Amphiphilic type rare earth polyacid catalytic material and preparation method and application thereof

A rare earth polyacid and catalytic material technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problems of low product quality and poor technical level, etc. Achieve the effect of improving solubility, solving solidification and catalyst recovery

Inactive Publication Date: 2013-02-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the production of epoxy resin is still monopolized by several large foreign companies, while small Chinese enterprises have defects such as poor technical level and low product quality.

Method used

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  • Amphiphilic type rare earth polyacid catalytic material and preparation method and application thereof
  • Amphiphilic type rare earth polyacid catalytic material and preparation method and application thereof
  • Amphiphilic type rare earth polyacid catalytic material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. Add 26mmol Na 2 WO 4 2H 2 O was dissolved in 20ml of water, and 2.5mmol LaCl dissolved in it was added dropwise 3 ·7H 2 In the hot aqueous solution of O, adjust the pH=7.0-7.5 with acetic acid.

[0022] b. Stir at a temperature of 90°C to a colorless clear solution. Then the solution was cooled to room temperature, and then cooled and crystallized at 3°C ​​to obtain Na 9 [LaW 10 o 36 ].

[0023] c. Take 0.27mmol of Na 9 [LaW 10 o 36 ] was dissolved in 10-20ml water, 2.3mmol of DDA-Br was dissolved in chloroform, and Na 9 [LaW 10 o 36 ] solution was dropped into chloroform solution and stirred at room temperature for 2h. ;

[0024] d. After the reaction is completed, add water to extract 3-5 times, take the organic layer and suspend the solution to obtain a colorless solid, which is DDA 9 [LaW 10 o 36 ].6H 2 O(DDA-LaW 10 ).

Embodiment 2

[0026] a. Add 26mmol Na 2 WO 4 2H 2O was dissolved in 20ml of water, and 2.6mmol CeCl dissolved in it was added dropwise 3 ·6H 2 In the hot aqueous solution of O, adjust the pH=7.0-7.5 with acetic acid.

[0027] b. Stir at a temperature of 90°C until a colorless clear solution is obtained. Then the solution was cooled to room temperature, and then cooled and crystallized at 3°C ​​to obtain Na 9 [ 10 o 36 ].

[0028] c. Take 0.28mmol of Na 9 [ 10 o 36 ] was dissolved in 10-20ml water, 2.7mmol of DDA-Br was dissolved in chloroform, and Na 9 [ 10 o 36 ] solution was dropped into chloroform solution and stirred at room temperature for 2h. ;

[0029] d. After the reaction is completed, add water to extract 3-5 times, take the organic layer and suspend the solution to obtain a colorless solid, which is DDA 9 [ 10 o 36 ].4H 2 O(DDA-CeW 10 ).

[0030] Catalyzed reaction embodiment 1

[0031] The catalytic reaction is carried out in a simple glass reactor with mag...

Embodiment 2

[0039] The amphiphilic rare earth multi-acid composite material prepared in Example 1 is selected as a catalyst to carry out the catalytic reaction of epoxidation reaction to different reaction substrates. The experimental conditions are the same as those in Catalytic Reaction Example 1, and the catalytic results are shown in Table 3. As can be seen from the table, for different reaction substrates, the selectivity of the catalytic reaction is still maintained, and the conversion rate of the corresponding reaction product epoxide is greatly improved.

[0040] table 3:

[0041] catalyst

[0042] Na 9 [LaW 10 o 36 ]

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Abstract

The invention relates to an amphiphilic type rare earth polyacid catalytic material and a preparation method and application thereof and belongs to the technical field of organic and inorganic composite materials. A chemical general formula is DDA9[MW10O36].Nh2o, and preparation steps comprise firstly preparing rare earth polyacid; preparing a polyacid solution; and wrapping the rare earth polyacid by using a cationic surface active agent through ion exchange reaction. The catalytic agent has good catalytic performance caused by lewis acid-base property specific to the rare earth polyacid, and introduction of the cationic surface active agent enables the catalytic agent to have hydrophilic and oleophilic characters. Simultaneously surface active agent groups in the catalytic agent quicken contact between substrate molecules and hydrogen peroxide and central polyacid portions. The amphiphilic type polyacid catalytic agent is used for enolic epoxidation reaction with a hydrogen peroxide water solution to serve as a hydrogen peroxide, and the amphiphilic type polyacid catalytic agent has high catalytic activity and high selectivity of epoxy products.

Description

technical field [0001] The invention belongs to the technical field of organic-inorganic composite materials, and in particular relates to a preparation method of an amphiphilic rare earth polyacid catalyst material and its application in the epoxidation reaction of enol in liquid phase. Background technique [0002] Polyacid compounds are a class of multimetal oxides containing V, Mo, W and other metals. Isopolyanions formed by the condensation of the same oxoacid ions are called isopolyacids. The condensation of different types of oxyacid anions is called heteropolyanion, and the acid is called heteropolyacid. At present, it is known that the atoms of nearly 70 kinds of elements can be used as heteroatoms in heteropolyacids, including all the first series transition elements, almost all the second and third series transition elements, plus B, Al, Ga, Si , Ge, Sn, P, As, Sb, Bi, Se, Te, I, etc. And each heteroatom can often exist in heteropolyanions in different valence ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/16C07D301/12
CPCY02P20/50
Inventor 宋宇飞刘璐肖亚萍
Owner BEIJING UNIV OF CHEM TECH
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