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Review on Template Removal Techniques for Synthesis of Mesoporous Silica Materials
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Review on Template Removal Techniques for Synthesis of Mesoporous Silica Materials
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Energy & Fuels

Cite this: Energy Fuels 2022, 36, 5, 2424–2446
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https://doi.org/10.1021/acs.energyfuels.1c04435
Published February 19, 2022

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Abstract

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The key step in the preparation of mesoporous silica materials is the removal of organic templates occluded inside the pores including nonionic, cationic, anionic surfactants and even ionic liquid (IL). The most common method to remove templates is conventional calcination under air at 550 °C. Although templates can be completely removed from the pores, calcination suffers many serious drawbacks including significant framework shrinkage, the collapse of the ordered structure, reduction of silanol concentrations on the pore wall (which are of high importance for postmodification), generation of large amounts of CO2 and organic amine compounds, the presence of carbon deposits or coke as a contaminant, elimination of organic functionalities (such as organoalkoxysilanes with amino groups), and the inability to recover or reuse expensive organic templates. That is why many attempts have been reported in the literature to develop novel methods for removing organic templates that are favorable from both economic and environmental standpoints for potentially large-scale applications. The current study reviews the recent development methods for template removal from various types of mesoporous silica materials. We have divided the template removal approaches into two categories: physical method and chemical method. The effects of those methods are discussed in detail on the textural and structural properties of mesoporous silica materials along with the template removal mechanism and their pores and coins.

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1. Introduction

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Mesoporous silica materials, for instance, the SBA (Santa Barbara Amorphous) series, MCM (Mobil Composition of Matter) series, and KIT (Korean Advanced Institute of Science and Technology) series have gained extensive attention over the last decades due to their highly tunable textural and chemical characteristics and are therefore used in different fields: biomedical and pharmaceutical applications, (1−3) adsorption of pollutants from wastewater, (4,5) catalysis, (6−9) aromatization, (10) biogas purification and upgrading, (11) sensing, (12) desulfurization, (13−20) for CO2 capture, (21−27) Li-ion battery application, (28) upgrading microalgal biocrude, (29) hydrodenitrogenation, (30) and hydrogen production. (31,32)Figure 1(a) displays the number of publications for mesoporous silica materials, and Figure 1(b) shows their applications in different research areas from 2000 to 2021 (Web of Science). Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (P123 copolymer), poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (pluronic F-127) as nonionic surfactants, cetyltrimethylammonium bromide (CTABr), and cetyltriethylammonium bromide (CTEABr) as cationic surfactants, and anionic surfactants such as sodium dodecyl benzenesulfonate (SDBS) and sodium dodecyl sulfate (SDS) as well as ionic liquid (IL) are the common organic templates used for the synthesis of mesoporous silica materials. The elimination of these templates from the pores is a crucial step in the synthesis of mesoporous silica materials. Thermal calcination is a common method for template removal in the laboratory due to high efficiency, easy operation, and required simple equipment. The significant reduction of silanol concentrations happens during calcination (which renders the sample unsuitable for postmodification), and accordingly, the structural shrinkage is invariably detected following template removal. Also, the recovery or reuse of expensive templates is not possible due to burning out of the template which results in CO2 and hazardous gas emissions that are both economically and environmentally unfavorable. Furthermore, calcination burns off not only the template but also the functional groups when the mesoporous silica materials are modified via a co-condensation method with functional groups. Therefore, alternate detemplating procedures to calcination are needed, and more recent attention has focused on new technologies and methods offering superior template removal performance. To the best of our knowledge, this is the first study to review the latest developed methods for template removal including chemical methods such as solvent extraction, chemical oxidation, and ionic liquid (IL) treatment and physical methods such as calcination, supercritical CO2 (SC–CO2), microwave-assisted treatment, ultrasonic-assisted treatment, ozone treatment, and plasma technology. This review paves the way for researchers to get more information about these developed methods by weighing their benefits and drawbacks before developing and designing new template removal methods. Therefore, in this current study, the methods for the elimination of templates from mesoporous silica materials will be comprehensively reviewed, and finally a new, green, and efficient method will be proposed for template removal.

Figure 1

Figure 1. (a) Number of publications for mesoporous silica materials from 2000 to 2021. (b) Applications of mesoporous silica materials in different research fields published on the Web of Science with the keyword of “mesoporous silica material” (accessed December 25, 2021).

2. Template Removal Approaches

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Several template removal methods have been reported in the literature. We have categorized these methods into physical and chemical methods. The physical methods are calcination, supercritical fluid, ozone treatment, microwave-assisted treatment, ultrasonic-assisted treatment, and plasma technology. The chemical methods are solvent extraction, chemical oxidation, and ionic liquid (IL) treatment.

2.1. Physical Methods

2.1.1. Calcination

Calcination in air is a common method and is widely used for template removal from pores. (33) Basso et al. (34) investigated the influence of calcination conditions (temperature and time) on the carbon content, silanol groups, and physical properties of SBA-15 and KIT-6. As shown in Figure 2, at 300 °C, the remaining carbon contents were 0.32% and 19% for SBA-15 and 0.42% and 0.30% for KIT-6 after 300 and 600 min, respectively. By increasing temperature to 400 and 500 °C, less of a difference in the amount of carbon was observed for both SBA-15 and KIT-6. Also, it can be seen that increasing the calcination time to 10 h at higher temperatures did not have a substantial effect on the removal of organic material. However, increasing the calcination period from 300 to 600 min resulted in a significant change in the carbon percent of SBA-15 at 300 °C, while residual carbon remained almost the same by increasing the calcination time from 300 to 600 min at a temperature more than 300 °C. Table 1 presents the physical properties of SBA-15 at various temperatures and times.

Figure 2

Figure 2. Residual carbon content for calcined SBA-15 and KIT-6 at various temperatures and times. Reproduced from ref (34). [Basso, A. M.; Nicola, B. P.; Bernardo-Gusmão, K.; Pergher, S. B. C. Tunable Effect of calcination of the silanol groups of KIT-6 and SBA-15 Mesoporous Materials. Applied Sciences2020, 10 (3), 970]. Copyright 2020, MDPI.

Table 1. Physical Properties of SBA-15 and KIT-6 in Ref (34)
  SBET (m2 g–1)Pore diameter (nm)VT (cm3 g–1)Wall thickness (nm)
Temperature (°C)Time (min)SBA-15KIT-6SBA-15KIT-6SBA-15KIT-6SBA-15KIT-6
3003005726957.57.20.790.824.515.8
3006006328267.56.10.860.984.417.9
4003006419057.87.50.841.074.716.0
40060011978527.57.91.521.035.015.9
500300109911749.07.31.691.443.316.7
5006007708747.87.40.981.204.215.6
SBA-15 had the highest specific surface area (SBET) at 400 °C calcination for 10 h. The SBET decreased as the calcination temperature increased to 500 °C, even increasing calcination time at this temperature decreased slightly the SBET of SBA-15 due to the dehydroxylation of the material. The pore diameter and total pore volume (VT) followed the same trend, reaching their maximum values of 0.9 nm and 1.69 cm3 g–1, respectively, after 3000 min 500 °C. The highest wall thickness of 5.0 nm was at 400 °C for 600 min. Regarding KIT-6, the highest SBET was obtained at 500 °C for 5 h, further increasing calcination time decreased its SBET, as presented in Table 1. KIT-6 had the highest VT and wall thickness at 500 °C for 5 h, while it has the highest pore diameter at the lower temperature of 400 °C for 10 h.
Moreover, by increasing the temperature, the conversion of geminal silanols has happened to siloxane. It was found that more silanol groups are preserved at 300 °C for 300 min rather than calcination at 400 °C. Nevertheless, calcination at 300 °C resulted in a small pore volume. It was suggested that calcination at a higher temperature, for example, 600 for 300 min, is unnecessary, time consuming, and a waste of silanol groups. Although the template is completely removed through calcination, there are some concerns with using this conventional method. The expensive organic template cannot be recovered after calcination. A high temperature and a long time are required to eliminate the template. During calcination, terrible smells, toxic and noxious gases, are produced leading to environmental pollution. Preserving large numbers of surface silanol groups is essential to functionalize the mesoporous siliceous materials for the desired application. During the calcination, the number of surface silanol groups reduces because of the dehydroxylation at higher temperatures for a prolonged time, and a significant structural shrinkage is observed resulting in the destruction of microporosity. (35,36) Moreover, calcination is not recommended if the material is functionalized with a less stable organic part because it might be eliminated together with the template.
Calcination was assisted by catalytic template treatment. Catalytic template removal is a fascinating technique in which metal acts as a catalyst for the oxidative elimination of the surfactant molecules during the calcination process. The calcination temperature in this process is less than the usual calcination temperature. The metals are injected in one step, as shown in Figure 3, or separately through impregnation. This technique has the benefit of lowering the calcination temperature substantially. This method was employed by Krawiec et al. (37) to prepare Pt/MC-41 and Pt/SBA-15. The calcination temperature and time were 450 °C and 5 h. They reported that Pt incorporation into SBA-15 pores was less successful in comparison to MCM-41 due to the long time required for the synthesis of SBA-15 (28 h). Indeed, during the long time synthesis, the diffusion of the metal precursor happened from the toluene to the mixture of ethanol–water resulting from TEOS hydrolysis. The surface area of sample 1 wt % Pt/SBA-15 was 825 m2 g–1, while that of of free metal SBA-15 was 786 m2 g–1. Other metals such as Pd and V2O5 have been used in this method.

Figure 3

Figure 3. In situ preparation of Pt/mesoporous composite materials using catalytic template removal method. Reproduced from ref (37). [Krawiec, P.; Kockrick, E.; Simon, P.; Auffermann, G.; Kaskel, S. Platinum-Catalyzed Template Removal for the in Situ Synthesis of MCM-41 Supported Catalysts. Chem. Mater.2006, 18 (11), 2663–2669].Copyright 2006, American Chemical Society.

