauw method. A sample was placed in a lab-made cylindrical glass cell with an inner diameter of 10 mm between an insulating support and a glass piston carrying four platinum/rhodium electrodes on the perimeter of its base. The pressure applied to the sponge was controlled with an L6E3 load cell (Zemic Europe BV, The Netherlands). The thickness of the sponge during the compression was determined with a displacement meter Digimatic Indicator 543-122FB (Mitutoyo Corp., Japan).
For the determination of resistance in another apparatus, a cylinder having 19.5 mm diameter and 60 mm length was cut from the sponge. The sponge cylinder was placed inside the transparent tube of the same inner diameter directing the compression and expansion of the sponge. Two phosphor bronze circular electrodes were placed on the bottom and on the top of the sponge in the cylinder. A four-wire setup allowing us to measure low resistances have been used for continuous AC measurement (voltage 1 V, frequency 1 kHz) of parallel resistance R of the sample with an LCR-6002 meter (GW-Instek, USA). The pressure sensor was placed under the Sauter TVL testing stand equipped by force gauge Sauter FH50 creating a maximum force of 50 N with a resolution of 0.01 N. The extent of compression and expansion was measured with an inbuilt deflection gauge with a resolution of 10 μm. The pressure P acting on the sensor was calculated using the formula P = F/A, where F is the force measured by the force gauge and A is an in-plane cross-sectional area of the sponge.

4.3. Antibacterial Tests

The antibacterial activity was determined using two common model bacterial species, the Staphylococcus aureus (CCM 4516) and Escherichia coli (CCM 4517) (both purchased from the Czech Collection of Microorganisms; Czech Republic). First, the bacterial suspension containing S. aureus or E. coli in nutrient broth (NB) and plate count-agar (PCA) (Sigma-Aldrich) was prepared according to 1/500 NB 8.4 g per 400 mL and PCA 9.4 g per 400 mL. The pieces of sponge of an external area of ∼350 mm2 were immersed in the bacterial suspension and gently shaken for 24 h at 37 °C. Thereafter, the bacterial suspensions from each sample were pipetted into plastic tubes subject to decimal dilutions. The individual solutions with the bacterial suspensions were homogenized, and 1 mL was pipetted onto agar. Samples were incubated for 24 h at 37 °C, and subsequently, the number of colonies (CFU mL–1) was evaluated using the computer-aided cell colony counting.

Author Information

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  • Corresponding Author
  • Authors
    • Miroslava Trchová - University of Chemistry and Technology, Prague, 166 28 Prague 6, Czech Republic;  Orcidhttps://orcid.org/0000-0001-6105-7578
    • Hayk Kasparyan - University of Chemistry and Technology, Prague, 166 28 Prague 6, Czech Republic
    • Dušan Kopecký - University of Chemistry and Technology, Prague, 166 28 Prague 6, Czech Republic
    • Zdeňka Kolská - Faculty of Science, J.E. Purkyně University, 400 96 Ústí nad Labem, Czech Republic
    • Jan Prokeš - Faculty of Mathematics and Physics, Charles University, 180 00 Prague 8, Czech Republic
    • Ivo Křivka - Faculty of Mathematics and Physics, Charles University, 180 00 Prague 8, Czech Republic
    • Jan Vajďák - Centre of Polymer Systems, Tomas Bata University in Zlín, 760 01 Zlín, Czech Republic
    • Petr Humpolíček - Centre of Polymer Systems, Tomas Bata University in Zlín, 760 01 Zlín, Czech Republic;  Orcidhttps://orcid.org/0000-0002-6837-6878
  • Notes
    The authors declare no competing financial interest.

Acknowledgments

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The authors thank the Czech Science Foundation (19-04859S and 21-09830S) and internal Prague University research project (A2_FCHI_2021_003) for financial support. P. H. and J. V. acknowledge the support of the project funded by the Ministry of Education, Youth and Sports of the Czech Republic (DKRVO RP/CPS/2020/001).

