Clean preparation method of magnalium based laminated 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: 2016-08-10
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Clean preparation method of magnalium based laminated composite hydroxide
  • Clean preparation method of magnalium based laminated composite hydroxide
  • Clean preparation method of magnalium based laminated composite hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step A: Weigh 3.48g of magnesium hydroxide and add it into 50g of deionized water, grind it in a ball mill for 10 minutes, and prepare A slurry.

[0022]Step B: take by weighing 2.564g Mg(NO 3 ) 2 .6H 2 O was added to 20ml deionized water to prepare a solution, Mg(NO 3 ) 2 The solution is added to the A slurry and stirred evenly to obtain the B slurry.

[0023] Step C: 2.4 g of pseudo-boehmite was weighed and added to 50 g of deionized water, and ground in a colloid mill for 10 minutes to prepare a pseudo-boehmite slurry. Prepare 5g of dilute nitric acid solution with a mass fraction of 5%, add the prepared dilute nitric acid solution dropwise to the pseudo-boehmite slurry under stirring, complete the dropwise addition in 5 minutes, then heat the pseudo-boehmite slurry to 90 °C and stirred for 1 hour to obtain C sol.

[0024] Step D: take by weighing 5.128g Mg(NO 3 ) 2 .6H 2 Add O to 50ml of deionized water to prepare a solution, add it to C sol, stir evenly to...

Embodiment 2

[0026] Step A, B: same as embodiment 1.

[0027] Step C: 2.4 g of pseudo-boehmite was weighed and added to 40 g of deionized water, and ground in a colloid mill for 15 minutes to prepare a pseudo-boehmite slurry. Prepare 8 g of dilute nitric acid solution with a mass fraction of 3%, add the prepared dilute nitric acid solution dropwise to the pseudo-boehmite slurry under stirring, complete the dropwise addition in 6 minutes, then heat the pseudo-boehmite slurry to 95 °C and stirred for 1 hour to obtain C sol.

[0028] Step D: Weigh 1.686g MgCO 3 Add it into 50ml of deionized water to prepare a solution, add it to C sol, stir evenly to obtain D sol; heat B slurry to 95°C, and add D sol dropwise to B slurry within 3 hours while stirring, After the dropwise addition, continue heating and stirring for 3 hours; after the reaction, filter and wash the slurry 3 times to obtain a layered composite hydroxide filter cake, and dry the filter cake in an oven at 100°C for 12 hours to obt...

Embodiment 3

[0030] Steps A and B: Same as Example 1, except that the weight of magnesium hydroxide in step A is 4.64g.

[0031] Step C: 2.4 g of pseudo-boehmite was weighed and added to 60 g of deionized water, and ground in a ball mill for 20 minutes to prepare a pseudo-boehmite slurry. Prepare 6g of dilute nitric acid solution with a mass fraction of 4%, add the prepared dilute nitric acid solution dropwise to the pseudo-boehmite slurry under stirring, complete the dropwise addition in 8 minutes, then heat the pseudo-boehmite slurry to 100 °C and stirred for 1 hour to obtain C sol.

[0032] 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 B slurry to 100°C, and stir under stirring to obtain D sol was added dropwise to B slurry within 4 hours, and continued to heat and stir for 3 hours after the dropwise addition; after the reaction, the slurry was filtered and washed 3 times to obtain a...

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Abstract

The invention provides a clean preparation method of a magnalium based laminated composite hydroxide. The method uses magnesium hydroxide, magnesium oxide, pseudo boehmite, inorganic acid and a material containing functional anions as raw materials, uses magnesium chloride or magnesium nitrate as a circulation medium, and uses the property of peptization under acidic condition of boehmite to improve the reaction activity of pseudoboehmite; the concentration of magnesium ions in solution is increased by using magnesium chloride or magnesium nitrate. The method accelerates the formation rate of laminated composite hydroxide, promotes the dissolution of magnesium hydroxide and magnesium oxide, shortens the reaction time, overcomes the defects of high reaction temperature and long time consumption in hydrothermal method for synthesis of laminated composite hydroxide, and can rapidly prepare magnalium based laminated composite hydroxide under mild conditions. Magnesium chloride and magnesium nitrate can be recycled; and the preparation process has no waste discharge, and is green and environment-friendly. The method has the advantages of abundant raw materials, low cost, simple preparation process, mild reaction conditions, and easiness to industrial production.

Description

[0001] Field [0002] The invention relates to the field of preparation of inorganic non-metallic 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 kind 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+ Represent divalent and trivalent metal cations respectively, x represents the change of metal element content, A n- Represents interlayer anions. LDHs have attracted extensive attention in recent years due to their unique two-dimensional layered structure and the exchangeability of interlayer anions. 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 me...

Claims

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Application Information

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Patent Type & Authority Applications(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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