Preparation method of stripping type hydrotalcite

A hydrotalcite and exfoliation type technology, applied in the field of preparation of exfoliated hydrotalcite, can solve the problems of incomplete exchange, harsh conditions, time-consuming and laborious, etc., and achieve the effects of uniform product structure, simple process and easy operation.

Inactive Publication Date: 2014-01-01
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN101913569B discloses a simple hydrotalcite stripping method, which uses hydrogen peroxide solution as a medium, but this method can only prepare LDHs containing metals that cannot be oxidized by hydrogen peroxide, and the use has certain limitations
CN101845241A discloses a preparation method and application of exfoliated hydrotalcite. In this invention, ethylene acrylic acid random copolymer must be added to disperse LDHs with macromolecules, otherwise the material cannot be completely exfoliated, and due to the introduction of macromolecular materials, The stripped LDHs cannot be used as catalyst supports
The process conditions are harsh, time-consuming and labor-intensive, and the economic consumption is huge
In the peeling process, the simpler the interlayer anions are, the easier they are to volatilize, and the laminates are more likely to be peeled off, and it is difficult for simple ions to replace carbonate ions. Therefore, the method disclosed in CN101734679A is often incompletely exchanged when ion-exchanging pillars, making Some hydrotalcites are difficult to be stripped, and the application has certain limitations, which limits the industrial production and application of hydrotalcite stripping

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Using commercially available hydrotalcite, place the hydrotalcite in a muffle furnace and calcinate it at 250°C for 12 hours to make a layered double hydroxyl compound metal oxide (LDO); weigh 4g of the obtained product and add it to a volume of 100mL , in a sodium formate solution with a concentration of 20mmol / L, precipitate, separate, wash, and dry under vacuum at 60°C; put the obtained product in a microwave oven, 100W, and heat for 5min to obtain a peeled hydrotalcite product.

Embodiment 2

[0018] Using self-made magnesium-aluminum hydrotalcite, put the hydrotalcite in a muffle furnace, and calcined it at 400°C for 1 hour to make a layered double hydroxyl compound metal oxide (LDO); weigh 4g of the obtained product and add it to the volume 50 mL of sodium formate solution with a concentration of 1 mol / L, precipitate, separate, wash, and dry in vacuum at 70°C; put the obtained product in a microwave oven at 700W, and heat for 1 min to obtain the exfoliated hydrotalcite product.

Embodiment 3

[0020] Using commercially available or self-made hydrotalcite, place the hydrotalcite in a muffle furnace and calcinate at 300°C for 8 hours to make a layered double hydroxyl compound metal oxide (LDO); weigh 4g of the obtained product and add it to the The volume is 80mL, the concentration is 100mmol / L sodium formate solution, precipitation separation, washing, vacuum drying at 60°C; put the obtained product in a microwave oven, 500W, and heat for 3min to obtain the exfoliated hydrotalcite product.

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PUM

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Abstract

The invention discloses a preparation method of stripping type hydrotalcite. The preparation method comprises the steps of calcining commercially available or self-made hydrotalcite into in a muffle furnace to prepare layered dihydroxy composite metal oxide; adding the layered dihydroxy composite metal oxide into an organic acid salt solution by using the memory effect of hydrotalcite, performing precipitation separation, washing and vacuum drying, then putting the product into a microwave oven, and heating by using a microwave technology to ensure that hydrotalcite is stripped and a stripped hydrotalcite product is obtained. The preparation method is simple in process, easy in operation and loose in condition, and the obtained product is uniform in structure.

Description

technical field [0001] The invention relates to a preparation method of exfoliated hydrotalcite, which belongs to the field of preparation of catalytic materials. Background technique [0002] Hydrotalcite-like compounds (LDHs) are compounds formed by the accumulation of interlayer anions and positively charged laminates. The general formula of hydrotalcite chemical structure is: [M 2+ 1-x m 3+ x(OH) 2 ] x+ [(A n- ) x / n mH 2 O], where M 2+ and M 3+ are the divalent and trivalent metal cations, such as Mg, located on the host laminates, respectively 2+ 、Ni 2+ , Zn 2+ , Mn 2+ 、Cu 2+ 、Co 2+ , Pd 2+ , Fe 2+ Equal divalent cations and Al 3+ 、Cr 3+ 、Co 3+ , Fe 3+ and other trivalent cations can form hydrotalcite; A n– It is an interlayer anion, which can include inorganic anion, organic anion, complex anion, same polyanion and heteropolyanion; x is M 3+ / (M 2+ +M 3+ ) The molar ratio is about 4:1 to 2:1; m is the number of interlayer water molecules. Its ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/14C01F7/02
Inventor 马建锋李良银姚超李定龙
Owner CHANGZHOU UNIV
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