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    Kopecká, J.; Kopecký, D.; Vrňata, M.; Fitl, P.; Stejskal, J.; Trchová, M.; Bober, P.; Morávková, Z.; Prokeš, J.; Sapurina, I. Polypyrrole nanotubes: mechanism of formation. RSC Adv. 2014, 4, 1551– 1558,  DOI: 10.1039/c3ra45841e
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    Polypyrrole nanotubes: mechanism of formation
    Kopecka, Jitka; Kopecky, Dusan; Vrnata, Martin; Fitl, Premysl; Stejskal, Jaroslav; Trchova, Miroslava; Bober, Patrycja; Moravkova, Zuzana; Prokes, Jan; Sapurina, Irina
    RSC Advances (2014), 4 (4), 1551-1558CODEN: RSCACL; ISSN:2046-2069. (Royal Society of Chemistry)
    This article presents a contribution to better understanding of the processes which take place during the synthesis of polypyrrole nanotubes using a structure-guiding agent, methyl orange. Polypyrrole was prepd. by oxidn. of pyrrole monomer with iron(III) chloride. In the presence of methyl orange, the formation of nanotubes was obsd. instead of the globular morphol. Two reaction schemes with reversed addns. of oxidant and monomer have been tested and they show remarkable influence on the produced morphol. Nanotubes with circular or rectangular profiles and diams. from tens to hundreds of nanometers have been obtained. FTIR and Raman spectra were used to assess the mol. structure of polypyrrole and detect residual methyl orange in the samples. The cond. of nanotubes compressed into pellets was as high as 68 S cm-1. The mechanism of nanotubular formation starting at the nucleus produced with the participation of org. dye is proposed. The growth of a nanotube, however, proceeds in the absence of a template. An alternative mechanism for the formation of nanotubes, the coating of solid templates with a polypyrrole overlayer, is also discussed.
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  5. 5
    Stejskal, J.; Kohl, M.; Trchová, M.; Kolská, Z.; Pekárek, M.; Křivka, I.; Prokeš, J. Conversion of conducting polypyrrole nanostructures to nitrogen-containing carbons and its impact on the adsorption of organic dye. Mater. Adv. 2021, 2, 706– 717,  DOI: 10.1039/d0ma00730g
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    Conversion of conducting polypyrrole nanostructures to nitrogen-containing carbons and its impact on the adsorption of organic dye
    Stejskal, Jaroslav; Kohl, Miroslav; Trchova, Miroslava; Kolska, Zdenka; Pekarek, Michal; Krivka, Ivo; Prokes, Jan
    Materials Advances (2021), 2 (2), 706-717CODEN: MAADC9; ISSN:2633-5409. (Royal Society of Chemistry)
    New types of materials were produced by gradual heating of a conducting polymer, polypyrrole, to elevated temps. Three polymers differing in morphol. - globules, nanofibers, and nanotubes - were exposed to temps. from 100 to 700°C in an argon atm. The yields always exceeded 50 wt%, and the morphol. features of the polymer were preserved. The transformation of polypyrrole salts to the corresponding bases followed by the carbonization was monitored by FTIR spectroscopy. The elemental anal. confirmed the subsequent conversion of polypyrrole to nitrogen-contg. carbon. The sp. surface areas were of the order of tens of m2 g-1; they increased from globules to nanotubes and nanofibers but were virtually independent of the exposition temp. The cond. of the powders was compared with that of the pellets when their prepn. was possible. As the temp. was increased up to 400°C, the cond. decreased for all samples by ca. 5 orders of magnitude, e.g., for nanofibers from 10 to 10-4 S cm-1 but recovered to 10-1 S cm-1 after the subsequent carbonization up to 700°C. Polypyrroles exposed to various temps. were then tested for the adsorption of org. dye, Reactive Black 5, from water. The dye adsorption on original polypyrroles strongly depended on the polymer morphol. Polypyrrole nanofibers were able to remove the dye completely with a capacity of 100 mg g-1, while the adsorption on polypyrrole globules was poor.
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    Fedorova, S.; Stejskal, J. Surface and precipitation polymerization of aniline. Langmuir 2002, 18, 5630– 5632,  DOI: 10.1021/la025665o
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    Surface and Precipitation Polymerization of Aniline
    Fedorova, Svetlana; Stejskal, Jaroslav
    Langmuir (2002), 18 (14), 5630-5632CODEN: LANGD5; ISSN:0743-7463. (American Chemical Society)
    The oxidative polymn. of aniline at surfaces precedes the pptn. polymn. in the bulk vol. of the aq. phase. This is illustrated by the faster formation of PANI in the presence of silica gel, a substrate with a high sp. surface area. The effect is explained by the heterogeneous catalysis of the PANI-chain initiation afforded by a surface. The coating of silica gel with a PANI overlayer does not take place only on the external surface of particles but also in the pores. The better understanding of the coating mechanism is likely to improve the quality of conducting polyaniline films deposited on the surface of various substrates.
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  7. 7
    Korupalli, C.; Li, H.; Nguyen, N.; Mi, F. L.; Chang, Y.; Lin, Y. J.; Sung, H. W. Conductive materials for healing wounds: their incorporation in electroactive wound dressings, characterization, and perspectives. Adv. Healthcare Mater. 2020, 10, 2001384,  DOI: 10.1002/adhm.202001384
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    Chatzimitakos, T. G.; Stalikas, C. D. Sponges and sponge-like materials in sample preparation: a journey from past to present and into the future. Molecules 2020, 25, 3673,  DOI: 10.3390/molecules25163673
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    Sponges and sponge-like materials in sample preparation: a journey from past to present and into the future
    Chatzimitakos, Theodoros G.; Stalikas, Constantine D.
    Molecules (2020), 25 (16), 3673CODEN: MOLEFW; ISSN:1420-3049. (MDPI AG)
    A review. Even though instrumental advancements are constantly being made in anal. chem., sample prepn. is still considered the bottleneck of anal. methods. To this end, researchers are developing new sorbent materials to improve and replace existing ones, with the ultimate goal to improve current methods and make them more efficient and effective. A few years ago, analternative trend was started toward sample prepn.: the use of sponge or sponge-like materials. These materials possess favorable characteristics, such as negligible wt., open-hole structure, high surface area, and variable surface chem. Although their use seemed promising, this trend soon reversed, due to either the increasing use of nanomaterials in sample prepn. or the limited scope of the first materials. Currently, with the development of new materials, such as melamine sponges, along with the advancement in nanotechnol., this topic was revived, and various functionalizations were carried out on such materials. The new materials are used as sorbents in sample prepn. in anal. chem. This review explores the development of such materials, from the past to the present and into the future, as well as their use in anal. chem.
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  9. 9
    Li, Y.; Fan, J.; Wang, R.; Shou, W.; Wang, L.; Liu, Y. 3D tree-shaped hierarchical flax fabric for highly efficient solar steam generation. J. Mater. Chem. A 2021, 9, 2248– 2258,  DOI: 10.1039/d0ta09570b
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    Three dimensional tree-shaped hierarchical flax fabric for highly efficient solar steam generation
    Li, Yaping; Fan, Jie; Wang, Run; Shou, Wan; Wang, Liang; Liu, Yong
    Journal of Materials Chemistry A: Materials for Energy and Sustainability (2021), 9 (4), 2248-2258CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
    Solar steam generation as a promising technol. has great potential for application in wastewater treatment and seawater desalination. However, it remains challenging to develop low-cost, high-efficiency steam generators that are suitable for large scale application. Here, inspired by the natural transpiration process of trees, we fabricated a three-dimensional (3D) hierarchical tree-shaped biomimetic flax fabric (TBFF) using an ordinary loom, consisting of a float layer, basket weave layer and plain weave layer, which showed directional water transport properties along the continuous warp yarns of the fabric. Then, the obtained TBFF was modified by one-step synthesis of large-area polydopamine-polypyrrole composite (PDA-PPy) nanofibers for a high hydrophilicity and a higher surface area. The hierarchical micro-capillary pores of yarns and macro-interlaced pore structures between the warp and weft yarns in such modified TBFF-PDA-PPy exhibit broadband light absorption, high-efficiency water supply, large evapn. area, and easy steam escape. Therefore, the continuous water transport paths formed by TBFF-PDA-PPy could deliver an attractive evapn. rate of 1.37 kg m-2 h-1, where the solar energy conversion efficiency was up to 87.4% under 1 sun illumination. Based on the facile fabrication, low cost and scalable manufg. process, this nature-inspired design of 3D hierarchical TBFF-PDA-PPy is expected to promote large-scale applications in water purifn. and seawater desalination.
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  10. 10
    Naskar, P.; Maiti, A.; Chakraborty, P.; Kundu, D.; Biswas, B.; Banerjee, A. Chemical supercapacitors: a review focusing on metallic compounds and conducting polymers. J. Mater. Chem. A 2021, 9, 1970– 2017,  DOI: 10.1039/d0ta09655e
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    Chemical supercapacitors: a review focusing on metallic compounds and conducting polymers
    Naskar, Pappu; Maiti, Apurba; Chakraborty, Priyanka; Kundu, Debojyoti; Biswas, Biplab; Banerjee, Anjan
    Journal of Materials Chemistry A: Materials for Energy and Sustainability (2021), 9 (4), 1970-2017CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
    A review. Capacitors began their journey in 1745, and to date have advanced in the form of supercapacitors. Supercapacitors are one of the advanced forms of capacitors with higher energy d., bridging capacitors and batteries. The energy storage through the formation of an elec. double layer is pivotal for supercapacitor technol. Accordingly, to further improve the energy d., surface faradaic (pseudocapacitive) processes are employed, and henceforth, the journey of chem. supercapacitors commenced. Herein, the materials, mechanisms and fabrication of chem. supercapacitors based on metallic compds. and conducting polymers are discussed in detail. The inherent limitations of these materials are addressed, and the feasible mitigation measures are identified. Poor cond., slow diffusion kinetics and rapid structural disintegration over cycling are the common constraints of metallic compds., which can be overcome by prepg. conductive nanocomposites. Thus, versatile conductive nanocomposites of metal oxides, hydroxides, carbides, nitrides, phosphides, phosphates, phosphites, and chalcogenides are elaborated. A lack of structural integrity is the prime obstacle for the realization of conducting polymer-based supercapacitors, which may be solved by forming composites with robust support from carbonaceous materials or metallic compds. Consequently, the composites of polyaniline, polypyrrole, polythiophene and polythiophene-derivs. are discussed. The historical accounts of early stages of works are emphasized in order to review the developmental pathways of chem. supercapacitors. The construction of full cells and their performance data are presented herein, which synchronize the behavior of practical scaled-up devices. To the best of our knowledge, this review is the first holistic description of chem. supercapacitors based on metallic compds. and conducting polymers from the first reports to recent advancements.
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  11. 11
    Bhat, S. A.; Zafar, F.; Mondal, A. H.; Mirza, A. U.; Rizwanul Haq, Q. M.; Nishat, N. Efficient removal of Congo red dye from aqueous solution by adsorbent films of polyvinyl alcohol/melamine-formaldehyde composite and bactericidal effects. J. Clean. Prod. 2020, 255, 120062,  DOI: 10.1016/j.jclepro.2020.120062
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    Sapurina, I. Yu.; Shishov, M. A.; Ivanova, V. T. Sorbents for water purification based on conjugated polymers. Russ. Chem. Rev. 2020, 89, 1115– 1131,  DOI: 10.1070/rcr4955
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    12
    Sorbents for water purification based on conjugated polymers
    Sapurina, Irina Yu.; Shishov, Mikhail A.; Ivanova, Valeria T.
    Russian Chemical Reviews (2020), 89 (10), 1115-1131CODEN: RCRVAB; ISSN:0036-021X. (IOP Publishing Ltd.)
    The sorption properties of polymers with a polyconjugated chain structure (polyaniline and polypyrrole) are considered. The mol. mechanism of sorption by these polymers of various compds. such as heavy metal ions, toxic org. compds. and micropathogens, which are the most hazardous and stubborn contaminants in water, is discussed. The use of such sorbents to purify water from micropathogens, including bacteria and viruses, is addressed for the first time. The adsorption capacity of polyconjugated polymers for these types of contaminants, the efficiency of water treatment by these sorbents and characteristics of the currently used sorbents are analyzed. The applicability of polyaniline and polypyrrole and composites based on them as high-performance versatile sorbents for water treatment is discussed, taking into account the sorbent properties such as high stability, lack of soly., lack of toxicity and ability to be regenerated and reused.
