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Synthesis method of catalyst capable of realizing catalytic oxidation reaction of organic matter in aqueous phase

A technology for catalytic oxidation and synthesis methods, which is applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, catalytic reactions, etc., and can solve problems such as difficult separation of organic products and solvents, and difficulty in reusing catalysts. , to achieve the effect of reuse

Inactive Publication Date: 2018-08-17
NANYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this type of system has some obvious disadvantages: (1) this type of catalyst is insoluble in water and easily soluble in organic solvents, so the reaction system needs to use a large amount of toxic organic solvents; (2) the catalyst is soluble in organic solvents during the reaction, After the reaction, the reuse of the catalyst is difficult; (3) the organic product obtained is difficult to separate from the solvent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The present invention is a kind of synthetic method that can realize the catalyst of organic matter catalytic oxidation reaction in water phase, adopts following method to synthesize:

[0020] Put 2.7 mmol of K 8 [SiW 10 O 36 ]·12H 2 O was rapidly dissolved in 2.8 mL of 1 M HCl, followed by the addition of 1.1 mL of 0.5 M NaVO 3 Aqueous solution, the mixture was stirred for 5 minutes to obtain a clear filtrate by suction filtration, i.e., silicotungsten alum-type polyoxometalates ([γ-1,2-H 2 SiV 2 W 10 O 40 ] 4- ) aqueous solution. 10.8 mmol of 3-(N,N-dimethylhexadecylammonium)-propanesulfonate was added to the filtrate, then 10 mL of absolute ethanol was added, and after stirring for half an hour, a yellow solid was obtained by suction filtration. The catalyst was washed three times with water and ethanol, and air-dried to obtain the catalyst.

[0021] A stable emulsion was formed with 5 μmol of catalyst, 2 mmol of thioanisole, 6 mmol of 30% hydrogen peroxide i...

Embodiment 2

[0023] The present invention is a kind of synthetic method that can realize the catalyst of organic matter catalytic oxidation reaction in water phase, adopts following method to synthesize:

[0024] Put 5.4 mmol of K 8 [SiW 10 O 36 ]·12H 2 O was rapidly dissolved in 5.6 mL of 1 M HCl, followed by the addition of 2.2 mL of 0.5 M NaVO 3 Aqueous solution, the mixture was stirred for 5 minutes to obtain a clear filtrate by suction filtration, i.e., silicotungsten alum-type polyoxometalates ([γ-1,2-H 2 SiV 2 W 10 O 40 ] 4- ) aqueous solution. 21.6 mmol of 3-(N,N-dimethylhexadecylammonium)-propanesulfonate was added to the filtrate, and then 20 mL of absolute ethanol was added, and after stirring for half an hour, a yellow solid was obtained by suction filtration. The catalyst was washed three times with water and ethanol, and air-dried to obtain the catalyst.

[0025] A stable emulsion was formed by combining 10 μmol of catalyst, 4 mmol of thioanisole, 12 mmol of 30% hyd...

Embodiment 3

[0027] The present invention is a kind of synthetic method that can realize the catalyst of organic matter catalytic oxidation reaction in water phase, adopts following method to synthesize:

[0028] 8.1 mmol of K 8 [SiW 10 O 36 ]·12H 2 O was rapidly dissolved in 8.4 mL of 1 M HCl, followed by the addition of 3.3 mL of 0.5 M NaVO 3 Aqueous solution, the mixture was stirred for 5 minutes to obtain a clear filtrate by suction filtration, i.e., silicotungsten alum-type polyoxometalates ([γ-1,2-H 2 SiV 2 W 10 O 40 ] 4- ) aqueous solution. 32.4 mmol of 3-(N,N-dimethylhexadecylammonium)-propanesulfonate was added to the filtrate, and then 30 mL of absolute ethanol was added, and after stirring for half an hour, a yellow solid was obtained by suction filtration. The catalyst was washed three times with water and ethanol, and air-dried to obtain the catalyst.

[0029] A stable emulsion was formed with 15 μmol of catalyst, 6 mmol of thioanisole, 18 mmol of 30% hydrogen peroxi...

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PUM

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Abstract

The invention provides a method for synthesizing a catalyst capable of realizing a catalytic oxidation reaction of organic matters in an aqueous phase. The method comprises the following steps: combining divanadium-substituted silicon tungsten alum polyoxometallate negative ions with 3-(N,N-dimethylhexadecylammonium)-propyl sulfonate in an acidic aqueous phase according to a molar ratio of 1:4, thereby obtaining the catalyst. The catalyst has excellent dispersity in the aqueous phase, and in the reaction process, the composite catalyst can form an emulsion system with aqueous solution, hydrogen peroxide oxidant and organic substrates. The catalyst synthesized by the invention can be used for developing a green catalytic oxidation system which can be repeatedly used.

Description

technical field [0001] The invention relates to a catalyst for chemical reaction, in particular to a method for synthesizing a catalyst capable of realizing the catalytic oxidation reaction of organic matter in an aqueous phase. Background technique [0002] Polyoxometalates (POMs) are a class of polyoxometallic compounds formed by the connection of pre-transition metal ions through oxygen. The range of polyoxometalates is mainly high-valence pre-transition metals (mainly V, Nb, Ta, Mo, W), which have the ability to form metal-oxygen cluster anions. Related research has also formed a popular subject - polyacid chemistry. Early polyacid chemistry believed that polyacid is a class of compounds obtained by the condensation and dehydration of two or more inorganic oxoacid anions, which can be divided into homopolyacids and heteropolyacids according to different compositions. [1] . The development of polyoxometalate chemistry has a history of nearly 200 years, and its related ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/36C07C315/02C07C317/14
CPCB01J31/36B01J2231/70C07C315/02C07C317/14
Inventor 赵伟杨春霞
Owner NANYANG NORMAL UNIV