The remaining trace of carbon after calcination is another disadvantage which is required further treatment, for example, in an oxygen (O2) or hydrogen (H2) stream to remove carbon on the silica surface. (38,39) Goworek et al. (40) have made efforts to remove surfactants from MCM-41 using H2 flow treatment at the temperature range from 110 to 250 °C for 15 h. The elemental analysis showed that the amounts of hydrocarbon species and nitrogen compounds are significantly reduced by increasing temperature to 250 °C as presented in Table 2. According to data in Table 2, calcined MCM-41 in O2 and MCM-41 treated in H2 flow at 250 °C exhibited almost the same SBET and VT values. The pore size distribution curves of calcined and H2-treated samples were quite narrow centered at 2.4 nm indicating high template removal efficiency of H2 flow treatment. The 29Si MAS NMR confirmed the high surface silanols content of MCM-41 treated in H2 flow at 250 °C. The gas chromatography–mass spectrometry (GC-MS) analysis showed that the retention times of aliphatic hydrocarbons for both calcined and H2 flow-treated MCM-41 are not identical due to differences in the surface properties of these materials. The collected products after H2 flow treatment were condensed and analyzed by GC-MS. The peaks observed in GC-MS were assigned to hexadecane and hexadecane-N,N-dimethylamine indicating that the structures of surfactant molecules were damaged during the H2 flow treatment only within the headgroup, and finally, the degradation products were evaporated. It was stated that the Hoffman degradation resulted in partial removal of amine groups and production of unsaturated product at a temperature below 250 °C. It might be possible to remove the remaining amount of amine compound in the MCM-41 skeleton through the burnoff process at high temperatures under oxidizing conditions. Although this method template can be removed at low temperatures, the deposition of carbon is more compared to calcination. Also, the removal time is long. The template cannot be recovered and reused, and a complex device is required.
Table 2. Elemental Analysis and Textural Properties of Calcined MCM-41 and H2-Treated MCM-41 in Ref (40)
Template removal method and conditionC (%)H (%)N (%)SBET (m2 g–1)VT (cm3 g–1)
H2 flow treatment at 110 for 15 h28.445.721.741430.22
H2 flow treatment at 150 for 15 h22.254.551.492820.29
H2 flow treatment at 200 for 15 h6.521.690.3210060.95
H2 flow treatment at 250 for 15 h3.891.250.1211691.10
Calcination in O2 at 550 for 8 h2.781.200.1111261.07

2.1.2. Supercritical CO2 (SC–CO2) Extraction

Supercritical CO2 (SC–CO2) extraction is used not only for the synthesis of adsorbent but also for template removal. The main advantage of this method is the adjustable physical and chemical properties including density, viscosity, diffusivity, and mass transfer by changing the operating pressure and temperature. For example, supercritical fluid (SCF) possesses high diffusivity and negligible surface tension, and penetration of solvent into cavities of mesoporous materials is rapid due to the gas-like viscosity of SFC. Since CO2 as a special chemical with a low critical temperature of 304.21 K and modest critical pressure of 7.38 MPa is cost effective, available, low toxic, and nonflammable, (41,42) SC–CO2 has attracted more attention of material scientists. SC–CO2 in the presence or absence of cosolvents has been employed for template removal from mesoporous materials, (35,36,43−47) as shown in Figure 4. van Grieken et al. (45) extracted the nonionic surfactant from SBA-15 using SC–CO2 in the presence and absence of ethanol as a cosolvent at various pressures and temperatures ranging from 60 to 110 °C for 24 h. The results disclosed that optimum removal efficiency of 79% is obtained upon using SC–CO2 at 90 °C and 140 atm, while the efficiency is decreased to 76% by increasing temperature to 110 °C at 210 atm due to the lower density of the supercritical fluid. A higher extraction efficiency can be achieved using SC–CO2 in comparison to the ethanol extraction method with a removal efficiency of 74%. The removal of the P123 copolymer from SBA-15 was enhanced by the addition of ethanol as a cosolvent so that removal efficiency increased to 81% at 90 °C and 130 atm. The silanol group concentration on the surface of SBA-15 was evaluated using 29Si nuclear magnetic resonance (NMR) by obtaining a Q3/Q4 ratio. This ratio for calcined SBA-15 was 0.14, much lower than that of SBA-15 treated by SC–CO2 in the absence and presence of ethanol having the values of 0.48 and 0.42, respectively. This result confirms that SC–CO2 preserves more silanol groups on the surface of SBA-15 compared to calcination. Finding optimum experimental conditions is important which was not considered in the experimental conditions reported by van Grieken et al. (45) It seems that temperature, pressure, extraction time, and type of cosolvent (if used) and flow rates of liquid CO2 and cosolvent (if used) are the main factors affecting the template removal efficiency, as reported in the literature. (35,43,46,47) When SC–CO2 was employed without adding cosolvents, the cationic surfactant was not removed from MCM-41, (44) while van Grieken et al. (45) observed that SC–CO2 alone was successful in removing the P123 copolymer from SBA-15 with a high removal efficiency, despite the extended reaction time (24 h).

Figure 4

Figure 4. Schematic of SC–CO2 extraction technique.

The extracted organic template can be recovered and reused at the end of the process. It should be mentioned again that adding cosolvent can increase the template removal efficiency compared to SC–CO2 alone because adding cosolvents can improve the solvating strength of SC–CO2. The supercritical conditions can facilitate the transfer and desorption of templates through the inner and outer diffusion in the mesopores of materials due to SC–CO2’s low viscosity and high diffusivity properties. Huang and co-workers (35,36) used methanol-modified SC–CO2 to extract cationic surfactant templates such as CTABr from MCM-41, MCM-48, and SBA-3 and cetyltriethylammonium bromide (CTEABr) from SBA-1. Their results showed the highest template removal efficiency of 95% for as-synthesized SBA-3 followed by as-synthesized MCM-48, SBA-1, and MCM-41 with efficiencies of 93%, 88%, and 78%, respectively. However, the destruction of the mesoporous framework of as-synthesized MCM-48 happened after template removal. They employed a curing treatment under vacuum for 14 h to improve the mesoporous structural stability of materials. Although cured as-synthesized materials had better ordered mesoporous structures and were stable after template removal, the template removal efficiency was reduced. Overall, it is not easy to carry out SC–CO2 because of equipment limitations and difficulty in achieving the appropriate temperature, pressure, and CO2 flow speed. (48)

2.1.3. Microwave-Assisted Treatment

Figure 5(a) illustrates a schematic of microwave-assisted treatment. Tian et al. (49) used microwave digestion to remove the template from SBA-15 and MCM-41. The sample was mixed with nitric acid (HNO3) and hydrogen peroxide (H2O2) and placed in a reactor. These chemicals are utilized in the chemical oxidation process for template removal, which is discussed later. The oxidation of the template by HNO3 and H2O2 is facilitated by the instantaneous high temperature (∼200 °C) and pressure (∼1.3 MPa) created by microwave radiation. The template in SBA-15 was completely removed within 2–3 min and confirmed by Fourier transform infrared spectroscopy (FT-IR) results. Also, the relative intensity of Si–OH bending bands at around 960 cm–1 was higher for SBA-15 treated by this method than calcined SBA-15. It suggests that microwave digestion-assisted treatment can preserve more silanol groups on the pore wall surface in comparison to calcination. Lai et al. (50) used microwave-assisted treatment to eliminate the template from the pores of as-synthesized SBA-15. The sample was mixed with 20 mL of ethanol/hexane (V/V, 1/1) as extract solvents and put on a watch glass, then heated for 2 min by microwave irradiation. The process for template removal was repeated three times. The obtained results were the same as those reported by Tian et al. (49) suggesting the effectiveness of this method in template removal. Chen et al. (48) used a combination of H2O2 treatment and a microwave to eliminate the template from SBA-15 and MCM-41. The process was catalyzed by Fe (NO3)3·9H2O or Cr (NO3)3·9H2O based on the Fenton reaction. Their results showed that the d-spacing values and the unit cell parameters (a0) of SBA-15 and MCM-41 treated by this method were the same as the as-synthesized samples, while larger than those of the calcined SBA-15 and MCM-41 demonstrating that the shrinkage of the textural framework was significantly reduced using this method compared to calcination. As Fe (NO3)3·9H2O was used as a Fenton reagent, SBA-15 has better pore properties. However, MCM-41 exhibited better textural parameters as Cr (NO3)3·9H2O was used as Fenton reagent. Figure 5(b) shows the proposed mechanism for template removal. There was a stronger interaction between Fe(III) and anionic silicate species (I) due to higher coordination ability Fe(III) compared to Cr(III); therefore, removal of the cationic surfactant (S+) from the MCM-41 system was not efficient. Moreover, trimethylamine species were produced by the decomposition of cationic surfactant CTABr (S+I) resulting in the activity loss of Fe(III) and Cr(III). That is why the cationic template was removed from MCM-41 in the presence of the Cr–H2O2 reagent. The H+ groups were significant in the removal of nonionic surfactant (S0) from SBA-15 in, as well as inhabiting, the interaction between Fe(III) and cationic silicate species (I+); As a result, employing Fe–H2O2 reagents, nonionic surfactant (S0) was efficiently removed from SBA-15.

Figure 5

Figure 5. (a) Schematic of microwave-assisted treatment. (b) Possible mechanism for template removal from MCM-41 and SBA-15 using H2O2 treatment assisted by microwave. Reproduced from ref (48). [Chen, L.; Jiang, S.; Wang, R.; Zhang, Z.; Qiu, S. A novel, efficient and facile method for the template removal from mesoporous materials. Chemical Research in Chinese Universities2014, 30 (6), 894–899]. Copyright 2014, Springer.

