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Synthesis and Exfoliation of Layered Hydroxide Zinc Aminobenzoate Compounds

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Synthesis and Exfoliation of Layered Hydroxide Zinc Aminobenzoate Compounds Journal of the Ceramic Society of Japan 117 [10] 1115-1119 2009 Paper Synthesis and exfoliation of layered hydroxide zinc aminobenzoate compounds Lifang ZHAO,*,** Jianyjing MIAO,* Hongshe WANG,* Yoshie ISHIKAWA** and Qi FENG**,† *Department of Chemistry and Chemical Engineering, Baoji University of Arts and Science, Baoji, Shanxi, 721007 P. R. China **Department of Advanced Materials Science, Faculty of Engineering, Kagawa University, 2217-20 Hayashi-cho, Takamatsu-shi, 761- 0396 Two types of layered hydroxide zinc o-aminobenzoate compounds with structures of layered basic metal salt (LBMS) were prepared by reacting of zinc hydroxide and o-aminobenzoic acid solution in a temperature range of 40–110°C. The formation reactions, structures, chemical compositions, and exfoliation behavior in alcohol solvents of the layered compounds were inves- tigated by using XRD, TG–DTA, SEM, and TEM. The layered phase with a basal spacing of 1.33 nm has an α-Ni(OH)2-like structure, and its chemical formula can be written as Zn(OH)1.27(o-NH2C6H4COO)0.73·nH2O. The 1.33 nm layered phase shows plate-like particle morphology. The plate-like crystals can be exfoliated into nanosheet-like particles in alcohol solvents. ©2009 The Ceramic Society of Japan. All rights reserved. Key-words : Layered hydroxide zinc aminobenzoate compound, Layered basic metal salt, Exfoliation reaction, Nanosheet [Received June 1, 2009; Accepted August 20, 2009] Another type of anion-exchangeable brucite-like layered metal 1. Introduction hydroxide compounds is known as layered basic metal salts Low-dimensional nanomaterials, such as zero-dimensional (LBMSs), and can be represented by a general formula of II m– 13) – nanoparticles, one-dimensional nanofibers and nanotubes, and [M (OH)2–x](A )x/m·nH2O. In the LBMS structure, the OH two-dimensional nanosheets, attract much attention due to their anions on the brucite hydroxide layer are partially replaced by special physical and chemical properties and potential applica- Am– anions, and Am– anions are anion-exchangeable. Some studies tions to nanotechnologies in wide fields. Exfoliation techniques on synthesis and structure of layered hydroxide zinc carbonate for layered compounds are interesting and useful for the prepa- compounds have been reported, and found that these layered ration of the two-dimensional nanosheets. Since the nanosheets compounds have the LBMS structure.14),15) Very recently we of the elementary layer with uniform thickness can be obtained have reported that layered hydroxide zinc benzoate compounds by using this low cost process, many studies have been carried can be prepared by the hydrothermal reaction of ZnO with ben- on the exfoliations of the layered compounds.1)–3) Up to now, zoic acid, and these compounds belong to LBMSs.16),17) Two many types of cation-exchangeable layered metal oxides, e.g. types of structures, zinc hydroxide-nitrate-like structure and α- 4) 5) layered titanates, and layered manganese oxides, have been Ni(OH)2-like structure, have been found in the layered hydroxide exfoliated by using organic amine intercalation reactions, which zinc benzoate compounds. We have achieved also the exfoliation offer variety of two-dimensional semiconductor nanomaterials. of the layered hydroxide zinc benzoate compounds in alcohol For anion-exchangeable layered compounds, only layered solvents, which is first time success in the exfoliation of LBMSs. double hydroxides (LDHs) have been successfully exfoliated. The exfoliated LBMS nanosheets are interesting two-dimensional The anion-exchangeable LDHs have a brucite-like structure with organic-inorganic nanocomposite, where the organic anions coor- II III m– II a general formula of [M 1–zM z(OH)2](A )z/m·nH2O, where M dinate directly to the metal ions in the metal hydroxide nano- is a divalent cation such as Mg2+, Mn2+, Fe2+, Ni2+, Zn2+, Cu2+, or sheet, which is different to the ionic binding between the LDH Co2+, MIII is a trivalent cation such as Al3+, Co, Mn3+, Cr3+, Fe3+, nanosheets and anions. 