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A kind of clean preparation method of layered composite hydroxide

A hydroxide, layered composite technology, applied in the preparation of organic compounds, cyanide reaction preparation, oxygen/ozone/oxide/hydroxide, etc., can solve the problem of high energy consumption, long heating time and high reaction temperature problem, to achieve the effect of simple preparation process, low price and mild reaction conditions

Active Publication Date: 2017-05-24
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction temperature of this method is high, the heating time is long, the energy consumption is large, and only micron-sized LDH can be prepared.

Method used

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  • A kind of clean preparation method of layered composite hydroxide
  • A kind of clean preparation method of layered composite hydroxide
  • A kind of clean preparation method of layered composite hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step A: Weigh 8.4g of calcium oxide and add it to 100g of deionized water, grind it in a ball mill for 2 minutes to prepare a calcium oxide slurry, and then add it to reactor A; weigh 16.05g of NH 4 Cl was added to 100ml deionized water to prepare a solution and added to reactor A, and stirred evenly.

[0026] Step B: Weigh 8.12g MgCl 2 . 6H 2 O and 4.826g AlCl 3 . 6H 2 O was added to 100ml of deionized water to prepare a salt solution and added to reactor B. Weigh 6.42gNH 4 Cl was added to 100ml deionized water to prepare a solution and added to reactor B, and stirred evenly.

[0027] C: Connect reactor A and reactor B with a condensing device, heat reactor A to 100°C and reactor B to 50°C under stirring. After 3 hours, the reactor A stopped heating and closed the condensing device, heated the reactor B to 100°C, continued to stir and react for 4 hours, cooled to room temperature after the reaction, and the precipitate was washed by centrifugation until the pH ...

Embodiment 2

[0029] Step A: Weigh 8.4g of calcium oxide and add it to 80g of deionized water, grind it in a ball mill for 1 minute, prepare calcium oxide slurry, and then add it to reactor A; weigh 24g of NH 4 NO 3 Add it into 120ml deionized water to prepare a solution and add it to reactor A, and stir evenly.

[0030] Step B: Weigh 12.18g MgCl 2 . 6H 2 O and 4.826g AlCl 3 . 6H 2 O was added to 100ml of deionized water to prepare a salt solution and added to reactor B. Weigh 2.64g (NH 4 ) 2 SO 4 Add it to 50ml deionized water to make a solution and add it to reactor B, and stir evenly.

[0031] C: Connect reactor A and reactor B with a condensing device, heat reactor A to 90°C and reactor B to 60°C under stirring. After 6 hours, the reactor A stopped heating and closed the condensing device, heated the reactor B to 90°C, continued to stir and react for 3 hours, cooled to room temperature after the reaction, the precipitate was washed by centrifugation until the pH value was les...

Embodiment 3

[0033] Step A: Same as Example 2.

[0034] Step B: with embodiment 2, difference is to take by weighing 1.92g (NH 4 ) 2 CO 3 Instead of the used (NH 4 ) 2 SO 4 .

[0035] C: Connect reactor A and reactor B with a condensing device, heat reactor A to 95°C and reactor B to 50°C under stirring. After 5 hours, stop the heating of reactor A and close the condensing device, heat reactor B to 80 ° C, continue to stir for 4 hours, 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 placed in Dry in an oven at 100°C for 12 hours to obtain the LDH product. Elemental analysis shows that the chemical composition formula of the product is: Mg 0.75 Al 0.25 (OH) 2 (CO 3 ) 0.125 0.8H 2 O.

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Abstract

The invention provides a clean preparation method of layered composite hydroxide, which uses divalent and trivalent soluble metal nitrates or chlorides as raw materials for building LDH laminates, calcium oxide as an alkali source, and chloride Ammonium or ammonium nitrate is used as the circulating medium, and the ammonia water generated by the reaction of calcium oxide and ammonium chloride or ammonium nitrate is used as the precipitating agent to precipitate divalent and trivalent soluble metal nitrates or chlorides to form high-purity layered composite hydroxide The by-product ammonium chloride or ammonium nitrate can be recycled, and calcium chloride or calcium nitrate can be used as industrial raw materials. The preparation process has no waste discharge and is environmentally friendly. The method has the advantages of rich source of raw materials, low price, simple preparation process, mild reaction conditions, and easy industrial production. The prepared LDH can be widely used in the fields of catalysis, adsorption, environmental protection, polymer plastics and the like.

Description

technical field [0001] The invention relates to the field of preparation of inorganic non-metal functional materials, in particular to a clean preparation method of layered composite hydroxide. Background technique [0002] 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). [0003] LDH is usually prepared by co-precipitation method, nucleation / cryst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B13/36C01F7/00C01B25/45C07C227/18C07C229/60C07C303/32C07C309/04C07C51/41C07C65/10C07C53/124
CPCC01B13/36C01B25/45C07C51/412C07C227/18C07C303/32C01P2002/72C01P2002/82C01P2004/03C01F7/785C01F7/78C07C229/60C07C309/04C07C65/10C07C53/124
Inventor 唐平贵李殿卿冯拥军陈廷伟
Owner BEIJING UNIV OF CHEM TECH
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