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Supported organic Cu(I) catalyst and preparation method and application thereof

A supported, catalyst technology, applied in the direction of organic compound/hydride/coordination complex catalysts, catalysts, catalytic reactions, etc., can solve the problems of polluting the environment, unable to reuse, and difficult to purify products.

Active Publication Date: 2017-09-19
深圳市冠华特化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0002] The Glaser reaction is one of the main methods for the coupling of terminal alkynes to prepare diynes. The traditional Glaser reaction mainly uses cuprous halide (CuX) as a catalyst. When cuprous halide is used as a catalyst for Glaser reaction, the product is not easy to purify and the catalyst is not easy to recycle. It cannot be reused; and the use of cuprous halide as a catalyst to catalyze the Glaser reaction requires long-term heating in an organic solvent, which not only pollutes the environment, but also consumes high energy

Method used

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  • Supported organic Cu(I) catalyst and preparation method and application thereof
  • Supported organic Cu(I) catalyst and preparation method and application thereof
  • Supported organic Cu(I) catalyst and preparation method and application thereof

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preparation example Construction

[0031] The invention provides a kind of preparation method of supported organic Cu (I) catalyst, comprises the following steps:

[0032] Carrying out the first grafting reaction of acidified attapulgite and mercaptosilane coupling agent in a benzene solvent to obtain mercapto-modified attapulgite;

[0033] Carrying out the second grafting reaction of the mercapto-modified attapulgite and isatoic anhydride in an alcohol solvent to obtain isatoic anhydride-mercapto-modified attapulgite;

[0034] The isatic anhydride-mercapto-modified attapulgite and cuprous halide are subjected to complexation and coordination reaction in an alcohol solvent to obtain a supported organic Cu(I) catalyst.

[0035] In the invention, acidified attapulgite (HATP) and mercaptosilane coupling agent are subjected to a first grafting reaction in a benzene solvent to obtain mercapto-modified attapulgite (SH-HATP). In the present invention, the pH value of the acidified attapulgite is preferably 2 to 4, mo...

Embodiment 1

[0074] Weigh 12g of attapulgite (ATP) into a 100mL three-necked flask, add 60mL of 4mol / L hydrochloric acid solution, disperse under ultrasonic waves for 20min, stir and reflux at 70°C for 24h, suction filter after the reaction, and add a small amount of deionized Dissolve in water, adjust the pH to about 3 with 2mol / L NaOH solution, and vacuum dry at 100°C to obtain a light yellow solid, which is acidified attapulgite (HATP);

[0075] Weigh 10g of acidified attapulgite into a 50mL flask, add 25mL of xylene, slowly add 2mL of γ-mercaptopropyltrimethoxysilane dropwise under stirring, disperse under ultrasonic waves for 20min, stir and reflux at 60°C for 4h, and filter the product with suction After separation, wash with xylene, absolute ethanol and deionized water in sequence, and vacuum dry at 100°C to obtain mercapto-modified attapulgite (SH-HATP);

[0076] Weigh 10g SH-HATP in a 50mL flask, add it to 25mL ethanol, disperse under ultrasonic wave for 20min, then add 2.5g isatoic...

Embodiment 2

[0083] The acidified attapulgite (HATP) that is 3.5 is prepared according to the method for embodiment 1 pH;

[0084] Weigh 10g of acidified attapulgite into a 50mL flask, add 30mL of benzene, slowly add 2mL of γ-mercaptopropyltriethoxysilane dropwise under stirring, disperse under ultrasonic waves for 25min, stir and reflux at 65°C for 3.5h, the product is pumped After filtration and separation, it was washed with benzene, absolute ethanol and deionized water in sequence, and vacuum-dried at 100°C to obtain mercapto-modified attapulgite (SH-HATP);

[0085] Weigh 10g of SH-HATP in a 50mL flask, add it to 30mL of methanol, disperse under ultrasonic waves for 20min, then add 2.5g of isatoic anhydride, stir and reflux at 75°C for 9h, the product is separated by suction filtration, washed with ethanol, and dried at room temperature , to obtain isatoic anhydride-mercapto modified attapulgite (ATBA-SH-HATP);

[0086] Weigh 3g of ATBA-SH-HATP into a 50mL flask, add 15mL of ethanol, ...

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Abstract

The invention provides a supported organic Cu(I) catalyst and a preparation method and application thereof. The preparation method provided by the invention comprises the following steps: modifying attapulgite by using a mercapto-silane coupling agent and isatoic anhydride to obtain isatoic anhydride-mercapto modified attapulgite, and enabling cuprous ions to be supported onto the isatoic anhydride-mercapto modified attapulgite through coordination to obtain the supported organic Cu(I) catalyst. The supported organic Cu(I) catalyst provided by the invention is high in catalytic activity and easy to separate, and can be repeatedly used, and supported organic Cu(I) catalyst is capable of catalyzing Glaser coupling reaction in an aqueous phase, and the reaction can be completed through short microwave heating.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a supported organic Cu(I) catalyst and its preparation method and application. Background technique [0002] The Glaser reaction is one of the main methods for the coupling of terminal alkynes to prepare diynes. The traditional Glaser reaction mainly uses cuprous halide (CuX) as a catalyst. When cuprous halide is used as a catalyst for Glaser reaction, the product is not easy to purify and the catalyst is not easy to recycle. It cannot be reused; and the use of cuprous halide as a catalyst to catalyze the Glaser reaction requires long-term heating in an organic solvent, which not only pollutes the environment, but also has high energy consumption. Contents of the invention [0003] In view of this, the object of the present invention is to provide a supported organic Cu(I) catalyst and its preparation method and application. The supported organic Cu(I) catalyst provided by t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26C07C2/76C07C15/50
CPCB01J31/1633B01J31/226B01J31/26B01J2231/4205B01J2531/16C07C2/76C07C2531/26C07C15/50
Inventor 赵朴素朱凤霞孙小军安礼涛高秀梅
Owner 深圳市冠华特化新材料有限公司
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