3+ 3+ m– 2– V , or Ga , and A is an exchangeable anion such as CO3 , In the present article, we described synthesis of a new type of NO3–, OH–, X–, etc. The z is the molar ratio of M3+/(M2++M3+), layered hydroxide zinc aminobenzoate compound and its exfoli- generally ranges between 0.2 and 0.4, and it determines the pos- ation reaction. To our best knowledge, no any study has been itive-layer charge density and the anion-exchange capacity.6) The reported on the synthesis and exfoliation of the layered hydroxide LDHs are a very attractive class of lamellar solids capable of pro- zinc aminobenzoate compound yet. The results of the exfoliation ducing various intercalation compounds and nanocomposites study will help us to understand the exfoliation reaction of using their anion-exchange properties and the wide possibility of LBMSs and effect of anion in the interlayer on the exfoliation manipulation. Recently much attention has been attracted on the reactions, and furthermore the exfoliation will give a new cate- LDHs exfoliation, and LDHs with the interlayer anions of gory for the nanosheets. dodecyl sulfate,7) glycine,8) amino acids,9) lactate,10) benzoate, 2. Experiment procedure 2,4-dichlorobenzoate-, hydroxybenzoate,11) and nitrate 12) have been successfully exfoliated. A 0.4 M NaOH solution (250 mL) was added dropwise into a 0.2 M Zn(NO3)2 solution (250 mL) at 10°C under stirring con- † Corresponding author: Q. Feng; E-mail: [email protected]. ditions for a period of 0.5 h. The product was aged in the reaction jp solution at 10°C for 4 h, and then was filtered, washed with dis- ©2009 The Ceramic Society of Japan 1115 JCS-Japan Zhao et al.: Synthesis and exfoliation of layered hydroxide zinc aminobenzoate compounds tilled water, and dried at 40°C for 1 d. This sample was used as the starting material for the preparation of the layered hydroxide zinc aminobenzoate compounds. For the preparation of the lay- ered hydroxide zinc aminobenzoate compounds, 0.5451 g of the starting material containing 3.2 mmol of Zn, o-aminobenzoic acid (o-NH2C6H4COOH), and 15 mL distilled water were sealed into a Teflon-lined autoclave with inner volume of 75 mL, and then hydrothermally treated at 40, 70, 90, 110 or 130°C for 12– 24 h under autogenous pressure. In this hydrothermal reaction, 0.132, 0.219, 0.395, 0.526, and 0.658 g of o-aminobenzoic acid were used to adjust the o-NH2C6H4COOH/Zn molar ratios in the reaction system to 0.3, 0.5, 0.9, 1.2 and 1.5, respectively. The product was filtered and washed with distilled water, and dried at 50°C for 1 d. The layered hydroxide zinc o-aminobenzoate compound (0.015 g) was added into an organic solvent (10 mL), and then ultrasonicated for 20 min or stirred for 1 d at room temperature Fig. 1. XRD patterns of (a) the starting material, and (b– d) products o for exfoliation treatment. After standing for 1 d, supernatant obtained by hydrothermal reaction of the starting material with -amino- ° r 24 h. The o-NH C H COOH/Zn molar ratios in colloidal solution was collected by pipetting off to separate the benzoic acid at 40 C fo 2 6 4 the reaction system are (b) 0.9, (c) 1.2, (d) 1.5, respectively. ●: 1.33 nm exfoliated nanosheet colloid solution from the unexfoliated solid layered phase; ■: 2.67 nm layered phase; : Zn(OH)2 phase. particles. The purified colloidal solution was dried using a * freeze-drier to obtain an exfoliated solid sample for the XRD and TG–DTA analyses. Saturation concentration (g·L–1) of the exfo- liated nanosheet sample was evaluated from the volume of the colloidal saturation solution and the weight after the freeze- drying treatment. Powder X-ray diffraction (XRD) analysis was carried out on a Shimadzu Co., XRD 6100 X-ray diffractometer with Cu Kα (λ = 0.15418 nm) radiation. Thermogravimetry (TG) and differ- ential thermal analysis (DTA) data were obtained on a Shimadzu Co., DTG60H thermal analyzer at a heating rate of 10°C/min in air. Scanning electron microscope (SEM) observation was car- ried out using a JEOL Ltd., JSM5500S. Transmission electron microscope (TEM) observation was performed on a JEOL Ltd., JEM3010 at 300 kV. In the TEM study of exfoliated sample, the exfoliated colloidal solution was supported on a microgrid, and dried at room temperature. 3. Results and discussion Fig. 2. XRD patterns of products obtained by reacting the starting mate- o ° o 3.1 Synthesis of layered hydroxide zinc o-amino- rial with -aminobenzoic acid at 70 C for 12 h. The -NH2C6H4COOH/Zn benzoate compounds molar ratios in the reaction system are (a) 0.3, (b) 0.5, (c) 0.9, (d) 1.2 and Figure 1 shows the XRD patterns of starting material and the (e) 1.5, respectively. ●: 1.33 nm layered phase; ◆: ZnO layered phase. products obtained by reacting the starting material with o-amino- benzoic acid at 40°C. The starting material was obtained by reacting NaOH solution and Zn(NO3)2 solution, and showed a ture conditions, suggesting the 2.67 nm layered phase is unstable XRD pattern of β-Zn(OH)2 phase (JCPDS No. 20-1435) (Fig. at high temperature. A small amount of ZnO phase was observed 1(a)). When the starting material was reacted with o-aminoben- also, due to the unreacted Zn(OH)2 phase was unstable and trans- zoic acid at 40°C, new diffraction peaks with d-values of 2.668, formed to ZnO phase under these conditions. 1.332, 0.6638, 0.4419 and 0.3377 nm were observed. The peaks The dependence of formations of the layered hydroxide zinc with d-values of 1.332, 0.6638, 0.4419 and 0.3377 nm can be o-aminobenzoate compounds on the o-NH2C6H4COOH/Zn assigned to a layered phase of hydroxide zinc o-aminobenzoate molar ratio and the reaction temperature are summarized in a compound with a basal spacing of 1.33 nm, and the peak with phase diagram of Fig.
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