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A clean preparation method of magnesium-aluminum-based layered composite hydroxide

A composite hydroxide and base layer technology, applied in the directions of aluminum compounds, chemical instruments and methods, nickel compounds, etc., can solve the problems of accelerating the formation rate of layered composite hydroxides, shortening the reaction time, and high reaction temperature, and achieving easy industrialization. The effect of production, shortened reaction time, simple preparation process

Active Publication Date: 2017-06-23
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention uses magnesium hydroxide or magnesium oxide, pseudo-boehmite, inorganic strong acid, and functional anion-containing substances as raw materials, uses magnesium chloride or magnesium nitrate as a circulating medium, and utilizes the property that pseudo-boehmite can be peptized under acidic conditions Improve the reactivity of pseudo-boehmite, use magnesium chloride or magnesium nitrate to increase the reaction rate of magnesium hydroxide and magnesium oxide, accelerate the formation rate of layered composite hydroxide, shorten the reaction time, and overcome the hydrothermal method to prepare layered composite hydrogen Oxide has the defects of high reaction temperature and long time consumption, and magnesium-aluminum-based layered composite hydroxide can be rapidly prepared under mild conditions

Method used

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  • A clean preparation method of magnesium-aluminum-based layered composite hydroxide
  • A clean preparation method of magnesium-aluminum-based layered composite hydroxide
  • A clean preparation method of magnesium-aluminum-based layered composite hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step A: Weigh 3.48g of magnesium hydroxide into 50g of deionized water, grind in a ball mill for 10 minutes to prepare A slurry.

[0024] Step B: Weigh out 2.564g Mg(NO 3 ) 2 .6H 2 O was added to 20ml deionized water to make a solution, and Mg(NO 3 ) 2 The solution is added to A slurry and stirred evenly to obtain B slurry.

[0025] Step C: Weigh 2.4 g of pseudo-boehmite, add it to 50 g of deionized water, grind in a colloid mill for 10 minutes, and prepare a pseudo-boehmite slurry. Prepare 5g of dilute nitric acid solution with a mass fraction of 5%, and add the prepared dilute nitric acid solution dropwise to the pseudo-boehmite slurry under stirring. The dripping is completed in 5 minutes, and then the pseudo-boehmite slurry is heated to 90 C sol was obtained by stirring for 1 hour at ℃.

[0026] Step D: Weigh out 5.128g Mg(NO 3 ) 2 .6H 2 O was added to 50ml of deionized water to prepare a solution, added to C sol, and stirred uniformly to obtain D sol; heat the B slurry t...

Embodiment 2

[0028] Steps A and B: same as in Example 1.

[0029] Step C: Weigh 2.4 g of pseudo-boehmite, add it to 40 g of deionized water, grind in a colloid mill for 15 minutes, and prepare a pseudo-boehmite slurry. Prepare 8g of dilute nitric acid solution with a mass fraction of 3%, and add the configured dilute nitric acid solution dropwise to the pseudo-boehmite slurry under stirring. The dripping is completed in 6 minutes, and then the pseudo-boehmite slurry is heated to 95 C sol is obtained by stirring for 1 hour at ℃.

[0030] Step D: Weigh 1.686g MgCO 3 Add it to 50ml of deionized water to prepare a solution, add it to C sol, stir evenly to obtain D sol; heat the B slurry to 95°C, add the D sol to the B slurry dropwise within 3 hours under stirring, After the dripping is completed, heating and stirring are continued for 3 hours; after the reaction, the slurry is filtered and washed 3 times to obtain a layered composite hydroxide filter cake, and the filter cake is dried in an oven a...

Embodiment 3

[0032] Steps A and B: Same as Example 1, except that the weight of magnesium hydroxide weighed in Step A is 4.64 g.

[0033] Step C: Weigh 2.4 g of pseudo-boehmite, add it to 60 g of deionized water, grind in a ball mill for 20 minutes, and prepare a pseudo-boehmite slurry. Prepare 6g of dilute nitric acid solution with a mass fraction of 4%, add the configured dilute nitric acid solution dropwise to the pseudo-boehmite slurry under stirring, and the dripping is completed in 8 minutes, and then heat the pseudo-boehmite slurry to 100 C sol is obtained by stirring for 1 hour at ℃.

[0034] Step D: Weigh 2.07g of salicylic acid and add it to 60ml of deionized water to prepare a solution, add it to C sol, stir evenly to obtain D sol; heat the B slurry to 100°C, and mix under stirring to obtain D sol was added dropwise to B slurry within 4 hours. After the addition, heating and stirring were continued for 3 hours; after the reaction, the slurry was filtered and washed 3 times to obtain...

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Abstract

A clean preparation method of magnesium-aluminum-based layered composite hydroxide. The present invention uses magnesium hydroxide and magnesium oxide, pseudo-boehmite, inorganic strong acid, and functional anion-containing substances as raw materials, uses magnesium chloride or magnesium nitrate as a circulating medium, and utilizes the property that pseudo-boehmite can be peptized under acidic conditions Improve the reactivity of pseudo-boehmite, use magnesium chloride or magnesium nitrate to increase the concentration of magnesium ions in the solution, accelerate the formation rate of layered composite hydroxide and promote the dissolution of magnesium hydroxide and magnesium oxide, shorten the reaction time, overcome the water The preparation of layered composite hydroxide by thermal method has the disadvantages of high reaction temperature and long time consumption, but magnesium-aluminum-based layered composite hydroxide can be rapidly prepared under mild conditions. Magnesium chloride and magnesium nitrate can be recycled, and there is no waste discharge in the preparation process, which is green and environmentally friendly. The method has the advantages of rich source of raw materials, low price, simple preparation process, mild reaction conditions, easy industrial production and the like.

Description

[0001] Field [0002] The invention relates to the field of preparation of inorganic non-metal functional materials, in particular to a clean preparation method of magnesium-aluminum-based layered composite hydroxide. Background technique [0003] Layered Double Hydroxides (LDH for short) is a type of anionic layered clay, its chemical formula is [M 2+ 1-x M 3+ x (OH) 2 ] x+ (A n- x / n ).mH 2 O, where M 2+ , M 3+ Respectively represent divalent and trivalent metal cations, x represents the change of metal element content, A n- Represents interlayer anions. LDH has a unique two-dimensional layered structure and the exchangeability of interlayer anions, and has received extensive attention in recent years. The unique properties of LDH make it widely used in the fields of catalysis, adsorption, ion exchange and polymer material additives (flame retardants, heat stabilizers and other functional additives). [0004] LDH is usually prepared by co-precipitation method, nucleation / crystalliz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/00C01G3/00C01G9/00C01G53/00
CPCC01G3/006C01G9/006C01G53/006C01P2004/03C01P2002/82C01P2002/72C01F7/78
Inventor 唐平贵李殿卿冯拥军陈廷伟
Owner BEIJING UNIV OF CHEM TECH
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