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Preparation method of nano LDH (layered double hydroxides)

A composite hydroxide and nano-layered technology, applied in chemical instruments and methods, nickel compounds, iron compounds, etc., can solve the problems of high energy consumption, long heating time, and high cost of LDH preparation, and achieve easy industrial production and preparation The effect of simple process and rich source of raw materials

Active Publication Date: 2016-04-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Co-precipitation and nucleation / crystallization isolation methods both use NaOH as the alkali source, and about 0.8 tons of NaOH are needed to produce 1 ton of LDH. Applications in the field
The uniform precipitation method usually uses urea as a precipitating agent, and the urea is slowly decomposed by heating to release ammonia to precipitate metal cations to form LDH. However, this method takes a long time to heat, consumes high energy, and can only prepare micron-sized LDH, and it is difficult to synthesize nano-sized LDH.

Method used

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  • Preparation method of nano LDH (layered double hydroxides)
  • Preparation method of nano LDH (layered double hydroxides)
  • Preparation method of nano LDH (layered double hydroxides)

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Step A: Weigh 5.88g of calcium oxide and add it into 110g of deionized water, grind it in a ball mill for 5 minutes, and prepare a calcium oxide slurry. Weigh 12.198gMgCl 2 . 6H 2 O and 7.2429g AlCl 3 . 6H 2 O was added to 100ml deionized water to prepare a salt solution.

[0025] Step B: Add the prepared salt solution dropwise to the calcium oxide slurry under magnetic stirring, and the dropwise addition is completed in 30 minutes, then heat the slurry to 60°C and continue to stir for 6 hours. After the reaction, filter and wash the slurry for 3 times A composite hydroxide filter cake is obtained.

[0026] C: Disperse the filter cake obtained in step B into 100ml of deionized water and grind it with a ball mill for 2 minutes to obtain a composite hydroxide slurry. Weigh 0.2g of disodium edetate into the slurry, stir evenly, and then weigh Take 1.9gNa 2 CO 3 Add it into the slurry, stir and react at 60°C for 1 hour, cool to room temperature after the reaction, ...

Embodiment 2

[0028] Step A: Same as Example 1, the difference is to weigh calcium oxide and MgCl 2 . 6H 2 The masses of O are 7.56g and 18.297g, respectively.

[0029] Step B: Add the prepared salt solution dropwise to the calcium oxide slurry under magnetic stirring, and the dropwise addition is completed in 20 minutes, then heat the slurry to 80°C and continue stirring for 3 hours. After the reaction, filter and wash the slurry 4 times A composite hydroxide filter cake is obtained.

[0030] Step C: Disperse the filter cake obtained in Step B into 150ml of deionized water and grind it with a ball mill for 4 minutes to obtain a composite hydroxide slurry. Weigh 0.4g of disodium edetate into the slurry, stir evenly, and then Weigh 2.0gNa 2 CO 3 Add it into the slurry, stir and react at 60°C for 1 hour, cool to room temperature after the reaction, the precipitate is washed by centrifugation until the pH value is less than 8, and the sample is dried in an oven at 100°C for 10 hours to ob...

Embodiment 3

[0032] Step A: Weigh 5.88g of calcium oxide and add it into 100g of deionized water, grind it in a ball mill for 8 minutes, and prepare a calcium oxide slurry. Weigh 15.384gMg(NO 3 ) 2 . 6H 2 O and 11.253gAl(NO 3 ) 3 . 9H 2 O was added to 90ml deionized water to prepare a salt solution.

[0033] Step B: Add the prepared salt solution dropwise to the calcium oxide slurry under mechanical stirring, and the dropwise addition is completed in 40 minutes, then heat the slurry to 90°C and continue to stir for 2 hours. After the reaction, filter and wash the slurry 4 times A composite hydroxide filter cake is obtained.

[0034] C: Disperse the filter cake obtained in step B into 120ml of deionized water and grind it with a ball mill for 2 minutes to obtain a composite hydroxide slurry. Weigh 0.5g of disodium aminotriacetate and add it to the slurry. After stirring evenly, weigh 4.68g of NaH 2 PO 4 2H 2 O was added to the slurry, stirred and reacted at 70°C for 2 hours, cool...

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Abstract

The invention provides a low-cost preparation method of nano LDH (layered double hydroxides). According to the method, divalent soluble metal nitrate or chloride and tervalent soluble metal nitrate or chloride are taken as raw materials of LDH laminates, calcium oxide is taken as an alkali source, calcium precipitation impurities are prevented from being formed through chelation of a calcium ion chelating agent, and high-purity nano LDH is prepared. The preparation method is simple, high temperature and high pressure are not required, special equipment is not required, sources of the raw materials are rich, and the cost is low. The nano LDH can be widely applied to the field of adsorption separation, catalysis, high polymer materials and the like.

Description

[0001] Field [0002] The invention relates to the field of preparation of inorganic non-metallic functional materials, in particular to a preparation method of nano-layer 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 method, nucleation / crystall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/00C01B25/26C01G53/00C01G49/00C07F19/00
CPCC01B25/26C01G49/009C01G53/006C07F13/005C07F15/045C01P2002/72C01P2002/82C01P2004/03C01P2004/64C01F7/78
Inventor 唐平贵李殿卿冯拥军陈廷伟
Owner BEIJING UNIV OF CHEM TECH
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