Although the microwave-assisted treatment has some advantages such as efficient and quick elimination of the organic template, less shrinkage of the framework, and less energy consumption, it suffers several drawbacks including difficulty in controlling the conditions of the microwave-assisted treatment in the case of some mesoporous materials, emission of CO2 and toxic gases at the end of process due to the decomposition of surfactant, using solvents for assisting the process, and inability to recover or reuse the surfactant. (51,52)

2.1.4. Ultrasonic-Assisted Treatment

The ultrasonic technique is the well-defined process based on sonochemistry principles in which molecules undergo a chemical reaction owing to the application of powerful ultrasound irradiation (20 kHz–10 MHz). (53,54) Essentially, there is no chemical reaction during the direct interaction of ultrasonic radiation with the molecules; however, when ultrasonic radiation interacts with liquid, an alternating pattern of pressures is developed. Indeed, the acoustic cavitation (process of bubble formation, growth, and collapse under altering pressure) happens due to the interaction of ultrasonic radiation with the liquids and release of the accumulated ultrasonic energy in the bubbles producing energy with a very high local temperature of 5000 K and pressure of 1000 bar in few microseconds, (55−59) as shown in Figure 6(a).

Figure 6

Figure 6. (a) Generation of acoustic bubbles by ultrasonic irradiation. (b) Schematic of ultrasonic-assisted treatment.

Figure 6(b) depicts a schematic of ultrasonic-assisted treatment. This method has been utilized for template elimination from the pores of mesoporous materials. The ultrasonic treatment was used for detemplating MCM-41 by Jabariyan and Zanjanchi (60,61) for the first time and later by Pirez et al. (62) for template removal from SBA-15 and propylsulfonic acid (PrSO3H)-functionalized SBA-15.
Jabariyan and Zanjanchi (60) have optimized the template removal conditions assisted by ethanol such as sonication time and temperature. The results disclosed that the SBET and VT values increased as the sonication time and temperature increased within the studied ranges. Longer sonication time resulted in a slight reduction of SBET thanks to the slight destruction to the mesoporous structure of MCM-41. At the temperature of 60 °C and sonication time of 30 min, MCM-41 exhibited a higher SBET of 1325 m2 g–1 and VT of 0.471 cm3 g–1 than calcined MCM-41 possessing the SBET and VT of 1276 m2 g–1 and 0.454 cm3 g–1, respectively. This confirms the efficiency of this method for the template removal from as-synthesized MCM-41.
Ultrasonication was shown to be an effective technique for removing P123 from PrSO3H-SBA-15 by Pirez et al. (62) However, in the case of virgin SBA-15, there was a great difference between the P123 percentage removed by ultrasonic irradiation and reflux extraction. As shown in Table 3, ultrasonication was ineffective in removing the template from the synthesized SBA-15 in methanol, while template removal of 90% was obtained reflux extraction. This may indicate that thermal activation is required to overcome hydrogen bonding interactions between the P123 template and isolated silanol groups, or ultrasonic irradiation could be conducted at moderate temperature for example 60 °C. As reported by Jabariyan and Zanjanchi, (60) the rate of template extraction from MCM-41 is relatively fast under ultrasonic irradiation in ethanol at a temperature of 60 °C rather than 25 °C providing a higher SBET and VT.
Table 3. Template Removal from SBA-15 and PrSO3-SBA-15 in Ref (62)a
Template removal methodSolventTime (h or min)Solvent:Sample (cm3 g–1)Template removed (%)
SBA-15
Calcination98
 Toluene24 h50035
RefluxTetrahydrofuran (THF)24 h50080
RefluxAcetone24 h50076
RefluxEthanol24 h50076
RefluxMethanol24 h50080
RefluxMethanol24 h100090
UltrasonicationMethanol5 min50039
UltrasonicationMethanol30 min50045
UltrasonicationMethanol1 h50043
PrSO3-SBA-15
RefluxToluene24 h50062
RefluxTHF24 h50069
RefluxAcetone24 h50078
RefluxEthanol24 h50072
RefluxMethanol24 h50074
RefluxMethanol24 h100089
UltrasonicationMethanol5 min50089
UltrasonicationMethanol5 min10090
UltrasonicationMethanol1 h50090
a

Reflux method and ultrasonic extraction were conducted at 60 °C and room temperature, respectively.

On the other hand, the template was efficiently removed from PrSO3H-SBA-15 under ultrasonic irradiation in comparison to the solvent extraction method (as will be discussed later). As shown in Table 3, template extraction using methanol was more efficient than other studied solvents. After the second reflux with methanol, about 89% template was removed, as confirmed from Thermogravimetric analysis (TGA) between 150 and 350 °C. Using reflux for extraction of template required a long time about 24 h consuming 3600 W. Therefore, methanol was used for ultrasonic irradiation. The obtained result is interesting so that the template was efficiently removed from the pores within 5 min at room temperature using ultrasonic irradiation consuming about 3 W. Their results disclosed that ultrasonic irradiation leads to a less lattice shrinkage of PrSO3H-SBA-15 which possessed a higher a0 of 11.2 nm and the pore wall thickness of 5.1 nm in comparison to that of PrSO3H-SBA-15 treated by solvent extraction having a0 of 11 nm and the pore wall thickness of 4.9 nm. All of these findings suggest that ultrasonic-assisted treatment is an efficient method and comparable with SC–CO2 and microwave methods.
One of the notable advantages of ultrasonic-assisted treatment is that the recovery of the template is possible at the end of the template removal process. Jabariyan and Zanjanchi (60) studied the structure of the template removed from MCM-41 after sonication. Figure 7(a) displays the FT-IR spectrum of the CTABr–ethanol mixture for the sake of comparison. Figure 7(b) and (c) depicts FT-IR spectra of effluents obtained after 15 min sonication at 40 °C and 60 min sonication at 60 °C, respectively. As seen in Figure 7(a)–(c), the spectra of all samples were similar, indicating that the structure of CTABr was preserved after sonication in ethanol. In another study, (61) these authors investigated the concentration of CTABr after ultrasonic irradiation using a double-beam UV spectrophotometer. As shown in Figure 7(d), the concentration of CTABr was increased by increasing the sonication time; however, further increasing sonication time resulted in a decrease of CTABr concentration indicating that degradation of CTABr happened at longer sonication times. During ultrasonic irradiation, the surfactant molecules migrate apart from each other, causing micelle disruption in the alcohol solution. This matter was already well established in the field of drug delivery. (63−65) It was stated that ultrasonic vibrations cannot damage the hydrophobic tail of the organic template flocked in the micelle core. By acceleration of micelle disruption, they converted to monomers. The hydroxyl radicals (HO) attack these monomers through the hydrophilic head of micelles in bulk solution; consequently, their nature is changed as a monomer in the CTABr structure. Therefore, provided that only micelle disruption happens during the ultrasonic irradiation, the structure of the surfactant removed by ultrasonic treatment is unaffected in alcohol and may be utilized for further synthesis.

Figure 7

Figure 7. FT-IR spectra of (a) fresh CTABr-ethanol solution, (b) effluents after 15 min sonication at 40 °C, and (c) effluents after 60 min sonication at 40 °C. Panels (a) and (b) were reproduced from ref (60). [Jabariyan, S.; Zanjanchi, M. A. A simple and fast sonication procedure to remove surfactant templates from mesoporous MCM-41. Ultrason. Sonochem.2012, 19 (5), 1087–1093]. Copyright 2012 Elsevier. (d) UV–vis spectra for the methanol–effluent solutions after sonication at 40 °C and different times. Reproduced from ref (61). [Zanjanchi, M. A.; Jabariyan, S. Application of ultrasound and methanol for rapid removal of surfactant from MCM-41. J. Serb. Chem. Soc.2014, 79 (1), 25–38]. Copyright 2014, Serbian Chemical Society.

2.1.5. Ozone Treatment

Low-pressure mercury lamps are applied in ozone generation. These lamps will emit ultraviolet (UV) light with two peaks in the UV light band, one at 254 nm with the energy of 472 kJ/mol and another at 185 nm with the energy of 647 kJ mol–1. Since these energy values are higher than bonding energies in organic compounds such as C–H (413 kJ mol–1), C–C (348 kJ/mol), and C–O (352 kJ mol–1); UV lights are capable of removing the template at room temperature by breaking these bonds in the organic template. (66,67) The UV lamp is protected by a quartz tube, and both together are placed at the central axis of a reactor chamber. By passing air or O2 through the chamber, it is subjected to photolysis of the O2 molecule resulting in the formation of ozone.
Keene et al. (68) used this method for the first time to remove surfactant from MCM-41. In their study, ozone was generated from a simple UV lamp from atmospheric O2 at room temperature (although the temperature within the pores of MCM-41was higher). The FT-IR and TGA results indicated that the template was efficiently removed from MCM-41. However, the reaction time was longer by about 24 h, and CO2 is generated at the end of the process. Later, since the amount of generated ozone cannot be adjusted, and the reaction was long because of the low concentration of ozone (less than 1% by weight), instead of using a UV lamp, they employed an ozone generator. (69) To reduce the reaction time, ozone was generated via an electric discharge method. Their results showed that most of the CTABr surfactants were removed after 14 h from MCM-41 with a high SBET of 1019 m2 g–1 and pore diameter of 2.7 nm as well as a 5.52% carbon percentage. The structure of MCM-41 collapsed when the ozonation period was increased up to 26 h. Also, it was reported that template removal efficiency is lowered if the ozonation time is less than 14 h. (52,69)
Joshi et al. (70) used ozone treatment for P123 removal from as-synthesized SBA-15 at 80 °C for 120 min. Figure 8(a) shows the ozone reaction setup. It was stated that the carbon backbone of the P123 copolymer is highly oxygenated; thus, it reacts easily with ozone, causing the polymeric chains to become oligomers and further oxidation of the polymeric chains to occur through alcoholic and carbonyl groups. The results revealed that SBA-15 treated by ozone has a surface area of 711 m2 g–1 which was comparable with that of calcined SBA-15 (749 m2 g–1). Also, Barett–Joyner–Halenda (BJH) pore size and VT values for SBA-15 treated by ozone were higher than calcined SBA-15. The remained carbon values for both SBA-15 treated by ozone and calcination were 3% and 0.5%, respectively. As shown in the IR spectroscopy spectra, the intensity of C–H vibration bonds decreased significantly after ozone treatment indicating the elimination of the P123 copolymer from SBA-15 (Figure 8(b)). Moreover, the transmission electron microscopy (TEM) image shows that SBA-15 treated by ozone is a highly ordered structure (Figure 8(c)). The template removal efficiency of ozone treatment through the TGA analysis was not investigated by Joshi et al. (70) in order to compare with calcination or other methods discussed here.