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  13. 13
    Stejskal, J. Interaction of conducting polymers, polyaniline and polypyrrole, with organic dyes: polymer morphology control, dye adsorption and photocatalytic decomposition. Chem. Pap. 2020, 74, 1– 54,  DOI: 10.1007/s11696-019-00982-9
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    13
    Interaction of conducting polymers, polyaniline and polypyrrole, with organic dyes: polymer morphology control, dye adsorption and photocatalytic decomposition
    Stejskal, Jaroslav
    Chemical Papers (2020), 74 (1), 1-54CODEN: CHPAEG; ISSN:1336-9075. (Springer International Publishing AG)
    A review. Conducting polymers, such as polyaniline and polypyrrole, have frequently been discussed in the literature due to ease of prepn. and high application potential. These polymers have been obsd. to interact with org. dyes because of the similarity in the conjugated mol. structure of both moieties. The interaction manifests itself in three fundamental directions that have been so far treated sep. The first is represented by the cond. enhancement and morphol. control when using org. dyes as templates in polypyrrole prepn. The adsorption of dyes on conducting polymers is the second field oriented at the water pollution treatment. Finally, the photocatalytic decompn. of org. dyes aims at the similar environmental target. The last two applications do not require the presence of cond. which, on the other hand, is a key parameter of conducting polymers. The future design of advanced adsorbents, however, has to exploit both the cond. and electroactivity in the control of pollutant adsorption or degrdn. For this reason, all these interactions and their practical impact are considered in the present review.
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  14. 14
    Senguttuvan, S.; Senthilkumar, P.; Janaki, V.; Kamala-Kannan, S. Significance of conducting polyaniline based composites for the removal of dyes and heavy metals from aqueous solution and wastewaters - A review. Chemosphere 2021, 267, 129201,  DOI: 10.1016/j.chemosphere.2020.129201
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    14
    Significance of conducting polyaniline based composites for the removal of dyes and heavy metals from aqueous solution and wastewaters - A review
    Senguttuvan, S.; Senthilkumar, P.; Janaki, V.; Kamala-Kannan, S.
    Chemosphere (2021), 267 (), 129201CODEN: CMSHAF; ISSN:0045-6535. (Elsevier Ltd.)
    A review. Dyes and heavy metals pollution have become a major environmental concern worldwide. Various methods, such as advanced oxidn., biodegrdn., pptn., flocculation, ultra filtration, ion-exchange, electro-chem. degrdn. and coagulation, have been proposed for the removal of dyes and heavy metals from contaminated wastewater. Of these methods, adsorption and detoxification are considered as the most promising and economically viable. Polyaniline-based composites, a material prepd. by combining polyaniline with one or more similar or disimilar materials, have been reported as good adsorbents to remove and detoxify different groups of pollutants due to their unique phys. and chem. properties. In the last decade, several studies have reported the effective adsorption (⊂95%) of dyes and heavy metals onto polyaniline based composites. Furthermore, some polyaniline -composites reduced the adsorbed heavy metals into less toxic state. This review compiles the application of different polyaniline composites for adsorption and/or detoxifcation of dyes and heavy metals and documents composite prepn. methods, morphol. and properties of the composites, and mechanism of dyes and heavy metals adsorption. Based on the avilabile literature, this review suggests that more studies are warranted to understand the influence of various conditions and exptl. variables on dyes and heavy metals removal from wastewater and/or aq. soln.
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  15. 15
    Stejskal, J.; Sapurina, I.; Vilčáková, J.; Jurča, M.; Trchová, M.; Kolská, Z.; Prokeš, J.; Křivka, I. One-pot preparation of conducting melamine/polypyrrole/magnetite ferrosponge. ACS Appl. Polym. Mater. 2021, 3, 1107– 1115,  DOI: 10.1021/acsapm.0c01331
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    15
    One-Pot Preparation of Conducting Melamine/Polypyrrole/Magnetite Ferrosponge
    Stejskal, Jaroslav; Sapurina, Irina; Vilcakova, Jarmila; Jurca, Marek; Trchova, Miroslava; Kolska, Zdenka; Prokes, Jan; Krivka, Ivo
    ACS Applied Polymer Materials (2021), 3 (2), 1107-1115CODEN: AAPMCD; ISSN:2637-6105. (American Chemical Society)
    Polypyrrole was deposited in situ on the macroporous open-cell melamine sponge by the oxidn. of pyrrole with iron(III) chloride. The oxidant was used in excess, and the reaction mixt. after the polymn. thus contained both iron(II) and iron(III) chlorides. These subsequently provided magnetite after treatment with ammonia soln. The conducting melamine/polypyrrole produced in the first step thus afforded melamine/polypyrrole/magnetite ferrosponge in the second. The composite sponge was characterized with respect to mol. structure by FTIR spectroscopy. The dependence of cond. on the sponge compression is provided and magnetic properties have also been detd. The performance of sponge in electromagnetic radiation shielding in GHz region is demonstrated. While conducting polypyrrole afforded the radiation reflection, magnetite added the absorption component.
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  16. 16
    Li, X.; Sun, Q.; Kan, Y.; Zhu, Y.; Pang, Z.; Li, M.; Jin, Y. Self-powered humidity sensor based on polypyrrole/melamine aerogel for real-time humidity monitoring. IEEE Sensor J. 2021, 21, 2604– 2609,  DOI: 10.1109/jsen.2020.3027743
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    16
    Self-powered humidity sensor based on polypyrrole/melamine aerogel for real-time humidity monitoring
    Li, Xiaoqiang; Sun, Qian; Kan, Yan; Zhu, Yanan; Pang, Zengyuan; Li, Mengjuan; Jin, Yang
    IEEE Sensors Journal (2021), 21 (3), 2604-2609CODEN: ISJEAZ; ISSN:1558-1748. (Institute of Electrical and Electronics Engineers)
    Measuring or monitoring air humidity is an increasing demands in the various fields. In this work, a simple and convenient method was utilized to prep. a melamine aerogel (MA) based sensor for humidity measurement. The sensing material was made from polymn. of polypyrrole (PPy) in the matrix of MA. The surface morphol. was characterized by SEM (SEM) to examine the inner structure of the sensing material. MA was chosen as the substrate owing to the porous structure, which facilities the adsorption of water mols. from the air. The self-powered humidity sensor was manufd. by adhering conductive tapes on both side of PPy modified MA (PPy@MA). The sensor has a flexible, ultralight and ultraporous structure, and could generate humidity-induced open-circuit voltage from the concn. gradient of the H+ ions. The PPy@MA sensor exhibited the response and recovery time of 1.1 s and 4.5 s, resp., when it is used for sensing the flowing wet air (RH 75 %). Furthermore, the sensitivity of the self-powered humidity sensor was evaluated by assessing the moisture changes of the human skin, and the moisture from the human breath.
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  17. 17
    Wu, X.; Lei, Y.; Li, S.; Huang, J.; Teng, L.; Chen, Z.; Lai, Y. Photothermal and Joule heating-assisted thermal management sponge for efficient cleanup of highly viscous crude oil. J. Hazard. Mater. 2021, 403, 124090,  DOI: 10.1016/j.jhazmat.2020.124090
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    17
    Photothermal and Joule heating-assisted thermal management sponge for efficient cleanup of highly viscous crude oil
    Wu, Xingwang; Lei, Yonggang; Li, Shuhui; Huang, Jianying; Teng, Lin; Chen, Zhong; Lai, Yuekun
    Journal of Hazardous Materials (2021), 403 (), 124090CODEN: JHMAD9; ISSN:0304-3894. (Elsevier B.V.)
    Fast and efficient cleanup of high-viscosity oil spills on the sea is still a global challenge today. Traditional recycling methods are either energy demanding or inefficient. Hydrophobic/oleophilic sorbents are promising candidates to handle oil spills, but they have limited ability to recover high viscosity oil. In this work, we report a superhydrophobic/oleophilic carbon nanotubes (CNT) and polypyrrole (PPy) coated melamine sponge (m-CNT/PPy@MS). The CNT/PPy coating enables the sponge to convert light and electricity to heat, ensuring that the absorbent can adapt to various working environments. The rapid heat generation on the sponge surface can significantly reduce the viscosity of crude oil and accelerate the absorption rate, thereby achieving the purpose of rapid recovery of oil spills. Under one sun illumination (1.0 kW/m2) and an applied voltage (8 V), the surface temp. of the m-CNT/PPy@MS can reach 118.6°C. The complete penetration time of oil droplets is 93.5% less than that of an unheated sponge. In addn., under half sun irradn. intensity and 11 V, the porous sponge absorbed 6.92 kg/m2 of crude oil in the first minute, which is about 31 times as much as that of an unheated sponge. Finally, we demonstrate a continuous absorption system, consisting of a self-heating m-CNT/PPy@MS and peristaltic pump, that can continuously recover oil spills on the sea surface. In view of its unique design, lower cost and fast oil absorption speed, this work provides a new option to tackle large-scale oil spill disasters on the sea surface.
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    Mahmud, H. N. M. E.; Huq, A. K. O.; Yahya, R. B. The removal of heavy metal ions from wastewater/aqueous solution using polypyrrole-based adsorbents: a review. RSC Adv. 2016, 6, 14778– 14791,  DOI: 10.1039/c5ra24358k
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    Qin, C.; Yue, Z.; Chao, Y.; Forster, R. J.; Maolmhuaidh, F. Ó.; Huang, X.-F.; Beirne, S.; Wallace, G. G.; Chen, J. Bipolar electroactive conducting polymers for wireless cell stimulation. Appl. Mater. Today 2020, 21, 100804,  DOI: 10.1016/j.apmt.2020.100804
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    Sapurina, I.; Riede, A.; Stejskal, J. In-situ polymerized polyaniline films. Synth. Met. 2001, 123, 503– 507,  DOI: 10.1016/s0379-6779(01)00349-6
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    In-situ polymerized polyaniline films 3. Film formation
    Sapurina, I.; Riede, A.; Stejskal, J.
    Synthetic Metals (2001), 123 (3), 503-507CODEN: SYMEDZ; ISSN:0379-6779. (Elsevier Science S.A.)
    Polyaniline films were produced on a glass surface immersed in the reaction mixt. during the oxidative polymn. of aniline. Glass supports placed in the reaction mixt. at the start of the oxidn. were gradually removed during the reaction. The thickness of the films produced on glass, assessed by optical absorption, was followed as a function of reaction time. The progress of polymn. was monitored by temp. changes. In another expt., glass supports were successively inserted into the polymn. mixt. The formation of polyaniline films on glass precoated with polyaniline was also investigated. A proposed model of film formation is based on the concept of primary and secondary nucleation. Oligoaniline cation radicals adsorbed on the glass surface nucleate the primary growth of polyaniline film, and the secondary nucleation occurs on the produced polyaniline layer.
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    Stejskal, J.; Sapurina, I. Polyaniline: thin films and colloidal dispersions (IUPAC technical report). Pure Appl. Chem. 2005, 77, 815– 826,  DOI: 10.1351/pac200577050815
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    21
    Polyaniline: Thin films and colloidal dispersions
    Stejskal, Jaroslav; Sapurina, Irina
    Pure and Applied Chemistry (2005), 77 (5), 815-826CODEN: PACHAS; ISSN:0033-4545. (International Union of Pure and Applied Chemistry)
    Several workers from various institutions in six countries have prepd. thin films and colloidal polyaniline dispersions. The films were produced in situ on glass supports during the oxidn. of anilinium chloride with ammonium peroxydisulfate in water. The av. thickness of the films, assessed by optical absorption, was 125 ± 9 nm, and the cond. of films was 2.6 ± 0.7 S cm-1. Films prepd. in 1 mol l-1 HCl had a similar thickness, 109 ± 10 nm, but a higher cond., 18.8 ± 7.1 S cm-1. Colloidal polyaniline particles stabilized with a water-sol. polymer, poly(N-vinylpyrrolidone) [poly(1-vinylpyrrolidone-2-one)], have been prepd. by dispersion polymn. The av. particle size, 241 ± 50 nm, and polydispersity, 0.26 ± 0.12, have been detd. by dynamic light scattering. The prepn. of these two supramol. polyaniline forms was found to be well reproducible.
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This article is cited by 11 publications.

