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Layered double hydroxide and preparation method thereof

A layered bimetal and hydroxide technology, applied in the direction of oxide/hydroxide preparation, oxygen/ozone/oxide/hydroxide, chemical instruments and methods, etc., can solve the impure morphology of interlayer anions , Complicated and cumbersome operation, irregularities and other problems, to achieve the effect of overcoming poor structural regularity, uniform particle size distribution, and regular layered structure

Inactive Publication Date: 2010-03-10
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a layered double metal hydroxide and its preparation method, which overcomes the low crystallinity of LDHs prepared by precipitation method, insufficient order of hydroxylated laminates, complex and cumbersome operation, and long production process. ; The sol-gel method has the disadvantages of high cost of preparation, easy to cause environmental pollution, and impure anions between layers and irregular morphology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Accurately weigh Ni(NO 3 ) 2 ·6H 2 O and Fe(NO 3 ) 3 9H 2 O, mixed salt solution was prepared with deionized water, and the concentration of metal ions in the solution was [Ni 2+ ]=0.0067mol / L, [Fe 3+ ]=0.0033mol / L, this mixed solution is placed in the beaker, prepare NaBH in addition 4 solution, [NaBH 4 ]=0.04mol / L. Equal volumes of mixed salt solution and NaBH 4The solution is poured into a rapidly rotating colloid mill (3000 rev / min), and after stirring for 3 minutes, the nano-metal particles obtained by reduction are transferred to an autoclave with a polytetrafluoroethylene liner, and the amount ratio of the total metal substance is added. Ammonium nitrate of 1, and hydrothermal crystallization at 120°C for 6 hours, after naturally cooling to room temperature, the obtained precipitate was washed with deionized water until neutral, and dried at 60°C for 12 hours to obtain [Ni 0.67 Fe 0.33 (OH) 2 ](NO 3 ) 0.33 The target product, LDHs, has a particle si...

Embodiment 2

[0017] Accurately weigh Ni(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 9H 2 O, mixed salt solution was prepared with deionized water, and the concentration of metal ions in the solution was [Ni 2+ ]=0.04mol / L, [Al 3+ ]=0.01mol / L, this mixed solution is placed in the beaker, prepare NaBH in addition 4 solution, [NaBH 4 ]=0.2mol / L. Equal volumes of mixed salt solution and NaBH 4 The solution is poured into a rapidly rotating colloid mill (5000 rev / min), and after stirring for 5 minutes, the nano-metal particles obtained by reduction are transferred to an autoclave with a polytetrafluoroethylene liner. Ammonium carbonate of 2, and hydrothermal crystallization at 200°C for 48 hours, after natural cooling to room temperature, the obtained precipitate was washed with deionized water until neutral, and dried at 60°C for 12 hours to obtain [Ni 0.8 Al 0.2 (OH) 2 ](CO 3 ) 0.1 The target product, LDHs, has a particle size of 80nm.

Embodiment 3

[0019] Accurately weigh Co(NO 3 ) 2 ·6H 2 O and Fe(NO 3 ) 3 9H 2 O, mixed salt solution was prepared with deionized water, and the concentration of metal ions in the solution was [Co 2+ ]=0.009mol / L, [Fe 3+ ]=0.003mol / L, put this mixed solution in a beaker, and prepare NaBH 4 solution, [NaBH 4 ]=0.04mol / L. Equal volumes of mixed salt solution and NaBH 4 The solution is poured into a rapidly rotating colloid mill (6000 rev / min), and after stirring for 10 minutes, the nano-metal particles obtained by reduction are transferred to an autoclave with a polytetrafluoroethylene liner, and the amount ratio of the total metal substance is added. 5 sodium carbonate, and hydrothermal crystallization at 120°C for 6 hours, after naturally cooling to room temperature, the obtained precipitate was washed with deionized water until neutral, and dried at 80°C for 24 hours to obtain [Co 0.75 Fe 0.25 (OH) 2 ](CO 3 ) 0.125 The target product, LDHs, has a particle size of 30nm.

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Abstract

The invention relates to a layered double hydroxide and a preparation method thereof, belonging to the technical field of metal hydroxide preparation. A chemical formula of the layered double hydroxide is as follows: (M1(1-x)M2x(OH)2)(A<n->)x / n), wherein x is larger than or equal to 0.2 and smaller than or equal to 0.33; M1 represents any one or more of divalent metal ions including Mg<2+>, Zn<2+>, Ni<2+>, Co<2+>, Ca<2+>, Cu<2+>, Fe<2+> and Mn<2+>; M2 represents any one or two of trivalent metal ions including Fe<3+> and Al<3+>; A<n-> represents any one of interlayer anions including CO3<2->,NO3<->, Cl<-> and SO4<2->; and the grain size ranges from 12 nm to 80 nm. The invention has the advantages that the preparation method is a direct method for preparing the layered double hydroxide with high crystallinity, layered structure regularity, wide application range and adjustable particle size. The preparation method comprises the following steps: obtaining highly dispersed metal nanoparticle sol by utilizing the action of colloid mill axial shear force and the sodium borohydride reducibility, and then performing slow oxydrolysis in a hydrothermal system, and the like to generate thenano layered double hydroxide with layered structure regularity and adjustable particle size. The method has the advantages of wide application range, low cost, simple operation and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of double metal hydroxides. In particular, a layered double metal hydroxide and a preparation method thereof are provided, and the prepared product has a regular layered structure and adjustable nanoparticle size. Background technique [0002] Layered double hydroxides (LDHs) are a new class of nanoscale inorganic functional materials with a layered structure, and their chemical composition can be expressed as [M z+ 1-X m 3+ X (OH) 2 ] X+ (A n- ) X / n mH 2 O, where M 2+ for Mg 2+ 、Ni 2+ 、Co 2+ , Zn 2+ 、Cu 2+ and other divalent metal cations; M 3+ for Al 3+ 、Cr 3+ , Ga 3+ 、In 3+ , Fe 3+ 、Sc 3+ and other trivalent metal cations; A n- is an anion, such as CO 3 2- , NO 3 - , Cl - , OH - , SO 4 2- 、PO 4 3- 、C 6 h 4 (COO) 2 2- Such as inorganic, organic ions and complex ions. In the LDHs crystal structure, due to the influence of the lowest lattice energy effect and its lattice ...

Claims

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Application Information

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IPC IPC(8): B82B1/00B82B3/00C01B13/00C01B13/14
Inventor 李峰张春芳刘玉成范国利张法智张慧李殿卿段雪
Owner BEIJING UNIV OF CHEM TECH
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