Figure 8

Figure 8. (a) Schematic of ozone treatment set up, (b) normalized ATR spectra of samples, and (c) TEM image of SBA-15 treated by H2O2. Reproduced from ref (70). [Joshi, H.; Jalalpoor, D.; Ochoa-Hernández, C.; Schmidt, W.; Schüth, F. Ozone Treatment: A Versatile Tool for the Postsynthesis Modification of Porous Silica-Based Materials. Chem. Mater.2018, 30 (24), 8905–8914]. Copyright 2018, American Chemical Society.

The OH radicals can be generated by UV light in conjunction with H2O2 to get rid of organic contaminants in wastewater. (71,72) In this process, organic pollutants are oxidized to CO2 and water by OH radicals produced by the interaction between ultraviolet light and H2O2. Later, Xiao et al. (73) used the UV/H2O2 process to eliminate the P123 copolymer from as-synthesized SBA-15 by dispersion in an aqueous solution of H2O2 and adjusting pH values with hydrochloric acid (HCl). Then, the mixture was irradiated using a medium-pressure Hg light for 3 to 4 h while stirring. The pH of the aqueous solution of H2O2 had a great influence on the physicochemical properties of the sample. The rate of formation of OH radicals and their reactions with organic molecules are affected by pH. TGA results showed that the template can be more completely removed at lower pH than higher pH. Moreover, the sample treated at higher pH had a lower SBET and smaller VT than the sample treated under acidic conditions. The main disadvantages of this method can be that the organic templates cannot be recovered, and toxic gases are produced leading to pollution of the environment. (35)

2.1.6. Plasma Technology

Nonthermal plasma (NTP) or cold plasma is an efficient method to eliminate organic molecules through a highly oxidizing environment at ambient temperature. The glow discharge (GD) and dielectric barrier discharge (DBD, or silent discharge) are two examples of NTP which have been used to degrade templates from zeolite and mesoporous silica materials. (74−80)
For the production and treatment of catalysts, GD is employed as NTP with a high electron temperature (104–105 K) and a low gas temperature (as low as room temperature) because it is energy efficien and works at very mild conditions, and its operational time is shortened. (81−84) A schematic of GD plasma is depicted in Figure 9(a). It comprises two electrodes in a chamber that is filled with O2 as the plasma-forming gas after evacuation to below 1 Torr. The temperature of GD plasma could be lower than 50 °C. To prevent the entering of fine particles into the vacuum pump, a few drops of water are added to the SBA-15 before starting the template removal. Figure 9(b) shows the moving striations observed in the positive column when the as-synthesized SBA-15 is loaded. Then, in this positive column, the template is decomposed due to a strong interaction between the fluxes of plasma-active species (e.g., O2+, O, electron) and the SBA-15 surface. The color of the glow is determined by the type of gas in the tube. A blue-violet color is observed in the glow discharge plasma shown in Figure 9(b) because the chamber was fed with O2 as the plasma-forming gas. It should be noted that some gases are produced during template removal which could influence the GD performance; therefore, the amount of O2-forming GD gas should be sufficient for maintaining the stable discharge plasmas. The elemental analysis result shows that the carbon contents of the SBA-15 template were removed by GD plasma (SBA-15-GD) over 120 min and calcination (SBA-15-C) at 550 °C for 5 h under the heating rate of 1.75 °C min–1 were 1.28% and 0.3%. These results indicate that the template removal efficiency of GD plasma is much higher than that of methanol extraction, as discussed before. Figure 9(c) illustrates the N2 adsorption–desorption isotherms of samples. From the obtained results, SBA-15-GD possessed a higher SBET of 1025 m2 g–1 than SBA-15-C with the SBET of 827 m2 g–1. Moreover, the higher unit-cell size and the pore wall thickness of SBA-15-GD indicate that the shrinkage by GD is less than that by calcination because of applying low temperature for the elimination of the template. Also, it was found that more silanol densities are preserved on the surfaces by employing GD plasma rather than conventional calcination which is beneficial for postsynthesizing of silica support. Overall, it can be concluded that although about 94.8% of the template was removed by using GD plasma, the exposure time still is long at about 120 min.

Figure 9

Figure 9. (a) Schematic of GD plasma, (b) loaded sample on a quartz boat placed in the positive column of O2-forming GD, and (c) N2 isotherms and BJH pore size distributions (inset) of SBA-15-C and SBA-15-GD. Reproduced from ref (78). [Yuan, M.-H.; Wang, L.; Yang, R. T. Glow Discharge Plasma-Assisted Template Removal of SBA-15 at Ambient Temperature for High Surface Area, High Silanol Density, and Enhanced CO2 Adsorption Capacity. Langmuir2014, 30 (27), 8124–8130]. Copyright 2014, American Chemical Society.

DBD is generally considered a low-temperature plasma oxidation technology due to its operation under ambient conditions (at room temperature and atmosphere). DBD has been extensively utilized in many applications such as catalyst preparation and modification, (85−87) surface modification of nanofibers, (88) pollutant control (wastewater purification and engine exhaust control), (89−93) ozone generation, (94,95) hydrogen production from the reforming of biogas, (96) oxygen reduction reaction of electrocatalysts, (97) removal of volatile organic compounds (VOCs), (98,99) and remediation of pyrene and ciprofloxacin contaminated soil. (100−102) Recently, DBD was employed to eliminate the template from mesoporous materials, (75−77) particularly SBA-15. (74,80) The DBD plasma technology can be categorized into single dielectric-barrier discharge (SDBD) and double dielectric-barrier discharge (DDBD).
SDBD plasma is a promising technique that has exhibited a better performance to remove the template accompanied by less structure shrinkage and increased silanol density. A schematic of SDBD is shown in Figure 10(a) which has been employed for the template removal from SBA-15, (80) MCM-41, (76) and Zeolite Socony Mobil-5 (ZSM-5). (77) Wang et al. (80) used the SDBD reactor to eliminate the P123 copolymer from SBA-15. The FT-IR spectra of as-synthesis SBA-15, SBA-15-C, and SBA-15-DBD are illustrated in Figure 10(b). Normally, the aliphatic stretching and bending vibrations are observed at wavenumbers between 2950 and 2840 cm–1 and 1500–1350 cm–1, respectively. (103) As can be seen in Figure 10(b), these peaks appeared in the spectrum of as-synthesized SBA-15 signifying the presence of P123 copolymer. However, it was completely removed after SDBD treatment and calcination. Another interesting feature of Figure 10(b) is that there was a dramatic decrease in the intensity of the Si–OH bending band after calcination thanks to the dehydroxylation at higher temperatures for a prolonged time. The intensity of the Si–OH bending band of SBA-15-DBD is almost the same as the as-synthesized SBA-15, indicating that the DBD treatment can preserve more silanol groups on the pore wall as already proved from template removal of SBA-15 via GD plasma. The remaining silanol groups were further confirmed by 29Si solid sate NMR spectra. Figure 10(c) shows the N2 sorption–desorption isotherms of SBA-15-C and SBA-15-DBD together with their physicochemical properties. The wall thicknesses of both samples are the same, while SBA-15-DBD possessed higher SBET, VT, and larger pore size values because of the less lattice shrinkage in comparison to SBA-15-C treated at high temperature.

Figure 10

Figure 10. (a) Schematic of the SDBD apparatus. Reproduced from ref (85). [Guo, Q.; With, P.; Liu, Y.; Gläser, R.; Liu, C.-j. Carbon template removal by dielectric-barrier discharge plasma for the preparation of zirconia. Catal. Today2013, 211, 156–161]. Copyright 2013, Elsevier. (b) FT-IR spectra of samples and (c) N2 sorption–desorption isotherms of the sample treated by calcination and NTP along with their physicochemical properties. Panels (b) and (c) were reproduced from ref (80). [Wang, L.; Yao, J.; Wang, Z.; Jiao, H.; Qi, J.; Yong, X.; Liu, D. Fast and low-temperature elimination of organic templates from SBA-15 using dielectric barrier discharge plasma. Plasma Science and Technology2018, 20 (10), 101001]. Copyright 2018, IOPscience.

Aumond et al. (74) used a quartz reactor for template removal of SBA-15. A mixture of 80/20 helium/O2 was used as the feed gas. It has been well established that helium is a better energy carrier, and using this gas can considerably reduce plasma treatment time. The results showed that the pronounced lattice shrinkage by NTP is less because of the development of ultramicroporosity and larger hexagonal structured mesoporosity in comparison with the calcination method. Since NTP using a quartz reactor is working at room temperature, more silanol densities were preserved on the surfaces. Another advantage of using this method is that a less exposure time of about 15 min is needed for the template removal. The authors did not explain further the reaction mechanism of the template degradation using NTP. The interaction between the SBA-15 powder surface and active species such as positive ion O2+ and negative ions O and O2– as well as O3 resulted in the decomposition of the template. Indeed, the composition of the exhaust gases (mainly CO and CO2 associated with H2O) indicated direct oxidation of the template molecules.
Alternatively, plasma in an aqueous solution, also known as solution plasma, is a high potential plasma that was used to remove templates. Pootawang et al. (104,105) used the solution plasma process to eliminate the P123 template from mesoporous silica materials, as depicted in Figure 11(A). Various active species, such as high active radicals (e.g., H, O, OH, HO2), high energy electrons, and UV radiation can be physically created during discharge in an aqueous solution. The effects of discharge solution pH and discharge time were investigated on the template removal. There is no substantial variation in the intensity of the first peak in the small-angle X-ray diffraction (SAXRD) patterns shown in Figure 11(B), but the strength of the second peak was clearly identified in the different amounts.