  1. Jianming Zhao, Xingyue Guo, Jiayu Yang, Yajie Xie, Yudong Zheng. In Situ Polymerization of Methylene Blue on Bacterial Cellulose for Photodynamic/Photoelectricity Synergistic Inhibition of Bacterial Biofilm Formation. ACS Applied Materials & Interfaces 2023, 15 (37) , 43591-43606. https://doi.org/10.1021/acsami.3c09449
  2. Musashi Seike, Makoto Uda, Toyoko Suzuki, Hideto Minami, Shinya Higashimoto, Tomoyasu Hirai, Yoshinobu Nakamura, Syuji Fujii. Synthesis of Polypyrrole and Its Derivatives as a Liquid Marble Stabilizer via a Solvent-Free Chemical Oxidative Polymerization Protocol. ACS Omega 2022, 7 (15) , 13010-13021. https://doi.org/10.1021/acsomega.2c00327
  3. Jaroslav Stejskal, Dušan Kopecký, Hayk Kasparyan, Jarmila Vilčáková, Jan Prokeš, Ivo Křivka. Melamine Sponges Decorated with Polypyrrole Nanotubes as Macroporous Conducting Pressure Sensors. ACS Applied Nano Materials 2021, 4 (7) , 7513-7519. https://doi.org/10.1021/acsanm.1c01634
  4. Fahanwi Asabuwa Ngwabebhoh, Tomáš Sáha, Jaroslav Stejskal, Miroslava Trchová, Dušan Kopecký, Jiří Pfleger. Conducting polypyrrole-coated leathers. Progress in Organic Coatings 2023, 179 , 107495. https://doi.org/10.1016/j.porgcoat.2023.107495
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  11. Jaroslav Stejskal, Irina Sapurina, Jarmila Vilčáková, Petr Humpolíček, Thanh Huong Truong, Mikhail A. Shishov, Miroslava Trchová, Dušan Kopecký, Zdeňka Kolská, Jan Prokeš, Ivo Křivka. Conducting polypyrrole-coated macroporous melamine sponges: a simple toy or an advanced material?. Chemical Papers 2021, 75 (10) , 5035-5055. https://doi.org/10.1007/s11696-021-01776-8
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  • Abstract

