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Rosette-like Layered Double Hydroxides: Adsorbent Materials for the Removal of Anionic Pollutants from Water

  • Kenji Tamura*
    Kenji Tamura
    National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    *E-mail: [email protected]
    More by Kenji Tamura
  • Rina Kawashiri
    Rina Kawashiri
    National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    Faculty of Bioscience and Applied Chemistry, Hosei University, 3-7-2 Kajino-cho, Koganei, Tokyo 184-8584, Japan
  • Nobuo Iyi
    Nobuo Iyi
    National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    More by Nobuo Iyi
  • Yujiro Watanabe
    Yujiro Watanabe
    Faculty of Bioscience and Applied Chemistry, Hosei University, 3-7-2 Kajino-cho, Koganei, Tokyo 184-8584, Japan
  • Hiroshi Sakuma
    Hiroshi Sakuma
    National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
  • , and 
  • Masumi Kamon
    Masumi Kamon
    National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    More by Masumi Kamon
Cite this: ACS Appl. Mater. Interfaces 2019, 11, 31, 27954–27963
Publication Date (Web):July 26, 2019
https://doi.org/10.1021/acsami.9b08719
Copyright © 2019 American Chemical Society

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    Abstract

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    Rosette-like layered double hydroxide (roseLDH) crystals with interlayer CO32– anions were synthesized by the reaction of Mg(NO3)2, Al(NO3)3, and hexamethylenetetramine (HMT) at 140 °C over 4 days. Crystals as large as 20 μm were produced when using a specific range of HMT concentrations. The substitution of CO32– interlayer ions with ClO4 or Cl anions was achieved by the addition of perchloric acid or hydrochloric acid, respectively, to dispersion of material in methanol. The products were denoted as CO32–roseLDH, ClO4roseLDH, and ClroseLDH, respectively. These LDHs were characterized using X-ray diffraction under controlled relative humidity, as well as by Fourier transform infrared spectroscopy and scanning electron microscopy. Adsorption experiment with anions such as phosphate (HPO42–) and nitrate (NO3) was conducted by using ClO4roseLDH and ClroseLDH. The results indicate that both anions were adsorbed through an ion-exchange mechanism. The maximum HPO42– adsorption capacity at equilibrium on ClO4roseLDH was 1.6 mmol g–1 (49.6 mg P g–1), which corresponds to approximately 75% of the total positive layer charge. ClroseLDH showed a similar adsorption capability. Commercially available platelike LDH particles were essentially impermeable to water flow due to clogging, while the roseLDH crystals showed excellent permeability, an order of magnitude higher than that exhibited by the platelike LDH synthesized using a homogeneous precipitation method with different growth conditions. Anion adsorption during batch and flow-through test with the ClO4roseLDH (mean particle diameter ∼ 38 μm) in a packed bed showed good uptake of HPO42– and NO3 from aqueous solutions. These results demonstrate the potential of roseLDH materials to serve as a column filler adsorbent of the hazardous anions.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acsami.9b08719.

    • Measurement of the water permeability coefficient; characterization of ClroseLDH; SEM image and EDS image of ClO4roseLDH; solution pH before/after HPO42– adsorption experiment for ClO4roseLDH: Langmuir plot of adsorption isotherm of ClO4roseLDH for HPO42– anions; SEM images of HPO42–-adsorbed ClO4roseLDH; adsorption isotherms of ClO4roseLDH for NO3; FTIR spectra of NO3 adsorbed onto ClO4roseLDH by the effect of the NO3 initial concentration; change in the basal spacing with relative humidity for ClO4roseLDH and ClO4roseLDH treated with 16.1 mol m–3 HPO42– solution; hydration behavior change by the adsorption of NO3 onto ClO4roseLDH under controlled RH; typical SEM images of prepared powders used for water permeability tests: sieved CO32–roseLDH and CO32–hexaDH powders; nitrogen adsorption isotherms for prepared particles; UV–vis spectra of (a) a methyl orange solution and (b) a filtrate; and permeability test (HPO42– solution) of the column packed with ClroseLDH (PDF)

    • Clear filtrate was obtained as a result of the adsorption of the dye (MP4)

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