Figure 11

Figure 11. Plasma solution process. (A) Scheme image of the solution plasma experimental setup. (B) SAXRD patterns of mesoporous silica discharged in different pHs at fixed 15 min of discharge time: (a) as-synthesized silica, (b) pH 3, (c) pH 7, and (d) pH 11. (C) SAXRD patterns of mesoporous silica discharged at different discharge times in pH 3: (a) as-synthesized silica, (b) 1 min, (c) 5 min, and (d) 15 min. TEM images of mesoporous silica discharged in different pH values at fixed 15 min of discharge time: (D) pH 3, (E) pH 7, and (F) pH 11. Reproduced from ref (104). [Pootawang, P.; Saito, N.; Takai, O. Solution plasma for template removal in mesoporous silica: pH and discharge time varying characteristics. Thin Solid Films2011, 519 (20), 7030–7035]. Copyright 2015, Elsevier.

The intensity of the second peak was lower at a pH of 7, while the sample exhibited a high intensity of the second peak when the pH of the discharge solution was adjusted to 7 or 11. This result indicates a high capability of the template removal process in acid and base solutions rather than neutral pH. Figure 11(C) shows the effect of discharge time on structural properties. As seen in Figure 11(C), the second peak intensity was much higher at the discharge time of 15 min. This result demonstrated that the rate of organic decomposition increased as discharge duration increased and was influenced by the number of active species, which had a strong tendency to create more as the system’s temperature and energy increased. The parallel channels with a uniaxial cylindrical mesopore arrangement are visible in the TEM images presented in Figure 11(D)–(F). The structural morphology of the mesopore structure was unaffected by changes in pH and discharge time.
Despite its advantages, for instance, simple experimental setup, stable and reproducible plasma conditions, and operating at atmospheric pressure and relatively low temperature, (78,85,99) SDBD plasma still has some significant limitations, including the need for a greater electrical voltage to create a strong electric field and the deposition of solid byproducts on the reactor’s inner surface and electrodes, which affect its performance. DDBD plasma technology is a modified version of SDBD plasma that has a better discharge efficiency and longer electrode lifespan. (49) DDBD plasma has been mostly utilized to remove air pollutants, particularly VOCs. (98,99) So far, there is no report on using DDBD plasma for template removal; therefore, DDBD plasma can be utilized for the template elimination from mesoporous siliceous materials. Furthermore, the plasma solution technique has some drawbacks, including the need for a high voltage to generate a continuous plasma discharge and low energy efficiency.
The oxidation mechanism of template elimination for the production of molecular sieves such as MCM-41 and ZSM-5 using DBD plasma was studied by Liu et al. (75) As illustrated in Figure 12(a), the infrared image showed that the template was removed at the highest temperature of 125 °C for 75 min. As can be seen in Figure 12(c), the color of MCM-41 was changed during template removal by increasing time. The fresh white sample became yellow after 15 min, showing that the template and plasma species were reacting. By increasing the time to 60 min, the sample became brown. The sample becomes white again after around 75 min. This marks the end of the template removal process. The mechanism study of template removal under DBD plasma is difficult due to complex reactions between active species and template molecules. The electrons play a vital role in the dissociation of template molecules. The energetic electron bombardment can decompose template molecules producing H2 and methane gases during the process. CO2 is also formed through oxidation with active oxygen species (O and O3). During the template elimination from MCM-41, mass spectra of gases revealed the presence of N2O gas as one of the products. As shown in Figure 12(b), FT-IR results of MCM-41 confirmed that MCM-41 templates are removed using DBD plasma so that C–H stretching and bending vibrations disappeared completely after 75 min. Also, the oxidation of nitrogen species in the organic template was observed by bands appearing at a wavenumber of about 1384 cm–1 from 15 to 60 min.

Figure 12

Figure 12. (a) Infrared image of the sample during the template removal process using DBD. Reproduced from ref (77). [Liu, Y.; Pan, Y.-x.; Kuai, P.; Liu, C.-j. Template Removal from ZSM-5 Zeolite Using Dielectric-Barrier Discharge Plasma. Catal. Lett.2010, 135 (3), 241–245]. Copyright 2010, Springer. (b) FT-IR spectra of MCM-41 during the detemplating process using DBD plasma. (c) Color changes of the samples during the template removal using DBD. Panels (b) and (c) were reproduced from ref (75). [Liu, Y.; Wang, Z.; Liu, C.-j. Mechanism of template removal for the synthesis of molecular sieves using dielectric barrier discharge. Catal. Today2015, 256, 137–141]. Copyright 2015, Elsevier.

2.2. Chemical Methods

2.2.1. Solvent Extraction

Template extraction using solvents is a common method for template removal, (106−121) as shown in Figure 13. de Ávila et al. (107) used different solvents such as water, acetonitrile, dichloromethane, ethanol, acetone, and methanol to eliminate the template from SBA-15 pores. The results indicated that water had the lowest effect on the template extraction, and the amount of remained P123 template was about 45.9% which was almost the same as the not-extracted one. Among studied solvents, however, methanol has the highest efficiency to remove the template. After template extraction using methanol, SBA-15 possessed about 10.3% of P123, and the result was in agreement with the amount of C of about 4.8% obtained from elemental analysis. The SBET, VT, and pore diameter of SBA-15 extracted with methanol were 703 m2 g–1, 0.995 cm3 g–1, and 15.2 nm, respectively. Moreover, the effect of extraction time on template removal was investigated using the aforementioned solvents. The results indicated that less extraction time of about 6 h is enough to remove the template when methanol was used as the extraction solvent in comparison to other solvents with a longer extraction time of up to 48 h to complete the template extraction. Chun et al. (122) used several solvents for extraction of pluronic F-127 such as methanol, ethanol, acetone, n-hexane, and iso-propanol. It was found that when methanol was employed as the solvent extraction, the highest efficiency of 78.8% was obtained. The above-mentioned results indicate that methanol has a better performance to remove the templates among polar and nonpolar solvents. A mixture of HCl and ethanol was reported for extractions of P123 and CTABr from SBA-15 (123,124) and MCM-48, (125) respectively. Sulfuric acid (H2SO4) was used to extract F-127 and P123 from a mesostructured polymer–silica composite (126) and SBA-15, (124) respectively, and also a mixture of H2SO4 and sodium hydroxide (NaOH) was utilized for removal of a P123 copolymer from SBA-15. (124) To generate mesopores and micropores in SBA-15, Schüth et al. (127) used H2SO4 under reflux at 95 °C for 24 h to partially remove a P123 copolymer from as-synthesized SBA-15 followed by calcination to decompose the occluded poly(ethylene oxide) chains in the silica matrix and to create micropores. The authors demonstrated that the ether cleavage by sulfuric acid at quite a low temperature resulted in the formation of mesopores due to the elimination of the PO groups. Following a thermal treatment in air at 200 °C to produce micropores, the EO chains, which are less accessible to the acid, may be destroyed. Thus, SBA-15 material with superior properties than the traditional calcined SBA-15 material has resulted from such acid and low-temperature treatments (larger mesopore size, larger micropore volume). However, this process is time consuming and requires two stages to remove the template from as-synthesized SBA-15.

Figure 13

Figure 13. Schematic of solvent extraction technique.

Grudzien et al. (128) used a combination of solvent extraction (ethanol/HCl) and temperature-controlled calcination to remove F-127 from SBA-16. Their results showed that SBA-16 has a higher SBET, VT and pore diameter and less framework shrinkage when the template was removed using this combination method in comparison to calcination alone, although the carbon percentage of the latter one was less than the former one. A mixture of ethanol/HCl with a molar ratio of (1:1) was used to remove mixed anionic surfactants such as sodium dodecyl benzenesulfonate (SDBS) and sodium dodecyl sulfate (SDS) from mesoporous silica materials. (129) The pore size distribution showed two narrow and broad peaks located at 10.3 and 30.7 nm, respectively. Samples had a low SBET of 217 m2 g–1. The formation of large pores indicates that a mixed anionic surfactant could be removed from the pores during solvent extraction. The mixture of ethanol–HCl was also used to remove CTAB from SBA-1 synthesized by cocondensation of TEOS and phenyltriethoxysilane (PhTES). (114) When the TEOS/PhTES molar ratio was (7:1), SBA-1 exhibited SBET and VT of 980 m2 g–1 and 0.47 cm3 g–1, respectively. The SBET and VT values were reduced when this ratio was reduced. The TGA data, on the other hand, revealed that surfactant remained in the pores of SBA-1, particularly at lower TEOS/PhTES molar ratios. The same result was reported for mesoporous silica material grafted by aminopropyltriethoxysilane (APS). (130)
Another study showed the removal of SDS using the mixture of HCl and acetonitrile so that 89% of SDS was removed as conformed by elemental analysis. (131) Yokoi et al. (132) used the mixture of HCl and acetonitrile to remove the SDBS, SDS, and lauric acid sodium salt (LAS) anionic surfactants from pores. The elemental analysis results showed that 88%, 89%, and 91% of SDBS, SDS, and LAS surfactants were removed, respectively, following the solvent extraction at room temperature for 2 h. The final powder was unstable when SDBS was used as a surfactant upon the solvent extraction. Also, the extracted samples had a lower SBET than calcined counterparts due to the retention of aminopropyl moieties on the surface.
Rahman et al. (133) used 5 wt % aqueous dimethyl sulfoxide (DMSO) solution to remove the template from mesoporous silica synthesized using sodium silicate as a silica source from bagasse ash. The sample extracted by a 5 wt % aqueous DMSO solution showed a typical type IV isotherm with an H2 type of hysteresis indicating the mesoporosity of the obtained material. The extracted sample exhibited a higher SBET of 656 m2 g–1 than the calcined sample, which had an SBET of 486 m2 g–1 at pH 3. The process of template removal has a substantial impact on the pore volume. The pore volume of silica obtained during solvent extraction was approximately 0.8 cm3 g–1, while that obtained through calcination was around 0.2 cm3 g–1. For solvent extraction, the pore diameter increases dramatically as the pH rises, but it remains relatively constant for calcination. The pore diameter was around 4 nm for calcination, and it varies from 3 nm at pH 2 to 18 nm at pH 7 for solvent extraction.
Solvent extraction was employed to remove dual templates of F-127 and P123 from SBA-16 functionalized by carboxyethylsilanetriol sodium salt (CES) using 8 wt % H2SO4 solutions. (118) After solvent extraction, the sample had SBET and VT of 575 m2 g–1 and 0.71 cm3 g–1, respectively, and exhibited a sharp diffraction peak with a higher intensity in comparison to as-synthesized counterpart. Also, after acid extraction, the TEM image demonstrated the presence of distinctive pores of ordered mesoporous silica. Although these findings show that acid extortion is a viable strategy for removing the template from surface-functionalized mesoporous silica materials, template removal takes a longer duration of 24 h. (118)
Zhou et al. (134) used solvent extraction with acetonitrile in an autoclave at 90 °C to remove IL as a template from mesoporous silica, namely, 1-butyl-3-methyl-imidazolium-tetrafluoroborate, [C4mim]BF4. The FT-IR revealed that imidazolium ν(C–H) stretching region (3200–3000 cm–1) of the IL vanishes completely. The sample had SBET and VT of 801 m2 g–1 and 1.27 cm3 g–1, respectively. These results indicate the effectiveness of solvent extraction in IL removal from the pores. Although IL was removed completely, the extraction was repeated several times, and a high volume of solvent was used.
The solvent extraction method is more advantageous than the calcination method because more silanol groups can be preserved, and shrinkage of pores is not significant after template extraction. However, the solvent extraction method is far from practical application. From the economic and environmental perspectives, this method is not beneficial due to a large volume consumption of organic solvent and the required high energy for solvent recovery. Above all, the template may not be completely removed even when the extraction treatment is repeated several times.