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    Figure 1

    Figure 1. Melamine sponges after being compressed with hand and released: (a) polypyrrole coating and (b) reduced polypyrrole content deposited in the presence of PVP.

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    Figure 2

    Figure 2. Polypyrrole coating produced on the threads of melamine sponge during (a) precipitation polymerization and in the dispersion mode stabilized (b) with PVP or (c) colloidal nanosilica.

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    Figure 3

    Figure 3. Micrographs of melamine sponge coated with polypyrrole (a) in the absence of any stabilizer, (b) in the presence of PVP, or (c) colloidal nanosilica taken at lower (left) and higher magnification (right).

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    Figure 4

    Figure 4. Transmission electron micrograph of (a) polypyrrole dispersion particles stabilized with PVP and (b) aggregates produced in the presence of colloidal nanosilica.

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    Figure 5

    Figure 5. ATR FTIR spectra of the melamine sponge coated with polypyrrole in the absence (PPy) and in the presence of PVP (+PVP) or colloidal nanosilica (+silica). The spectra of melamine (M), PVP, and nanosilica are shown for the comparison.

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    Figure 6

    Figure 6. Molecular structure of (a) polypyrrole salt (hydrochloride) and (b) melamine incorporated in melamine/formaldehyde sponge. R = H or a linkage to another melamine unit.

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    Figure 7

    Figure 7. (a) Adsorption isotherms and (b) pore size distribution of the melamine sponge coated with polypyrrole (squares) compared with the coating in the presence of PVP (circles) or colloidal nanosilica (triangles).

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    Figure 8

    Figure 8. Conductivity of the melamine sponges coated with polypyrrole in the absence and in the presence of PVP or colloidal nanosilica.

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    Figure 9

    Figure 9. Resistance of the melamine sponge coated with polypyrrole in the absence (squares) and in the presence of PVP (circles) or colloidal nanosilica (triangles) during compression (full symbols) and pressure release (open symbols).

