Method for preparing hydrotalcite

A technology of hydrotalcite and ammonia water, applied in chemical instruments and methods, oxide/hydroxide preparation, chromium oxide/hydrate, etc., can solve problems such as troubles, achieve good application prospects, simplify the process, and be cheap

Inactive Publication Date: 2010-09-01
HUZHOU TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method requires real-time control of the pH value of the solution during the preparation, which brings considerable trouble to the material preparation.
Due to the fai

Method used

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  • Method for preparing hydrotalcite
  • Method for preparing hydrotalcite
  • Method for preparing hydrotalcite

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Aqueous ammonia and ammonium chloride were used to prepare 500ml of buffer solution with pH=10. Take 0.2mol AlCl 3 ·6H 2 O and 0.6mol MgCl 2 ·6H 2 O, add 200ml of water to form a mixed salt solution, slowly drop the mixed salt solution into the buffer solution under stirring at room temperature, continue stirring for 1 hour after the titration is completed, crystallize in an oven at 65°C for 20 hours, filter, and wash the filter cake Until the filtrate is neutral, it is dried at 55°C for 24 hours and then ground into a white powder to obtain chloride ion pillared magnesium aluminum hydrotalcite (Mg 0.75 Al 0.25 (OH) 2 Cl 0.25 mH 2 O), denoted as Mg 3 A1-Cl-LDHs.

[0028] The synthesized Mg 3 Al-Cl-LDHs samples were analyzed by powder X-ray diffraction (PXRD), using ARL SCINTAG X-ray diffractometer, Cu Kα (0.1545nm), tube pressure 45kV, tube flow 40mA, scan speed 2° min -1 , 2θ ranges from 1.5 to 80°. Synthetic sample Mg 3 The XRD patterns of Al-Cl-LDHs are ...

Embodiment 2

[0031] Aqueous ammonia and ammonium chloride were used to prepare 500 ml of buffer solution with pH=9. Take 0.2mol AlCl 3 ·6H 2 O and 0.4mol MgCl 2 ·6H 2 O, add 200ml of water to make a mixed salt solution, slowly drop the mixed salt solution into the buffer solution under stirring at room temperature, continue stirring for 1.5h after the titration is completed, crystallize in an oven at 65°C for 24h, filter, and filter cake Wash until the filtrate is neutral, dry at 65°C for 18 hours, and then grind it into a white powder to obtain chloride ion pillared magnesium aluminum hydrotalcite (Mg 0.67 Al 0.33 (OH) 2 Cl 0.33 mH 2 O). XRD and SEM characterizations showed that the synthesized sample had a single crystal phase, a hexagonal plate shape, uniform grain size distribution, and an average particle size of about 90nm.

Embodiment 3

[0033] Aqueous ammonia and ammonium chloride were used to prepare 500ml of buffer solution with pH=10. Take 0.2mol AlCl 3 ·6H 2 O and 0.8mol MgCl 2 ·6H 2 O, add 200ml of water to make a mixed salt solution, slowly drop the mixed salt solution into the buffer solution under stirring at room temperature, continue stirring for 1.25h after the titration is completed, crystallize in an oven at 95°C for 6h, filter, and filter cake Wash until the filtrate is neutral, add ammonia water to the filtrate, adjust its pH to 10, and use it as a new buffer solution. The filter cake was dried at 55°C for 20 hours and then ground into a white powder to obtain chloride ion pillared magnesium aluminum hydrotalcite (Mg 0.8 Al 0.2 (OH) 2 Cl 0.2 mH 2 O). XRD and SEM characterizations showed that the synthesized sample had a single crystal phase, a hexagonal plate shape, uniform grain size distribution, and an average particle size of about 85nm.

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Abstract

The invention relates to a method for preparing hydrotalcite, which comprises the following steps of: (1) preparation of buffer solution, namely preparing the buffer solution with a pH value of 9 to 10 by using aqueous ammonia and ammonium chloride or aqueous ammonia and ammonium bicarbonate; (2) dripping of metal salt solution, namely dripping the metal salt solution into the stirred buffer solution, and continuously stirring the solution for 1 to 1.5 hours after the dripping is finished; (3) crystallization and washing, namely crystallizing the stirred mixed solution for 6 to 24 hours at the temperature of between 55 and 95 DEG C, and filtering and washing the crystallized solution to obtain filter solution and filter cakes; and (4) drying and grinding, namely drying the filter cakes at the temperature of between 55 and 95 DEG C and grinding the filter cakes into powder. The method provides a stable solution environment with a pH value of 9 to 10 for the formation of the hydrotalcite by using the buffer solution used as a precipitating agent, ensures complete crystal phase structure and uniform grain size of a hydrotalcite product, and solves the problems of difficult pH value control, wide grain size distribution and the like during preparing the hydrotalcite by using a traditional co-precipitation method in the industry.

Description

technical field [0001] The invention relates to a preparation method of hydrotalcite. Background technique [0002] Hydrotalcite (Layered Double Hydroxides, referred to as LDHs), is a layered anionic clay, the general chemical formula is [M 2+ 1-x m 3+ x (OH) 2 ](A n- ) x / n mH 2 O, where M 2+ and M 3+ Represent divalent and trivalent metal ions, such as Mg 2+ , Zn 2+ 、Co 2+ 、Ni 2+ and Al 3+ , Fe 3+ and other metal cations; x is M 3+ / (M 2+ +M 3+ ) Molar ratio, 0.20~0.33; A n- is an intercalation anion, such as CO 3 2- , NO 3 - , heteropolyanions, metal complex ions, etc. [0003] Due to the unique layer cation adjustability and interlayer anion exchangeability of this kind of material, it has great application potential in catalysis, adsorption, ion exchange, synthetic materials, daily chemical industry, superconductivity and environmental protection. , so people have carried out extensive research on the preparation method of hydrotalcite in order to...

Claims

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Application Information

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IPC IPC(8): C01B13/14C01F7/02C01G3/02C01G9/02C01G51/04C01G49/02C01G53/04C01F11/02C01G37/02C01G15/00C01G49/16
Inventor 潘国祥曹枫唐培松陈海锋徐敏虹伍涛
Owner HUZHOU TEACHERS COLLEGE
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