2.2.2. Chemical Oxidation

H2O2 treatment is based on an advanced oxidation process where the surfactant decomposition happens by in situ HO generation. The Fenton-based oxidation process is frequently applied for HO generation taking place in the presence of H2O2 and some metal ions (such as Ni, Fe, Bi, Cr, and Zn). H2O2 treatment catalyzed by Fe was applied to remove the template of MCM-41 (135) and zeolite beta. (136,137) Later, Zhang et al. (138) used H2O2 for the generation of HO catalyzed by Fe cations to eliminate the template of SBA-15 at 70 °C for 7 h. The following reactions show the template removal using H2O2 catalyzed by Fe3+ and Fe2+ cations. In reaction 5, HO radicals oxidize the organic template entrapped within the structure; finally, mesoporous material is obtained, and H2O and CO2 are generated (reaction 5).
(1)
(2)
(3)
(4)
(5)
The results showed that the carbon content of materials was significantly reduced to 0.4% and even more reduction to 0.2% when the template of SBA-15 was extracted by ethanol and then H2O2 treatment catalyzed by Fe cations. However, the carbon content of calcined SBA-15 was 0.1%. The SBA-15 treated by H2O2 had a higher silanol value of 44% than that of the calcined counterpart with a 30% silanol value determined by 29Si NMR. Also, template removal using H2O2 increased SBET and VT of SBA-15 compared to conventional calcination. (138) Zhang and Melián-Cabrera (139) reported similar results. In their study, the effects of secondary treatments such as direct drying, hydrothermal treatment, and solvent exchange were investigated on the structural and textural properties of SBA-15.
On the other hand, this process has two main disadvantages of a long time for template removal and the limitation of mesoporous silica for desired application because of the existence of metal ions in the silica framework. Also, CO2 is generated after completing the process, as mentioned above. It was reported that H2O2 has enough power to eliminate the template for pores of MCM-41 in the presence or absence of metal ions (Fe3+) with a significantly shorter reaction time (1 h). (140) Later, Barczak (108) used the H2O2 treatment method without a Fenton reaction to remove the P123 copolymer from pores of SBA-15 at 108 °C for 3 h, and the results were compared with extraction and calcination methods. The carbon content of SBA-15 treated by H2O2 was 0.6% which is comparable with the results stated by Zhang et al. (138) with the Fenton reaction. Figure 14(a) displays the scanning electron microscope (SEM) images of SBA-15 treated by different methods. As can be seen, the SBA-15 materials had the same morphology of parallel hexagonal cylinders with a “sausage-like” shape. As displayed in Figure 14(b), the N2 adsorption–desorption isotherms of SBA-15 materials showed a type IV isotherm according to the IUPAC classification associated with their mesoporous structure with hysteresis loops. Also, the results showed that SBA-15 treated by H2O2 exhibited a higher SBET of 953 than those treated by extraction (688 m2 g–1) and calcination (726 m2 g–1). Moreover, from SAXRD patterns shown in Figure 14(c), it was found that the framework shrinkage is significantly reduced through H2O2 treatment and extraction; however, the first sharp reflection and the other two weak reflections were less intense and shifted toward higher values indicating the occurrence of framework shrinkage during calcination. As seen in Figure 14(c), two minor reflections were resolved well, and their intensities were higher for SBA-15 treated by H2O2 than that treated by calcination indicating a better organization obtained by surfactant removal via H2O2 treatment. Therefore, these results confirm that H2O2 treatment is an effective method to eliminate the most anchored poly(oxypropylene) blocks remaining with only very small amounts of the template in the pores. In another interesting effort done by Yang et al., (141) the template was removed using H2O2 in the crystallization process. The coupling of the crystallization process and hydrothermal oxidation with H2O2 facilitates further condensation and slight framework shrinkage. The hydrothermal stability of materials was investigated using boiling water for 72 h under reflux. Their results showed that the sample treated by H2O2 could maintain about 86% of its specific surface, while the sample without H2O2 treatment had a less ordered structure and preserved only 24% of its specific surface area.

Figure 14

Figure 14. Characterization of SBA-15 materials treated by different methods: SBAP, as-synthesized SBA-15; SBAC, SBA-15 treated by calcination; SBAE, SBA-15 treated by extraction; and SBAH, SBA-15 treated by H2O2. (a)–(c) SEM images. (d) N2 adsorption–desorption isotherms. (e) SAXRD patterns. Reproduced from ref (108). [Barczak, M. Template removal from mesoporous silicas using different methods as a tool for adjusting their properties. New J. Chem.2018, 42 (6), 4182–4191]. Copyright 2018, Royal Society of Chemistry.

Lu et al. (142) used a chemical oxidation method at a low temperature of 60 or 90 °C with a duration of 4 or 24 h for template removal from SBA-15 using a potassium permanganate (KMnO4)–H2SO4 solution as an oxidizer. This method was efficient for the purification of carbon nanotubes from amorphous carbons. (143) According to the findings, the temperature and reaction time have great effects on the formation of manganese oxide on the exterior surface of SBA-15. The reaction between the template and KMnO4 is mainly controlled by temperature so that there is manganese oxide on the exterior surface at low temperature, while there is no deposition of manganese oxide on SBA-15 at higher temperatures (60 or 90 °C). Regarding the effect of reaction time, if the temperature is low, for example, room temperature, the reaction time should be longer. The SBA-15 treated by chemical oxidation at 90 °C for 24 h had a higher SBET, VT, and pore diameter of 940 m2 g–1, 1.42 cm3 g–1, and 9.8 nm, respectively, indicating better textual properties in comparison to calcined SBA-15. Compared with calcined SBA-15 with a0 of 10.5 nm, the SBA-15 treated by KMnO4 had a0 = 11.8 nm, indicating less of a shrinkage structure during KMnO4 treatment compared to calcination. Ding et al. (144) used HNO3 oxidation to remove the P123 copolymer from SBA-15 at 100 °C for 12 h. Through this method, block copolymer P123 is easily oxidized into small molecules, such as formaldehyde, formic acid, acetaldehyde, acetic acid, and CO2. The SBET, VT, and BJH pore size values for SBA-15 treated by HNO3 oxidation were 714.6 m2 g–1, 1.30 cm3 g–1, and 6.79 nm, respectively, while those for calcined SBA-15 were 723.8 m2 g–1, 0.86 cm3 g–1, and 5.36 nm, respectively. Moreover, the positions of the diffraction peaks of the SBA-15 treated by HNO3 oxidation were basically the same as those of as-synthesized SBA-15, while the positions of the diffraction peaks of calcined SBA-15 are obviously shifted to a high angle. This indicates less shrinkage of framework during HNO3 oxidation treatment compared to calcination. The result showed that the removing ratio of the template of SBA-15 is 82.5%. The advantage of HNO3 oxidation treatment over KMnO4–H2SO4 solution treatment is that the reduction product can be easily removed by washing, therefore, avoiding the use of KMnO4 or other metal oxidants in the process of oxidizing the template.