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  • References

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      A review. Polypyrrole (PPy) has unique features such as easy synthesis, environmental stability, and high elec. cond. (approx. 105 S/cm and even >380 S/cm) for bulk and thin-film materials. Thus, PPy is applied in numerous well-established applications, such as in sensors, supercapacitors, and resonators. These applications take advantage of the unique properties achieved through the structure and properties of PPy. This article comprehensively elaborates the methods used to synthesize conductive PPy, along with the important factors affecting its cond. Emphasis is given to versatile and basic approaches that enable control of the microstructural features that eventually det. PPy cond. Despite the intensive research in this area, no previous study has presented all possible relevant information about PPy fabrication and the important factors influencing its elec. cond.
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    4. 4
      Kopecká, J.; Kopecký, D.; Vrňata, M.; Fitl, P.; Stejskal, J.; Trchová, M.; Bober, P.; Morávková, Z.; Prokeš, J.; Sapurina, I. Polypyrrole nanotubes: mechanism of formation. RSC Adv. 2014, 4, 1551– 1558,  DOI: 10.1039/c3ra45841e
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      Polypyrrole nanotubes: mechanism of formation
      Kopecka, Jitka; Kopecky, Dusan; Vrnata, Martin; Fitl, Premysl; Stejskal, Jaroslav; Trchova, Miroslava; Bober, Patrycja; Moravkova, Zuzana; Prokes, Jan; Sapurina, Irina
      RSC Advances (2014), 4 (4), 1551-1558CODEN: RSCACL; ISSN:2046-2069. (Royal Society of Chemistry)
      This article presents a contribution to better understanding of the processes which take place during the synthesis of polypyrrole nanotubes using a structure-guiding agent, methyl orange. Polypyrrole was prepd. by oxidn. of pyrrole monomer with iron(III) chloride. In the presence of methyl orange, the formation of nanotubes was obsd. instead of the globular morphol. Two reaction schemes with reversed addns. of oxidant and monomer have been tested and they show remarkable influence on the produced morphol. Nanotubes with circular or rectangular profiles and diams. from tens to hundreds of nanometers have been obtained. FTIR and Raman spectra were used to assess the mol. structure of polypyrrole and detect residual methyl orange in the samples. The cond. of nanotubes compressed into pellets was as high as 68 S cm-1. The mechanism of nanotubular formation starting at the nucleus produced with the participation of org. dye is proposed. The growth of a nanotube, however, proceeds in the absence of a template. An alternative mechanism for the formation of nanotubes, the coating of solid templates with a polypyrrole overlayer, is also discussed.
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    5. 5
      Stejskal, J.; Kohl, M.; Trchová, M.; Kolská, Z.; Pekárek, M.; Křivka, I.; Prokeš, J. Conversion of conducting polypyrrole nanostructures to nitrogen-containing carbons and its impact on the adsorption of organic dye. Mater. Adv. 2021, 2, 706– 717,  DOI: 10.1039/d0ma00730g
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      5
      Conversion of conducting polypyrrole nanostructures to nitrogen-containing carbons and its impact on the adsorption of organic dye
      Stejskal, Jaroslav; Kohl, Miroslav; Trchova, Miroslava; Kolska, Zdenka; Pekarek, Michal; Krivka, Ivo; Prokes, Jan
      Materials Advances (2021), 2 (2), 706-717CODEN: MAADC9; ISSN:2633-5409. (Royal Society of Chemistry)
      New types of materials were produced by gradual heating of a conducting polymer, polypyrrole, to elevated temps. Three polymers differing in morphol. - globules, nanofibers, and nanotubes - were exposed to temps. from 100 to 700°C in an argon atm. The yields always exceeded 50 wt%, and the morphol. features of the polymer were preserved. The transformation of polypyrrole salts to the corresponding bases followed by the carbonization was monitored by FTIR spectroscopy. The elemental anal. confirmed the subsequent conversion of polypyrrole to nitrogen-contg. carbon. The sp. surface areas were of the order of tens of m2 g-1; they increased from globules to nanotubes and nanofibers but were virtually independent of the exposition temp. The cond. of the powders was compared with that of the pellets when their prepn. was possible. As the temp. was increased up to 400°C, the cond. decreased for all samples by ca. 5 orders of magnitude, e.g., for nanofibers from 10 to 10-4 S cm-1 but recovered to 10-1 S cm-1 after the subsequent carbonization up to 700°C. Polypyrroles exposed to various temps. were then tested for the adsorption of org. dye, Reactive Black 5, from water. The dye adsorption on original polypyrroles strongly depended on the polymer morphol. Polypyrrole nanofibers were able to remove the dye completely with a capacity of 100 mg g-1, while the adsorption on polypyrrole globules was poor.
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    6. 6
      Fedorova, S.; Stejskal, J. Surface and precipitation polymerization of aniline. Langmuir 2002, 18, 5630– 5632,  DOI: 10.1021/la025665o
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      Surface and Precipitation Polymerization of Aniline
      Fedorova, Svetlana; Stejskal, Jaroslav
      Langmuir (2002), 18 (14), 5630-5632CODEN: LANGD5; ISSN:0743-7463. (American Chemical Society)
      The oxidative polymn. of aniline at surfaces precedes the pptn. polymn. in the bulk vol. of the aq. phase. This is illustrated by the faster formation of PANI in the presence of silica gel, a substrate with a high sp. surface area. The effect is explained by the heterogeneous catalysis of the PANI-chain initiation afforded by a surface. The coating of silica gel with a PANI overlayer does not take place only on the external surface of particles but also in the pores. The better understanding of the coating mechanism is likely to improve the quality of conducting polyaniline films deposited on the surface of various substrates.
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    7. 7
      Korupalli, C.; Li, H.; Nguyen, N.; Mi, F. L.; Chang, Y.; Lin, Y. J.; Sung, H. W. Conductive materials for healing wounds: their incorporation in electroactive wound dressings, characterization, and perspectives. Adv. Healthcare Mater. 2020, 10, 2001384,  DOI: 10.1002/adhm.202001384
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      There is no corresponding record for this reference.
    8. 8
      Chatzimitakos, T. G.; Stalikas, C. D. Sponges and sponge-like materials in sample preparation: a journey from past to present and into the future. Molecules 2020, 25, 3673,  DOI: 10.3390/molecules25163673
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      8
      Sponges and sponge-like materials in sample preparation: a journey from past to present and into the future
      Chatzimitakos, Theodoros G.; Stalikas, Constantine D.
      Molecules (2020), 25 (16), 3673CODEN: MOLEFW; ISSN:1420-3049. (MDPI AG)
      A review. Even though instrumental advancements are constantly being made in anal. chem., sample prepn. is still considered the bottleneck of anal. methods. To this end, researchers are developing new sorbent materials to improve and replace existing ones, with the ultimate goal to improve current methods and make them more efficient and effective. A few years ago, analternative trend was started toward sample prepn.: the use of sponge or sponge-like materials. These materials possess favorable characteristics, such as negligible wt., open-hole structure, high surface area, and variable surface chem. Although their use seemed promising, this trend soon reversed, due to either the increasing use of nanomaterials in sample prepn. or the limited scope of the first materials. Currently, with the development of new materials, such as melamine sponges, along with the advancement in nanotechnol., this topic was revived, and various functionalizations were carried out on such materials. The new materials are used as sorbents in sample prepn. in anal. chem. This review explores the development of such materials, from the past to the present and into the future, as well as their use in anal. chem.
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    9. 9
      Li, Y.; Fan, J.; Wang, R.; Shou, W.; Wang, L.; Liu, Y. 3D tree-shaped hierarchical flax fabric for highly efficient solar steam generation. J. Mater. Chem. A 2021, 9, 2248– 2258,  DOI: 10.1039/d0ta09570b
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      9
      Three dimensional tree-shaped hierarchical flax fabric for highly efficient solar steam generation
      Li, Yaping; Fan, Jie; Wang, Run; Shou, Wan; Wang, Liang; Liu, Yong
      Journal of Materials Chemistry A: Materials for Energy and Sustainability (2021), 9 (4), 2248-2258CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
      Solar steam generation as a promising technol. has great potential for application in wastewater treatment and seawater desalination. However, it remains challenging to develop low-cost, high-efficiency steam generators that are suitable for large scale application. Here, inspired by the natural transpiration process of trees, we fabricated a three-dimensional (3D) hierarchical tree-shaped biomimetic flax fabric (TBFF) using an ordinary loom, consisting of a float layer, basket weave layer and plain weave layer, which showed directional water transport properties along the continuous warp yarns of the fabric. Then, the obtained TBFF was modified by one-step synthesis of large-area polydopamine-polypyrrole composite (PDA-PPy) nanofibers for a high hydrophilicity and a higher surface area. The hierarchical micro-capillary pores of yarns and macro-interlaced pore structures between the warp and weft yarns in such modified TBFF-PDA-PPy exhibit broadband light absorption, high-efficiency water supply, large evapn. area, and easy steam escape. Therefore, the continuous water transport paths formed by TBFF-PDA-PPy could deliver an attractive evapn. rate of 1.37 kg m-2 h-1, where the solar energy conversion efficiency was up to 87.4% under 1 sun illumination. Based on the facile fabrication, low cost and scalable manufg. process, this nature-inspired design of 3D hierarchical TBFF-PDA-PPy is expected to promote large-scale applications in water purifn. and seawater desalination.
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    10. 10
      Naskar, P.; Maiti, A.; Chakraborty, P.; Kundu, D.; Biswas, B.; Banerjee, A. Chemical supercapacitors: a review focusing on metallic compounds and conducting polymers. J. Mater. Chem. A 2021, 9, 1970– 2017,  DOI: 10.1039/d0ta09655e
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      Chemical supercapacitors: a review focusing on metallic compounds and conducting polymers
      Naskar, Pappu; Maiti, Apurba; Chakraborty, Priyanka; Kundu, Debojyoti; Biswas, Biplab; Banerjee, Anjan
      Journal of Materials Chemistry A: Materials for Energy and Sustainability (2021), 9 (4), 1970-2017CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
      A review. Capacitors began their journey in 1745, and to date have advanced in the form of supercapacitors. Supercapacitors are one of the advanced forms of capacitors with higher energy d., bridging capacitors and batteries. The energy storage through the formation of an elec. double layer is pivotal for supercapacitor technol. Accordingly, to further improve the energy d., surface faradaic (pseudocapacitive) processes are employed, and henceforth, the journey of chem. supercapacitors commenced. Herein, the materials, mechanisms and fabrication of chem. supercapacitors based on metallic compds. and conducting polymers are discussed in detail. The inherent limitations of these materials are addressed, and the feasible mitigation measures are identified. Poor cond., slow diffusion kinetics and rapid structural disintegration over cycling are the common constraints of metallic compds., which can be overcome by prepg. conductive nanocomposites. Thus, versatile conductive nanocomposites of metal oxides, hydroxides, carbides, nitrides, phosphides, phosphates, phosphites, and chalcogenides are elaborated. A lack of structural integrity is the prime obstacle for the realization of conducting polymer-based supercapacitors, which may be solved by forming composites with robust support from carbonaceous materials or metallic compds. Consequently, the composites of polyaniline, polypyrrole, polythiophene and polythiophene-derivs. are discussed. The historical accounts of early stages of works are emphasized in order to review the developmental pathways of chem. supercapacitors. The construction of full cells and their performance data are presented herein, which synchronize the behavior of practical scaled-up devices. To the best of our knowledge, this review is the first holistic description of chem. supercapacitors based on metallic compds. and conducting polymers from the first reports to recent advancements.
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    11. 11
      Bhat, S. A.; Zafar, F.; Mondal, A. H.; Mirza, A. U.; Rizwanul Haq, Q. M.; Nishat, N. Efficient removal of Congo red dye from aqueous solution by adsorbent films of polyvinyl alcohol/melamine-formaldehyde composite and bactericidal effects. J. Clean. Prod. 2020, 255, 120062,  DOI: 10.1016/j.jclepro.2020.120062
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      There is no corresponding record for this reference.
    12. 12
      Sapurina, I. Yu.; Shishov, M. A.; Ivanova, V. T. Sorbents for water purification based on conjugated polymers. Russ. Chem. Rev. 2020, 89, 1115– 1131,  DOI: 10.1070/rcr4955
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      12
      Sorbents for water purification based on conjugated polymers
      Sapurina, Irina Yu.; Shishov, Mikhail A.; Ivanova, Valeria T.
      Russian Chemical Reviews (2020), 89 (10), 1115-1131CODEN: RCRVAB; ISSN:0036-021X. (IOP Publishing Ltd.)
