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Preparation method of LDHs (magnesium-based layered double hydroxides)

A composite hydroxide and magnesium hydroxide technology, which is applied in chemical instruments and methods, aluminum compounds, zinc compounds, etc., can solve the problems of high energy consumption, high reaction temperature, and long heating time, and achieve simple preparation process and high reaction efficiency. Mild Conditions, Inexpensive Effects

Active Publication Date: 2016-07-13
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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  • Preparation method of LDHs (magnesium-based layered double hydroxides)
  • Preparation method of LDHs (magnesium-based layered double hydroxides)
  • Preparation method of LDHs (magnesium-based layered double hydroxides)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step A: Weigh 3.36g of calcium oxide and add it into 50g of deionized water, grind it in a ball mill for 5 minutes, and prepare A slurry.

[0026] Step B: Weigh 15.384gMgCl 2 . 6H 2 O was added to 100ml deionized water to prepare a solution, and the MgCl 2 The solution was added to the A slurry within 10 minutes, and then continued to stir and react for 2 hours. After the reaction, the magnesium hydroxide precipitate was filtered and washed until the filtrate contained no calcium ions.

[0027] Step C: take by weighing 7.5gAl(NO 3 ) 3 . 9H 2 O was added to 100ml deionized water to prepare C solution.

[0028] Step D: the magnesium hydroxide filter cake that step B obtains is formulated into the slurry that solid content is 5%, weighs 1.92g (NH 4 ) 2 CO 3 Prepare a 50ml solution and add it to the magnesium hydroxide slurry, stir evenly to obtain D slurry.

[0029] Step E: Add C solution dropwise to D slurry under stirring state, and the dropwise addition is co...

Embodiment 2

[0031] Step A, B: same as embodiment 1.

[0032] Step C: take by weighing 2.975gZn (NO 3 ) 2 . 6H 2 O and 7.5gAl(NO 3 ) 3 . 9H 2 O was added to 50ml deionized water to prepare C solution.

[0033] Step D: the magnesium hydroxide filter cake that step B obtains is formulated into the slurry that solid content is 8%, weighs 1.44g (NH 4 ) 2 CO 3 Prepare a 50ml solution and add it to the magnesium hydroxide slurry, stir evenly to obtain D slurry.

[0034] Step E: Add C solution dropwise to D slurry under agitation, and the dropwise addition is completed in 90 minutes, then heat the reaction system to 95°C and continue to stir and react for 5 hours. After the reaction, filter and wash the slurry 4 times to obtain composite hydroxide The product filter cake was dried 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 0.5 Zn 0.167 al 0.333 (OH) 2 (CO 3 ) 0.167 0.6H 2 O.

Embodiment 3

[0036] Step A, B: same as embodiment 1.

[0037] Step C: take by weighing 5.95gZn (NO 3 ) 2 . 6H 2 O and 7.5gAl(NO 3 ) 3 . 9H 2 O was added to 150ml deionized water to prepare C solution.

[0038] Step D: the magnesium hydroxide filter cake that step B obtains is mixed with the slurry that solid content is 10%, weighs 1.85g (NH 4 ) 2 CO 3 After preparing 80ml solution, add it to the magnesium hydroxide slurry, stir evenly to obtain D slurry.

[0039] Step E: Add C solution dropwise to D slurry under stirring state, and the dropwise addition is completed in 30 minutes, then heat the reaction system to 80°C and continue to stir and react for 8 hours. After the reaction is completed, filter and wash the slurry 4 times to obtain composite hydroxide The product filter cake was dried 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 0.333 Zn 0.333 al 0.333 (OH) 2 (CO 3 ) ...

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Abstract

The invention provides a preparation method of LDHs (magnesium-based layered double hydroxides). According to the method, calcium oxides or calcium magnesium oxides are used as an alkali source, calcium oxides or calcium magnesium oxides and a magnesium salt are subjected to a precipitation reaction, magnesium hydroxide precipitates are produced, then the magnesium hydroxide precipitates and divalent and trivalent soluble metal nitrates or chlorides are used as raw materials, LDHs are prepared through a liquid-solid phase reaction, and byproducts, namely, magnesium chlorides or magnesium nitrates, can be used as raw materials. The method has the advantages that the raw materials are rich in source, the price is low, the preparation process is simple, reaction conditions are mild, industrial production is facilitated and the like, and prepared LDHs can be widely applied to fields of catalysis, adsorption, environmental protection, high-polymer plastic 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 magnesium-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 method, nucleatio...

Claims

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Application Information

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IPC IPC(8): C01F7/00C01G9/00
CPCC01G9/006C01P2002/72C01P2002/82C01P2004/03C01P2002/22C01F7/782
Inventor 唐平贵陈廷伟李殿卿冯拥军
Owner BEIJING UNIV OF CHEM TECH
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