2.2.3. Ionic Liquid (IL) Treatment

The IL treatment is the last method used for template removal, as shown in Figure 15. The idea of using IL for template removal comes from biomass delignification. To increase the accessibility of enzymes to cellulose and in turn improve the hydrolysis process, removal of lignin as an organic polymer is necessary. Wang and Yang (145) used IL 1-butyl-3-methylimidazolium chloride ([C4mim]Cl) to eliminate the P123 template from as-synthesized SBA-15 at 120 °C for 12 h and compared the results with conventional calcination at 500 °C for 6 h. The results revealed that the SBA-15 treated by calcination and IL showed BJH pore size distributions of 6.4 and 7.5 nm, respectively. This indicates that using IL treatment resulted in less shrinkage of the mesoporous framework structure compared to calcination. The TGA results showed that the P123 template was removed at least 92%, demonstrating that treatment was effective. Moreover, more silanol groups were retained in the SBA-15 framework treated by IL in comparison to that treated by calcination so that silanol numbers of SBA-15 treated by IL and calcination were 5.1 and 3.0 OH nm–2, respectively. Moreover, SBET and VT of SBA-15 treated by IL were 835.5 m2 g–1 and 1.09 cm3 g–1, respectively, which were comparable with the calcined counterpart. The template removal mechanism through IL treatment is similar to that of cellulose dissolution in ILs. The hydrogen bonds between the template P123 and the silanol groups on the surface are likely disrupted and broken by using IL so that the treated SBA-15 has a higher surface hydroxyl group density. The template removal at the low temperature of 120 °C and recovery of IL and P123 templates are the main advantages of this method. The disadvantages of this method might be the challenging synthesis route, potential toxicity, high cost, and required purification.

Figure 15

Figure 15. Schematic of IL treatment technique.

3. Challenges and Perspectives

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Mesoporous silica materials have attracted a lot of attention in recent decades due to their highly tunable textural and chemical characteristics, and they have been used as adsorbents and catalyst supports in a range of applications. Template removal is the most important and last step in the preparation of mesoporous silica materials, and it has a great effect on the final properties of desired materials. Calcination under an air atmosphere at a high temperature of 550 °C for more than 5 h is the common method to obtain porosity. Despite its great effectiveness at removing templates, calcination has several drawbacks, including structural shrinkage, reduced silanol concentrations, production of huge volumes of CO2, and the inability to recover or reuse expensive organic templates. Many efforts have been reported in the literature to develop alternative methods to calcination. Herein, we have reviewed the developed approaches to remove various types of templates, as shown in Table 4. The advantages and disadvantages of template removal methods are presented in Table 4. Most of these methods are effective to remove the template from the pores by preserving high silanol density with less shrinkage and possibly a higher micropore volume. However, due to the inability to recover or reuse the template, CO2 emissions at the end of the process, and particularly the requirement of a complicated and expensive apparatus for template removal, it is unlikely that these developed technologies will be used on a large scale in the next years.
Table 4. Comparing Different Template Removal Methods
Template removal methodAdvantagesDisadvantagesref
Physical method
CalcinationHighly template removal efficiencyConducting at high temperature, significant framework shrinkage, reduction of silanol concentrations, generation of large amounts of CO2 and toxic gases, and inability to recover or reuse templates (33−39)
SC–CO2 extractionHigh template removal efficiency in the presence of solvents, preserving high silanol concentration, and possible recovery or reuse of templateEquipment limitation, using cosolvents to enhance template removal efficiency, and difficulties to achieve the appropriate temperature, pressure, and CO2 flow speed (35,36,43−47)
Microwave-assisted treatmentHigh template removal efficiency, quick template removal, less energy consumption, and less framework shrinkageEmission of CO2 and toxic gases, inability to recover or reuse the surfactant, use of solvents for assisting the template removal process, and equipment limitation (49,50)
Ultrasonic-assisted treatmentHigh template removal efficiency, preserving high silanol concentration, less framework shrinkage, and possible recovery or reuse of templateIneffective to remove the template completely at low temperature in some cases, and required organic solvents (60−62)
Ozone treatmentHigh template removal efficiency and less carbon contentEmission of CO2 and toxic gases, longer reaction time in some cases, equipment limitation, and inability to recover or reuse the surfactant (52,68−70)
Plasma technologyHigh template removal efficiency, operation under ambient conditions, preserving high silanol concentration, less framework shrinkage, and less exposure timeEmission of CO2 and toxic gases, inability to recover or reuse the surfactant, equipment limitation, inability to recover or reuse the surfactant, higher carbon content compared to calcination, required greater electrical voltage, and deposition of solid byproducts on the reactor’s inner surface and electrodes (74−80)
Chemical methods
Solvent extractionPreserving high silanol concentration, less framework shrinkage, and possible recovery or reuse of templateLess template removal efficiency and large volume consumption of organic solvent (106−118)
Chemical oxidationHigh template removal efficiency, high silanol concentration, and less framework shrinkageLonger reaction time, the existence of metal ions in the framework (if Fenton reagents used), generation of CO2, and inability to recover or reuse the surfactant (108, 135, 138−141)
IL treatmentHigh template removal efficiency, high concentration of surface silanols, less framework shrinkage, required a low temperature of 120 °C, and possible recovery of templateChallenging synthesis route, potential toxicity, high cost, and required purification (145)
To remove the template from nonfunctionalized mesoporous silica materials, calcination is a preferred option in the laboratory regardless of its disadvantages. For many desired applications, mesoporous silica materials are functionalized with organic groups, for example, an amino group, via grafting and co-condensation methods. In such cases, calcination is no longer an option due to the elimination of the functional group along with the template, and the template is usually removed using a solvent extraction technique to preserve functional groups. Despite the fact that the process and apparatus are simple and the template might be recovered, removing the template through the solvent extraction approach is not good enough and requires a large amount of solvent and a lengthy time, so it is not the preferred method from environmental and economical perspectives.
For high template removal efficiency and a high silanol density, a combination of two or three methods is frequently utilized instead of high-temperature calcination alone. For instance, the template is removed first via solvent extraction and then calcination at a low temperature. The combination approach, on the other hand, comes at an additional expense and takes longer.
Because of several advantages such as ease of use, high template removal efficiency, less framework shrinkage, maintaining a high silanol density on the surface, template recovery, and no equipment limitations, we believe that IL treatment could be considered a potential approach for template removal. But still, some questions need to be answered, such as whether IL can effectively remove various types of surfactants (nonionic, cationic, and anionic) from various mesoporous silica materials. Furthermore, the template removal conditions need to be optimized by studying various factors such as, for example, solid to liquid ratio of the sample/IL, temperature, reaction time, ane stirring rate.
Despite the fact that there is relatively little evidence in the literature, IL treatment may attract researchers’ interests in the near future. But, bearing in mind that ILs suffer several disadvantages including potential toxicity, the creation of large amounts of waste, availability and cost issues, purification and complex reaction steps, poor biodegradability, and high viscosity which may limit their use in large-scale industrial applications, it is essential to find promising solvents as alternatives to IL for template removal.
Deep eutectic solvents (DESs), also known as IL analogues, have emerged as possible alternatives to ILs. DESs are composed of two or more components, namely, hydrogen bond acceptor (HBA) and hydrogen bond donor (HBD), which can associate with each other through hydrogen bonding interactions. (103,146−158) DESs share the same properties as ILs but enjoy several advantages over ILs: (1) They can be used without purification. (2) Their preparation is easy. (3) They have low cost, good renewability, and low toxicity.
Many types of ILs and DESs have been utilized for biomass delignifcation which are effective to break hydrogen bonds within the cellulose. Among DESs, acid-based DES, base DES, polyalocohol-based DES, and phenolic-based DES have been used for biomass delignifcation. (159,160) Among these DESs, choline chloride-oxalic acid (1:1) showed an excellent performance to remove lignin. As reported by Zhang et al., (161) biomass pretreatment with acid-based DESs such as choline chloride (ChCl)-oxalic acid (Ox) (1:1) removed 98.5% of lignin by stirring at 90 °C for 24 h. Moreover, their results showed that polyalocohol-based DES, ChCl-ethylene glycol (EG) (1:2), can remove about 87.6% of the lignin from corncob biomass. Also, the performance of IL or DES treatment in template removal is the same as that in biomass delignifcation. The DES can break the hydrogen bonding between hydroxyl groups on the surface of virgin mesoporous silica materials and the template at a low temperature leading to retaining a high silanol density on the surface as well. Due to the tunable properties of DESs, it is possible to prepare task-specific DES or ternary DES to enhance template removal efficiency. Therefore, as an alternative to IL treatment and future works, DES treatment is proposed for template removal from mesoporous silica materials.

4. Conclusions

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Template removal is a crucial step in the synthesis of mesoporous silica materials. In the present study, we have discussed several methods to remove a variety of templates such as nonionic, cationic, and anionic surfactants as well as IL from different types of mesoporous silica materials. Among physical and chemical methods discussed here, calcination and solvent extortion methods are widely used for template removal. However, it is frequently noted that thermal calcination at high temperatures for many hours has some drawbacks, including framework shrinkage, lower silanol content, and the burning off of costly templates, which results in CO2 and hazardous gas emissions. The latter method also necessitates a large volume of solvent and a long time, and it is inefficient in effectively removing the template. Therefore, to mitigate the problems related to conventional methods, many physical and chemical methods have been utilized for template removal. The literature survey indicates that the majority of the developed methods can efficiently remove templates while preserving the high silanol content at mild conditions. However, when these new methods for template removal were implemented, certain major issues remained that may limit their practical applicability: (1) Costly templates cannot be recovered or reused. (2) CO2 and hazardous gas are produced at the end of the process. (3) The equipment has limitations. Among the developed methods, IL treatment showed an excellent performance in template removal without suffering the above-mentioned problems.

Author Information

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  • Corresponding Author
  • Author
    • Hosein Ghaedi - School of Environment, Tsinghua University, Beijing 100084, China
  • Notes
    The authors declare no competing financial interest.

Biographies

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Hosein Ghaedi was born in the Iranian city of Chahvarz in the province of Fars in the year 1984. He is a Ph.D. candidate in Environmental Science and Engineering at Tsinghua University’s School of Environment (Beijing, China), where he is supervised by Prof. Ming Zhao. He earned his M.Sc. in Chemical Engineering from Malaysia’s Universiti Teknologi Petronas (UTP). His study focuses on utilizing deep eutectic solvents toward green synthesis and functionalization of mesoporous silica materials for CO2 capture.