      The sorption properties of polymers with a polyconjugated chain structure (polyaniline and polypyrrole) are considered. The mol. mechanism of sorption by these polymers of various compds. such as heavy metal ions, toxic org. compds. and micropathogens, which are the most hazardous and stubborn contaminants in water, is discussed. The use of such sorbents to purify water from micropathogens, including bacteria and viruses, is addressed for the first time. The adsorption capacity of polyconjugated polymers for these types of contaminants, the efficiency of water treatment by these sorbents and characteristics of the currently used sorbents are analyzed. The applicability of polyaniline and polypyrrole and composites based on them as high-performance versatile sorbents for water treatment is discussed, taking into account the sorbent properties such as high stability, lack of soly., lack of toxicity and ability to be regenerated and reused.
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    13. 13
      Stejskal, J. Interaction of conducting polymers, polyaniline and polypyrrole, with organic dyes: polymer morphology control, dye adsorption and photocatalytic decomposition. Chem. Pap. 2020, 74, 1– 54,  DOI: 10.1007/s11696-019-00982-9
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      13
      Interaction of conducting polymers, polyaniline and polypyrrole, with organic dyes: polymer morphology control, dye adsorption and photocatalytic decomposition
      Stejskal, Jaroslav
      Chemical Papers (2020), 74 (1), 1-54CODEN: CHPAEG; ISSN:1336-9075. (Springer International Publishing AG)
      A review. Conducting polymers, such as polyaniline and polypyrrole, have frequently been discussed in the literature due to ease of prepn. and high application potential. These polymers have been obsd. to interact with org. dyes because of the similarity in the conjugated mol. structure of both moieties. The interaction manifests itself in three fundamental directions that have been so far treated sep. The first is represented by the cond. enhancement and morphol. control when using org. dyes as templates in polypyrrole prepn. The adsorption of dyes on conducting polymers is the second field oriented at the water pollution treatment. Finally, the photocatalytic decompn. of org. dyes aims at the similar environmental target. The last two applications do not require the presence of cond. which, on the other hand, is a key parameter of conducting polymers. The future design of advanced adsorbents, however, has to exploit both the cond. and electroactivity in the control of pollutant adsorption or degrdn. For this reason, all these interactions and their practical impact are considered in the present review.
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    14. 14
      Senguttuvan, S.; Senthilkumar, P.; Janaki, V.; Kamala-Kannan, S. Significance of conducting polyaniline based composites for the removal of dyes and heavy metals from aqueous solution and wastewaters - A review. Chemosphere 2021, 267, 129201,  DOI: 10.1016/j.chemosphere.2020.129201
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      14
      Significance of conducting polyaniline based composites for the removal of dyes and heavy metals from aqueous solution and wastewaters - A review
      Senguttuvan, S.; Senthilkumar, P.; Janaki, V.; Kamala-Kannan, S.
      Chemosphere (2021), 267 (), 129201CODEN: CMSHAF; ISSN:0045-6535. (Elsevier Ltd.)
      A review. Dyes and heavy metals pollution have become a major environmental concern worldwide. Various methods, such as advanced oxidn., biodegrdn., pptn., flocculation, ultra filtration, ion-exchange, electro-chem. degrdn. and coagulation, have been proposed for the removal of dyes and heavy metals from contaminated wastewater. Of these methods, adsorption and detoxification are considered as the most promising and economically viable. Polyaniline-based composites, a material prepd. by combining polyaniline with one or more similar or disimilar materials, have been reported as good adsorbents to remove and detoxify different groups of pollutants due to their unique phys. and chem. properties. In the last decade, several studies have reported the effective adsorption (⊂95%) of dyes and heavy metals onto polyaniline based composites. Furthermore, some polyaniline -composites reduced the adsorbed heavy metals into less toxic state. This review compiles the application of different polyaniline composites for adsorption and/or detoxifcation of dyes and heavy metals and documents composite prepn. methods, morphol. and properties of the composites, and mechanism of dyes and heavy metals adsorption. Based on the avilabile literature, this review suggests that more studies are warranted to understand the influence of various conditions and exptl. variables on dyes and heavy metals removal from wastewater and/or aq. soln.
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    15. 15
      Stejskal, J.; Sapurina, I.; Vilčáková, J.; Jurča, M.; Trchová, M.; Kolská, Z.; Prokeš, J.; Křivka, I. One-pot preparation of conducting melamine/polypyrrole/magnetite ferrosponge. ACS Appl. Polym. Mater. 2021, 3, 1107– 1115,  DOI: 10.1021/acsapm.0c01331
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      15
      One-Pot Preparation of Conducting Melamine/Polypyrrole/Magnetite Ferrosponge
      Stejskal, Jaroslav; Sapurina, Irina; Vilcakova, Jarmila; Jurca, Marek; Trchova, Miroslava; Kolska, Zdenka; Prokes, Jan; Krivka, Ivo
      ACS Applied Polymer Materials (2021), 3 (2), 1107-1115CODEN: AAPMCD; ISSN:2637-6105. (American Chemical Society)
      Polypyrrole was deposited in situ on the macroporous open-cell melamine sponge by the oxidn. of pyrrole with iron(III) chloride. The oxidant was used in excess, and the reaction mixt. after the polymn. thus contained both iron(II) and iron(III) chlorides. These subsequently provided magnetite after treatment with ammonia soln. The conducting melamine/polypyrrole produced in the first step thus afforded melamine/polypyrrole/magnetite ferrosponge in the second. The composite sponge was characterized with respect to mol. structure by FTIR spectroscopy. The dependence of cond. on the sponge compression is provided and magnetic properties have also been detd. The performance of sponge in electromagnetic radiation shielding in GHz region is demonstrated. While conducting polypyrrole afforded the radiation reflection, magnetite added the absorption component.
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    16. 16
      Li, X.; Sun, Q.; Kan, Y.; Zhu, Y.; Pang, Z.; Li, M.; Jin, Y. Self-powered humidity sensor based on polypyrrole/melamine aerogel for real-time humidity monitoring. IEEE Sensor J. 2021, 21, 2604– 2609,  DOI: 10.1109/jsen.2020.3027743
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      16
      Self-powered humidity sensor based on polypyrrole/melamine aerogel for real-time humidity monitoring
      Li, Xiaoqiang; Sun, Qian; Kan, Yan; Zhu, Yanan; Pang, Zengyuan; Li, Mengjuan; Jin, Yang
      IEEE Sensors Journal (2021), 21 (3), 2604-2609CODEN: ISJEAZ; ISSN:1558-1748. (Institute of Electrical and Electronics Engineers)
      Measuring or monitoring air humidity is an increasing demands in the various fields. In this work, a simple and convenient method was utilized to prep. a melamine aerogel (MA) based sensor for humidity measurement. The sensing material was made from polymn. of polypyrrole (PPy) in the matrix of MA. The surface morphol. was characterized by SEM (SEM) to examine the inner structure of the sensing material. MA was chosen as the substrate owing to the porous structure, which facilities the adsorption of water mols. from the air. The self-powered humidity sensor was manufd. by adhering conductive tapes on both side of PPy modified MA (PPy@MA). The sensor has a flexible, ultralight and ultraporous structure, and could generate humidity-induced open-circuit voltage from the concn. gradient of the H+ ions. The PPy@MA sensor exhibited the response and recovery time of 1.1 s and 4.5 s, resp., when it is used for sensing the flowing wet air (RH 75 %). Furthermore, the sensitivity of the self-powered humidity sensor was evaluated by assessing the moisture changes of the human skin, and the moisture from the human breath.
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    17. 17
      Wu, X.; Lei, Y.; Li, S.; Huang, J.; Teng, L.; Chen, Z.; Lai, Y. Photothermal and Joule heating-assisted thermal management sponge for efficient cleanup of highly viscous crude oil. J. Hazard. Mater. 2021, 403, 124090,  DOI: 10.1016/j.jhazmat.2020.124090
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      17
      Photothermal and Joule heating-assisted thermal management sponge for efficient cleanup of highly viscous crude oil
      Wu, Xingwang; Lei, Yonggang; Li, Shuhui; Huang, Jianying; Teng, Lin; Chen, Zhong; Lai, Yuekun
      Journal of Hazardous Materials (2021), 403 (), 124090CODEN: JHMAD9; ISSN:0304-3894. (Elsevier B.V.)
      Fast and efficient cleanup of high-viscosity oil spills on the sea is still a global challenge today. Traditional recycling methods are either energy demanding or inefficient. Hydrophobic/oleophilic sorbents are promising candidates to handle oil spills, but they have limited ability to recover high viscosity oil. In this work, we report a superhydrophobic/oleophilic carbon nanotubes (CNT) and polypyrrole (PPy) coated melamine sponge (m-CNT/PPy@MS). The CNT/PPy coating enables the sponge to convert light and electricity to heat, ensuring that the absorbent can adapt to various working environments. The rapid heat generation on the sponge surface can significantly reduce the viscosity of crude oil and accelerate the absorption rate, thereby achieving the purpose of rapid recovery of oil spills. Under one sun illumination (1.0 kW/m2) and an applied voltage (8 V), the surface temp. of the m-CNT/PPy@MS can reach 118.6°C. The complete penetration time of oil droplets is 93.5% less than that of an unheated sponge. In addn., under half sun irradn. intensity and 11 V, the porous sponge absorbed 6.92 kg/m2 of crude oil in the first minute, which is about 31 times as much as that of an unheated sponge. Finally, we demonstrate a continuous absorption system, consisting of a self-heating m-CNT/PPy@MS and peristaltic pump, that can continuously recover oil spills on the sea surface. In view of its unique design, lower cost and fast oil absorption speed, this work provides a new option to tackle large-scale oil spill disasters on the sea surface.
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    18. 18
      Mahmud, H. N. M. E.; Huq, A. K. O.; Yahya, R. B. The removal of heavy metal ions from wastewater/aqueous solution using polypyrrole-based adsorbents: a review. RSC Adv. 2016, 6, 14778– 14791,  DOI: 10.1039/c5ra24358k
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      Qin, C.; Yue, Z.; Chao, Y.; Forster, R. J.; Maolmhuaidh, F. Ó.; Huang, X.-F.; Beirne, S.; Wallace, G. G.; Chen, J. Bipolar electroactive conducting polymers for wireless cell stimulation. Appl. Mater. Today 2020, 21, 100804,  DOI: 10.1016/j.apmt.2020.100804
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      There is no corresponding record for this reference.
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      Sapurina, I.; Riede, A.; Stejskal, J. In-situ polymerized polyaniline films. Synth. Met. 2001, 123, 503– 507,  DOI: 10.1016/s0379-6779(01)00349-6
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      In-situ polymerized polyaniline films 3. Film formation
      Sapurina, I.; Riede, A.; Stejskal, J.
      Synthetic Metals (2001), 123 (3), 503-507CODEN: SYMEDZ; ISSN:0379-6779. (Elsevier Science S.A.)
      Polyaniline films were produced on a glass surface immersed in the reaction mixt. during the oxidative polymn. of aniline. Glass supports placed in the reaction mixt. at the start of the oxidn. were gradually removed during the reaction. The thickness of the films produced on glass, assessed by optical absorption, was followed as a function of reaction time. The progress of polymn. was monitored by temp. changes. In another expt., glass supports were successively inserted into the polymn. mixt. The formation of polyaniline films on glass precoated with polyaniline was also investigated. A proposed model of film formation is based on the concept of primary and secondary nucleation. Oligoaniline cation radicals adsorbed on the glass surface nucleate the primary growth of polyaniline film, and the secondary nucleation occurs on the produced polyaniline layer.
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    21. 21
      Stejskal, J.; Sapurina, I. Polyaniline: thin films and colloidal dispersions (IUPAC technical report). Pure Appl. Chem. 2005, 77, 815– 826,  DOI: 10.1351/pac200577050815
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      Polyaniline: Thin films and colloidal dispersions
      Stejskal, Jaroslav; Sapurina, Irina
      Pure and Applied Chemistry (2005), 77 (5), 815-826CODEN: PACHAS; ISSN:0033-4545. (International Union of Pure and Applied Chemistry)
      Several workers from various institutions in six countries have prepd. thin films and colloidal polyaniline dispersions. The films were produced in situ on glass supports during the oxidn. of anilinium chloride with ammonium peroxydisulfate in water. The av. thickness of the films, assessed by optical absorption, was 125 ± 9 nm, and the cond. of films was 2.6 ± 0.7 S cm-1. Films prepd. in 1 mol l-1 HCl had a similar thickness, 109 ± 10 nm, but a higher cond., 18.8 ± 7.1 S cm-1. Colloidal polyaniline particles stabilized with a water-sol. polymer, poly(N-vinylpyrrolidone) [poly(1-vinylpyrrolidone-2-one)], have been prepd. by dispersion polymn. The av. particle size, 241 ± 50 nm, and polydispersity, 0.26 ± 0.12, have been detd. by dynamic light scattering. The prepn. of these two supramol. polyaniline forms was found to be well reproducible.
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    22. 22
      Xue, S.; Yin, G. Proton exchange membranes based on modified sulfonated poly(ether ether ketone) membranes with chemically in situ polymerized polypyrrole. Electrochim. Acta 2006, 52, 847– 853,  DOI: 10.1016/j.electacta.2006.06.019
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      22
      Proton exchange membranes based on modified sulfonated poly(ether ether ketone) membranes with chemically in situ polymerized polypyrrole
