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Preparation method and application of a temperature-sensitive interface catalyst

A catalyst and interface technology, applied in the field of temperature-sensitive interface catalysts, to achieve the effects of emulsion breaking and catalyst separation and recovery

Active Publication Date: 2021-02-02
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention is difficult for polyoxometalates to use H 2 o 2 or O 2 To solve the problem of good catalytic performance in the emulsion catalytic oxidation system of oxidants, a preparation method of a temperature-sensitive interfacial catalyst and its application in alcohol oxidation reactions are provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve 1 mmol of a hyperbranched amphiphilic polymer with a molecular weight of 3000 and an HLB value of 14 (the number of terminal hydroxyl groups is 3 mmol) in 100 mL of tetrahydrofuran, then add 0.3 mmol of Dess-Martin reagent, react at room temperature for 24 hours, and precipitate in ether The product was obtained, dried in vacuo, dissolved in 100mL of absolute ethanol, added 3mmol trimethylolaminomethane, refluxed for 4h, cooled to room temperature, added 4.5mmol sodium borohydride, reacted for 24h, precipitated in ether product, vacuum-dried, then the product was added to 100mL of N,N-dimethylformamide, and then 3mmol of (Bu 4 N)H 4 P 2 V 3 W 15 o 62 , reacted at 60°C for 10 days, precipitated the product in ether after cooling, and dried in vacuum to obtain the temperature-sensitive interfacial catalyst.

[0021] 50mmol benzyl alcohol and 250mmol water were added to a 50mL airtight reaction vessel; then 60mmol H 2 o 2 Into the above reaction system; the...

Embodiment 2

[0023] Dissolve 1mmol of a hyperbranched amphiphilic polymer with a molecular weight of 9800 and an HLB value of 30 (the number of terminal hydroxyl groups is 24mmol) in 100mL of tetrahydrofuran, then add 12mmol of Dess-Martin reagent, react at room temperature for 12h, and precipitate in ether The product was vacuum-dried, and the product was dissolved in 100 mL of absolute ethanol, and 24 mmol of trimethylolaminomethane was added, and refluxed for 12 hours. After cooling to room temperature, 60 mmol of sodium borohydride was added and reacted for 4 hours, and the product was precipitated in ether. Vacuum drying, then the product was added to 100mL of N,N-dimethylformamide, and then 48mmol of (Bu 4 N)H 4 P 2 V 3 W 15 o 62 , reacted at 90°C for 3 days, precipitated the product in ether after cooling, and dried in vacuum to obtain the temperature-sensitive interfacial catalyst.

[0024] Add 50mmol benzyl alcohol and 1000mmol water to a 50mL airtight reactor; then add 60mmo...

Embodiment 3

[0026] Dissolve 1 mmol of a hyperbranched amphiphilic polymer with a molecular weight of 15,000 and an HLB value of 22 (the number of terminal hydroxyl groups is 48 mmol) in 100 mL of tetrahydrofuran, then add 10 mmol of Dess-Martin reagent, react at room temperature for 24 hours, and precipitate in ether The product was vacuum-dried, and the product was dissolved in 100 mL of absolute ethanol, and 48 mmol of trimethylolaminomethane was added, and the reaction was refluxed for 12 hours. After cooling to room temperature, 90 mmol of sodium borohydride was added, and the product was reacted for 8 hours, and the product was precipitated in ether. Vacuum drying, then the product was added to 100mL of N,N-dimethylformamide, and then 60mmol of (Bu 4 N)H 4 P 2 V 3 Mo 15 o 62 , reacted at 70°C for 10 days, precipitated the product in ether after cooling, and dried in vacuum to obtain the temperature-sensitive interfacial catalyst.

[0027] 50mmol benzyl alcohol and 500mmol water ...

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Abstract

A method for preparing a temperature-sensitive interface catalyst and its application, belonging to the technical field of temperature-sensitive interface catalysts, can solve the problem that polyoxometalates are difficult to use in H 2 o 2 or O 2 The problem of showing good catalytic performance in the emulsion catalytic oxidation system of the oxidizing agent, the preparation method of the catalyst comprises: modifying the end group of a multi-branched amphiphilic polymer with terminal hydroxyl groups, and preparing a polymer whose terminal group is trimethylol matter; the trimethylol-terminated polymer is reacted with a polyoxometalate to obtain the interfacial catalyst of the present invention. The catalyst can be adsorbed at the oil-water interface of the emulsion, and catalyze the oxidation reaction of alcohol at the interface of the emulsion, and the separation and recovery of the catalyst can also be realized by changing the temperature.

Description

technical field [0001] The invention belongs to the technical field of temperature-sensitive interface catalysts, and in particular relates to a preparation method of an interface catalyst with temperature-sensitive performance and its application in emulsion catalytic oxidation. Background technique [0002] Polyoxometalates are a class of polyoxometallic cluster compounds with fixed nanometer size and spatial structure composed of early transition metal atoms and oxygen atoms. Polyoxometalates are both acidic and oxidizing, and have a unique coordination ability, so they become one of the important catalysts in the process of acid catalysis and oxidation catalysis. However, in the multiphase system of organic substrate-water, the area of ​​the organic phase / water phase interface is an important factor affecting this type of reaction, and polyoxometalates cannot be effectively adsorbed on the organic phase / water phase interface, so it is difficult to Show good catalytic pe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/18C07C45/29C07C47/54C07C49/403C07C49/04C07C49/213
CPCB01J31/069B01J2231/763C07C45/294C07C2601/14C07C47/54C07C49/403C07C49/04C07C49/213
Inventor 张越白雪丽黄鑫温亮薛丹丹赵永祥
Owner SHANXI UNIV
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