Dr. Ming Zhao is an Associate Professor of the School of Environment, Tsinghua University. He is the founder of the LBC Group (Lab for Bio-resource & Carbon-mitigation Technologies). He obtained his Ph.D. in Chemical Engineering from the University of Sydney in 2010. He joined Tsinghua University after the completion of his work at the Imperial College London in 2014. Dr. Zhao and his group possess expertise in thermo-chemical conversion of biomass (wastes) into clean energy and value-added chemicals and CO2 capture and utilization. The LBC Group has published 90+ peer-reviewed articles in recent years. Dr. Zhao also maintains linkage to the industry, and one of his gasification technologies has been commercialized for gaseous fuel production from solid wastes.

Acknowledgments

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Hosein Ghaedi and Ming Zhao are grateful for the support of the National Key Research and Development Program of China (2018YFC1901300).

Abbreviation Definition

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SBA

Santa Barbara Amorphous

MCM

Mobil Composition of Matter

KIT

Korean Advanced Institute of Science and Technology

ZSM-5

Zeolite Socony Mobil-5

P123

Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol)

F-127

Poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide)

CTABr

Cetyltrimethylammonium bromide

CTEABr

Cetyltriethylammonium bromide

SDBS

Sodium dodecyl benzenesulfonate

SDS

Sodium dodecyl sulfate

LAS

Lauric acid sodium

TEOS

Tetraethyl orthosilicate

PhTES

Phenyltriethoxysilane

APS

Aminopropyltriethoxysilane

CES

Carboxyethylsilanetriol sodium salt

HO

Hydroxyl radicals

UV

Ultraviolet

SCF

Supercritical fluid

SC–CO2

Suppercritical CO2

BJH

Barett–Joyner–Halenda

HCl

Hydrochloric acid

H2SO4

Sulfuric acid

HNO3

Nitric acid

PrSO3H

Propylsulfonic acid

H2O2

Hydrogen peroxide

DMSO

Dimethyl sulfoxide

KMnO4

Potassium permanganate

IL

Ionic liquid

[C4mim]Cl

1-Butyl-3-methylimidazolium chloride

[C4mim]BF4

1-Butyl-3-methyl-imidazolium-tetrafluoroborate

THF

Tetrahydrofuran

VOC

Volatile organic compound

VT

Total pore volume

SBET

BET specific surface area

a0

Unit cell parameter

NMR

Nuclear magnetic resonance

SAXRD

Small-angle X-ray diffraction

FT-IR

Fourier transform infrared spectroscopy

SEM

Scanning electron microscope

TEM

Transmission electron microscopy

TGA

Thermogravimetric analysis

GC-MS

Gas chromatography–mass spectrometry

NTP

Nonthermal plasma

DBD

Dielectric barrier discharge

SDBD

Single dielectric-barrier discharge

DDBD

Double dielectric-barrier discharge

GD

Glow discharge

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Energy & Fuels

Cite this: Energy Fuels 2022, 36, 5, 2424–2446
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  • Abstract

    Figure 1

    Figure 1. (a) Number of publications for mesoporous silica materials from 2000 to 2021. (b) Applications of mesoporous silica materials in different research fields published on the Web of Science with the keyword of “mesoporous silica material” (accessed December 25, 2021).

    Figure 2

    Figure 2. Residual carbon content for calcined SBA-15 and KIT-6 at various temperatures and times. Reproduced from ref (34). [Basso, A. M.; Nicola, B. P.; Bernardo-Gusmão, K.; Pergher, S. B. C. Tunable Effect of calcination of the silanol groups of KIT-6 and SBA-15 Mesoporous Materials. Applied Sciences2020, 10 (3), 970]. Copyright 2020, MDPI.

    Figure 3

    Figure 3. In situ preparation of Pt/mesoporous composite materials using catalytic template removal method. Reproduced from ref (37). [Krawiec, P.; Kockrick, E.; Simon, P.; Auffermann, G.; Kaskel, S. Platinum-Catalyzed Template Removal for the in Situ Synthesis of MCM-41 Supported Catalysts. Chem. Mater.2006, 18 (11), 2663–2669].Copyright 2006, American Chemical Society.

    Figure 4

    Figure 4. Schematic of SC–CO2 extraction technique.

    Figure 5

    Figure 5. (a) Schematic of microwave-assisted treatment. (b) Possible mechanism for template removal from MCM-41 and SBA-15 using H2O2 treatment assisted by microwave. Reproduced from ref (48). [Chen, L.; Jiang, S.; Wang, R.; Zhang, Z.; Qiu, S. A novel, efficient and facile method for the template removal from mesoporous materials. Chemical Research in Chinese Universities2014, 30 (6), 894–899]. Copyright 2014, Springer.

    Figure 6

    Figure 6. (a) Generation of acoustic bubbles by ultrasonic irradiation. (b) Schematic of ultrasonic-assisted treatment.

    Figure 7

    Figure 7. FT-IR spectra of (a) fresh CTABr-ethanol solution, (b) effluents after 15 min sonication at 40 °C, and (c) effluents after 60 min sonication at 40 °C. Panels (a) and (b) were reproduced from ref (60). [Jabariyan, S.; Zanjanchi, M. A. A simple and fast sonication procedure to remove surfactant templates from mesoporous MCM-41. Ultrason. Sonochem.2012, 19 (5), 1087–1093]. Copyright 2012 Elsevier. (d) UV–vis spectra for the methanol–effluent solutions after sonication at 40 °C and different times. Reproduced from ref (61). [Zanjanchi, M. A.; Jabariyan, S. Application of ultrasound and methanol for rapid removal of surfactant from MCM-41. J. Serb. Chem. Soc.2014, 79 (1), 25–38]. Copyright 2014, Serbian Chemical Society.

    Figure 8

    Figure 8. (a) Schematic of ozone treatment set up, (b) normalized ATR spectra of samples, and (c) TEM image of SBA-15 treated by H2O2. Reproduced from ref (70). [Joshi, H.; Jalalpoor, D.; Ochoa-Hernández, C.; Schmidt, W.; Schüth, F. Ozone Treatment: A Versatile Tool for the Postsynthesis Modification of Porous Silica-Based Materials. Chem. Mater.2018, 30 (24), 8905–8914]. Copyright 2018, American Chemical Society.

    Figure 9

    Figure 9. (a) Schematic of GD plasma, (b) loaded sample on a quartz boat placed in the positive column of O2-forming GD, and (c) N2 isotherms and BJH pore size distributions (inset) of SBA-15-C and SBA-15-GD. Reproduced from ref (78). [Yuan, M.-H.; Wang, L.; Yang, R. T. Glow Discharge Plasma-Assisted Template Removal of SBA-15 at Ambient Temperature for High Surface Area, High Silanol Density, and Enhanced CO2 Adsorption Capacity. Langmuir2014, 30 (27), 8124–8130]. Copyright 2014, American Chemical Society.

    Figure 10

    Figure 10. (a) Schematic of the SDBD apparatus. Reproduced from ref (85). [Guo, Q.; With, P.; Liu, Y.; Gläser, R.; Liu, C.-j. Carbon template removal by dielectric-barrier discharge plasma for the preparation of zirconia. Catal. Today2013, 211, 156–161]. Copyright 2013, Elsevier. (b) FT-IR spectra of samples and (c) N2 sorption–desorption isotherms of the sample treated by calcination and NTP along with their physicochemical properties. Panels (b) and (c) were reproduced from ref (80). [Wang, L.; Yao, J.; Wang, Z.; Jiao, H.; Qi, J.; Yong, X.; Liu, D. Fast and low-temperature elimination of organic templates from SBA-15 using dielectric barrier discharge plasma. Plasma Science and Technology2018, 20 (10), 101001]. Copyright 2018, IOPscience.

    Figure 11

    Figure 11. Plasma solution process. (A) Scheme image of the solution plasma experimental setup. (B) SAXRD patterns of mesoporous silica discharged in different pHs at fixed 15 min of discharge time: (a) as-synthesized silica, (b) pH 3, (c) pH 7, and (d) pH 11. (C) SAXRD patterns of mesoporous silica discharged at different discharge times in pH 3: (a) as-synthesized silica, (b) 1 min, (c) 5 min, and (d) 15 min. TEM images of mesoporous silica discharged in different pH values at fixed 15 min of discharge time: (D) pH 3, (E) pH 7, and (F) pH 11. Reproduced from ref (104). [Pootawang, P.; Saito, N.; Takai, O. Solution plasma for template removal in mesoporous silica: pH and discharge time varying characteristics. Thin Solid Films2011, 519 (20), 7030–7035]. Copyright 2015, Elsevier.

    Figure 12

    Figure 12. (a) Infrared image of the sample during the template removal process using DBD. Reproduced from ref (77). [Liu, Y.; Pan, Y.-x.; Kuai, P.; Liu, C.-j. Template Removal from ZSM-5 Zeolite Using Dielectric-Barrier Discharge Plasma. Catal. Lett.2010, 135 (3), 241–245]. Copyright 2010, Springer. (b) FT-IR spectra of MCM-41 during the detemplating process using DBD plasma. (c) Color changes of the samples during the template removal using DBD. Panels (b) and (c) were reproduced from ref (75). [Liu, Y.; Wang, Z.; Liu, C.-j. Mechanism of template removal for the synthesis of molecular sieves using dielectric barrier discharge. Catal. Today2015, 256, 137–141]. Copyright 2015, Elsevier.

    Figure 13

    Figure 13. Schematic of solvent extraction technique.

    Figure 14

    Figure 14. Characterization of SBA-15 materials treated by different methods: SBAP, as-synthesized SBA-15; SBAC, SBA-15 treated by calcination; SBAE, SBA-15 treated by extraction; and SBAH, SBA-15 treated by H2O2. (a)–(c) SEM images. (d) N2 adsorption–desorption isotherms. (e) SAXRD patterns. Reproduced from ref (108). [Barczak, M. Template removal from mesoporous silicas using different methods as a tool for adjusting their properties. New J. Chem.2018, 42 (6), 4182–4191]. Copyright 2018, Royal Society of Chemistry.

    Figure 15

    Figure 15. Schematic of IL treatment technique.

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