      Xue, Song; Yin, Geping
      Electrochimica Acta (2006), 52 (3), 847-853CODEN: ELCAAV; ISSN:0013-4686. (Elsevier B.V.)
      Sulfonated poly(ether ether ketone) (SPEEK) membranes were modified with chem. in situ polymd. polypyrrole (PPy). The effects of temp. and methanol concn. on the soln. uptake and the swelling ratio of SPEEK/PPy membranes were investigated. The soln. uptake and the swelling ratio of the membranes decreased upon the incorporation of PPy. When the methanol concn. increased, both the soln. uptake and the swelling ratio increased to a max., and then decreased. FT-IR, XRD, DSC and TGA were used to characterize the modified membranes. The methanol permeability of modified SPEEK membranes decreased upon the incorporation of PPy, and higher selectivity values were found for SPEEK/PPy membranes in comparison with pure SPEEK and Nafion 117 membranes.
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    23. 23
      Stejskal, J.; Kratochvíl, P.; Helmstedt, M. Polyaniline dispersions. 5. Poly(vinyl alcohol) and poly(N-vinylpyrrolidone) as steric stabilizers. Langmuir 1996, 12, 3389– 3392,  DOI: 10.1021/la9506483
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      23
      Polyaniline Dispersions. 5. Poly(vinyl alcohol) and Poly(N-vinylpyrrolidone) as Steric Stabilizers
      Stejskal, Jaroslav; Kratochvil, Pavel; Helmstedt, Martin
      Langmuir (1996), 12 (14), 3389-3392CODEN: LANGD5; ISSN:0743-7463. (American Chemical Society)
      When the oxidative polymn. of aniline proceeds in the presence of poly(vinyl alc.) or poly(N-vinylpyrrolidone), sterically-stabilized polyaniline dispersions are obtained. The particles have an av. diam. of about 300-600 nm as detd. by dynamic light scattering. The yield of polyaniline in dispersion form often decreased if the reaction mixt. was stirred during polymn. and dispersions were then accompanied by a macroscopic ppt. Poly(N-vinylpyrrolidone) is a more efficient stabilizer compared to poly(vinyl alc.). Microstructured composites, which contain up to ∼70 wt % of elec.-conducting polyaniline dispersed in an insulating matrix, can be prepd. from these dispersions.
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    24. 24
      Riede, A.; Helmstedt, M.; Sapurina, I.; Stejskal, J. In situ polymerized polyaniline films. J. Colloid Interface Sci. 2002, 248, 413– 418,  DOI: 10.1006/jcis.2001.8197
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      24
      In Situ Polymerized Polyaniline Films
      Riede, Andrea; Helmstedt, Martin; Sapurina, Irina; Stejskal, Jaroslav
      Journal of Colloid and Interface Science (2002), 248 (2), 413-418CODEN: JCISA5; ISSN:0021-9797. (Academic Press)
      Polyaniline films were grown on glass supports during dispersion polymns. of aniline using poly(N-vinylpyrrolidone) and hydroxypropyl cellulose as stabilizers. The initiation of polyaniline chains is proposed to be heterogeneously catalyzed by the surfaces immersed in the reaction mixt. Film formations in dispersion and pptn. polymns. are compared. Surfometry and optical absorption were used to assess the submicrometer film thickness, and FTIR spectroscopy was used to analyze the chem. structure of films and prove the absence of stabilizer. The film thickness was proportional to the dimensions of simultaneously produced colloidal polyaniline particles. The cond. of films increased with increasing film thickness. (c) 2002 Academic Press.
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    25. 25
      Mezhuev, Y. O.; Artyukhov, A. A.; Piskareva, A. I.; Shtil’man, M. I.; Gol’din, M. M.; Korshak, Y. V.; Solov’eva, I. V.; Evseev, A. K. Synthesis of aqueous polypyrrole dispersions stabilized with polyvinyl alcohol and preparation of hemocompatible films based on them. Russ. J. Appl. Chem. 2015, 88, 1026– 1032,  DOI: 10.1134/s107042721506021x
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      25
      Synthesis of aqueous polypyrrole dispersions stabilized with polyvinyl alcohol and preparation of hemocompatible films based on them
      Mezhuev, Ya. O.; Artyukhov, A. A.; Piskareva, A. I.; Shtil'man, M. I.; Gol'din, M. M.; Korshak, Yu. V.; Solov'eva, I. V.; Evseev, A. K.
      Russian Journal of Applied Chemistry (2015), 88 (6), 1026-1032CODEN: RJACEO; ISSN:1070-4272. (Pleiades Publishing, Ltd.)
      Stabilized polypyrrole dispersions were prepd. by oxidative polymn. of pyrrole in aq. soln. of polyvinyl alc. The influence of the concn. and mol. mass of polyvinyl alc. in the reaction mixt. on the size of the particles formed was examd., and the particle structure was detd. The possibility of prepg. hemocompatible films from aq. polypyrrole dispersions stabilized with polyvinyl alc. was demonstrated.
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    26. 26
      Stejskal, J.; Kratochvíl, P.; Armes, S. P.; Lascelles, S. F.; Riede, A.; Helmstedt, M.; Prokeš, J.; Křivka, I. Polyaniline dispersions. 6. Stabilization by colloidal silica particles. Macromolecules 1996, 29, 6814– 6819,  DOI: 10.1021/ma9603903
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      Polyaniline dispersions. 6. Stabilization by colloidal silica particles
      Stejskal, Jaroslav; Kratochvil, Pavel; Armes, Steven P.; Lascelles, Stuart F.; Riede, Andrea; Helmstedt, Martin; Prokes, Jan; Krivka, Ivo
      Macromolecules (1996), 29 (21), 6814-6819CODEN: MAMOBX; ISSN:0024-9297. (American Chemical Society)
      Aniline was polymd. in the presence of ultrafine colloidal silica particles (hydrodynamic diam. 35 nm) in aq. media and, given a sufficient silica concn., colloidally stable polyaniline-silica particles were obtained. The particle size of the resulting dispersions was detd. by both dynamic light scattering and disk centrifuge photosedimentometry. The typical size of these polyaniline-silica particles is in the range 300-600 nm and is insensitive to the concn. of components in the reaction mixt., temp., or acidity of the reaction mixt. Particles produced at 0° are spherical and their shape becomes less defined when polymn. proceeds at 25°. As the silica size is increased, the composite particles become larger and their raspberry morphol. more distinct. The elec. cond. of a typical polyaniline (37.8%)-silica composite is 6.1 × 10-2 S cm-1 at 25 °C. It grows with increasing temp. and does not depend on the frequency in the investigated range from 20 Hz to 1 MHz.
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      Riede, A.; Helmstedt, M.; Riede, V.; Zemek, J.; Stejskal, J. In situ polymerized polyaniline films. 2. Dispersion polymerization of aniline in the presence of colloidal silica. Langmuir 2000, 16, 6240– 6244,  DOI: 10.1021/la991414c
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      27
      In situ polymerized polyaniline films. 2. Dispersion polymerization of aniline in the presence of colloidal silica
      Riede, A.; Helmstedt, M.; Riede, V.; Zemek, J.; Stejskal, J.
      Langmuir (2000), 16 (15), 6240-6244CODEN: LANGD5; ISSN:0743-7463. (American Chemical Society)
      Composite polyaniline-silica films produced on glass surfaces during the dispersion polymn. of aniline in the presence of colloidal silica were investigated. The film morphol. and compn. were characterized by FTIR, UV-visible, and X-ray photoelectron spectroscopies. Compared with pure polyaniline films produced under similar conditions, the composite films are thinner and smoother, and their surface is silica-rich. The film thickness of both pure and composite films decreased as the polymn. temp. increased from 0 to 50 °C. To det. the particle size of polyaniline-silica dispersion particles, which are formed at the same time as the films, dynamic light scattering was used. The correlation between the particle size and film thickness is discussed. The elec. cond. of composite polyaniline films was only a little affected by the presence of silica.
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    28. 28
      Roosz, N.; Euvard, M.; Lakard, B.; Buron, C. C.; Martin, N.; Viau, L. Synthesis and characterization of polyaniline-silica composites: raspberry vs core-shell structures. Where do we stand?. J. Colloid Interface Sci. 2017, 502, 184– 192,  DOI: 10.1016/j.jcis.2017.04.092
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      28
      Synthesis and characterization of polyaniline-silica composites: Raspberry vs. core-shell structures. Where do we stand?
      Roosz, Nicolas; Euvard, Myriam; Lakard, Boris; Buron, Cedric C.; Martin, Nicolas; Viau, Lydie
      Journal of Colloid and Interface Science (2017), 502 (), 184-192CODEN: JCISA5; ISSN:0021-9797. (Elsevier B.V.)
      The synthesis of polyaniline-silica composites has been reinvestigated in view of the opposing results found in the literature. Firstly, we synthesized silica particles with tunable size using the Stober process. These silica particles have been fully characterized before being used as solid support for the polymn. of aniline. This polymn. was performed according to a published procedure where the pH of the reaction mixt. was below the pKa of aniline but at a value where the silica particles surface was still slightly neg. charged. The objective of this procedure was to favor electrostatic interactions between anilinium cations and the silica surface to lead to the formation of silica-polyaniline core-shell particles. Several sets of nanocomposites were prepd. under different exptl. conditions (oxidant/aniline ratio, silica concn., temp., silica particles diams.). The study evidenced that under all the conditions used the formation of core-shell nanoparticles is impossible. However, using different particle sizes, noticeable morphol. differences were obsd. The use of large silica particles led to the formation of non-uniform polyaniline-silica composites whereas the use of smaller particles always led to raspberry-like morphol. as reported by other groups in highly acidic media. The difference in morphol. led to different elec. properties with elec. conductivities measured at room temp. ranging from 1 .6× 10-3 to 2.5 × 10-5 S cm-1.
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    29. 29
      Wen, P.; Wang, Y.; Wang, N.; Zhang, S.; Peng, B.; Deng, Z. Preparation and characterization of melamine-formaldehyde/Ag composite microspheres with surface-enhanced Raman scattering and antibacterial activities. J. Colloid Interface Sci. 2018, 531, 544– 554,  DOI: 10.1016/j.jcis.2018.07.014
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      29
      Preparation and characterization of melamine-formaldehyde/Ag composite microspheres with surface-enhanced Raman scattering and antibacterial activities
      Wen, Peihua; Wang, Yadong; Wang, Ni; Zhang, Shengwen; Peng, Bo; Deng, Ziwei
      Journal of Colloid and Interface Science (2018), 531 (), 544-554CODEN: JCISA5; ISSN:0021-9797. (Elsevier B.V.)
      A facile and environmentally friendly approach was proposed to decorate Ag nanoparticles on melamine-formaldehyde (MF) colloidal particles (MF/Ag composite microspheres). In this approach, monodisperse MF colloidal particles were prepd. via a two-step org. sol-gel process and served as the active templates for the decoration of Ag nanoparticles. Then, the [Ag(NH3)2]+ ions as the Ag precursors can be adsorbed onto the surfaces of the MF colloidal particles and were in situ reduced into metallic Ag nanoparticles, forming MF/Ag composite microspheres. During this synthesis, neither presurface activation nor extra reductants were necessary. These MF/Ag composite microspheres can be used as the surface-enhanced Raman scattering (SERS) active substrates for the trace detection of org. compds., e.g., 4-aminobenzenethiol (4-ABT) and penicillin G sodium. Furthermore, these MF/Ag composite microspheres also showed excellent antibacterial activities against both Escherichia coli (E. coli, gram-neg. bacteria) and Staphylococcus aureus (S. aureus, gram-pos. bacteria).
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    30. 30
      da Silva, F. A. G.; Vieira, S. A.; Botton, S. D.; da Costa, M. M.; de Oliveira, H. P. Antibacterial activity of polypyrrole based nanocomposites: a mini-review. Polim.: Cienc. Tecnol. 2020, 30, e2020048  DOI: 10.1590/0104-1428.08020
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    31. 31
      Maráková, N.; Humpolíček, P.; Kašpárková, V.; Capáková, Z.; Martinková, L.; Bober, P.; Trchová, M.; Stejskal, J. Antimicrobial activity and cytotoxicity of cotton fabric coated with conducting polymers, polyaniline or polypyrrole, and with deposited silver nanoparticles. Appl. Surf. Sci. 2017, 396, 169– 176,  DOI: 10.1016/j.apsusc.2016.11.024
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      31
      Antimicrobial activity and cytotoxicity of cotton fabric coated with conducting polymers, polyaniline or polypyrrole, and with deposited silver nanoparticles
      Marakova, Nela; Humpolicek, Petr; Kasparkova, Vera; Capakova, Zdenka; Martinkova, Lenka; Bober, Patrycja; Trchova, Miroslava; Stejskal, Jaroslav
      Applied Surface Science (2017), 396 (), 169-176CODEN: ASUSEE; ISSN:0169-4332. (Elsevier B.V.)
      Cotton fabric was coated with conducting polymers, polyaniline or polypyrrole, in situ during the oxidn. of resp. monomers. Raman and FTIR spectra proved the complete coating of substrates. Polypyrrole content was 19.3 wt.% and that of polyaniline 6.0 wt.%. Silver nanoparticles were deposited from silver nitrate solns. of various concns. by exploiting the redn. ability of conducting polymers. The content of silver was up to 11 wt.% on polypyrrole and 4 wt.% on polyaniline. The sheet resistivity of fabrics was detd. The cond. was reduced after deposition of silver. The chem. cleaning reduced the cond. by less than one order of magnitude for polypyrrole coating, while for polyaniline the decrease was more pronounced. The good antibacterial activity against S. aureus and E. coli and low cytotoxicity of polypyrrole-coated cotton, both with and without deposited silver nanoparticles, were recorded, and they promise a broad applicability of this material. Polyaniline-coated samples showed lower antibacterial activity and higher cytotoxicity compared to polypyrrole-based materials.
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