A kind of braided mesoporous polymer-supported silver catalyst and its preparation method and application

A catalyst and polymer technology, applied in the field of preparation of braided mesoporous polymer-supported silver catalyst, can solve the problems of reduced catalyst practicability, large metal particle size, large catalyst dosage, etc., and achieve the effect of good industrial practical application potential.

Active Publication Date: 2021-06-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the catalyst consumption is relatively large in practical application, and the conversion number (TON) of the phenylpropylic acid product is only 36, which greatly reduces the practicability of the catalyst
In the early stage, we designed and prepared an Ag / Schiff-SiO by in situ reduction method 2 Catalyst (Green Chem., 2017, 19, 2080–2085, Chinese patent application number: 201611127460.6), which can catalyze the reaction under mild conditions (60 ° C, 1 atm) and can be recycled 5 times. The catalyst is used in practical applications The amount of catalyst used in the medium is small, and the conversion number (TON) of the phenylpropiolic acid product can be raised to 706, but the Ag / Schiff-SiO 2 Catalyst metal particle size is relatively large (about 6.3nm)

Method used

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  • A kind of braided mesoporous polymer-supported silver catalyst and its preparation method and application
  • A kind of braided mesoporous polymer-supported silver catalyst and its preparation method and application
  • A kind of braided mesoporous polymer-supported silver catalyst and its preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Preparation of Ag / KAPs-P catalyst:

[0022] First in the powdered SiO containing pyrrole (3.5mL, 50mmol), 15nm 2 (15g), PPh 3 (13.13g, 50mmol), in 300mL dichloroethane of FDA (13.5mL, 150mmol), add FeCl 3 (24.38g, 150mmol); after uniform stirring at room temperature, the temperature was raised to 45°C, and reacted for 5h under the protection of argon; reacted for 67h at 80°C; after the reaction, washed 3 times with methanol, and extracted with methanol for 24h; Dry at 120°C to constant weight, then etch with 4M FH solution to remove the hard template SiO 2 , and finally a black solid powder sample was obtained, which was named KAPs-P; then 200 mg of KAPs-P carrier was weighed, added to 20 mL of acetonitrile, and dispersed uniformly by ultrasonic at room temperature. Then 1 mL of AgTCM (0.5 mg) in acetonitrile was added, and 2 mL of NaBH was added under stirring 4 (50 mg) solution, and continued stirring at room temperature for 10 min. After the suspension is separa...

Embodiment 2

[0024] Preparation of Ag / KAPs-Py Catalyst

[0025] First in the powdered SiO containing pyrrole (3.5mL, 50mmol), 15nm 2 (6g), in 300mL dichloroethane of FDA (9mL, 100mmol), add FeCl 3 (16.2g, 100mmol); after stirring evenly at room temperature, the temperature was raised to 80°C, and reacted for 12h under the protection of argon; after the reaction, washed 3 times with methanol, extracted with methanol for 24h; and dried at 120°C until constant Heavy, and then etched with 4M HF solution to remove the hard template SiO 2 , and finally a black solid powder sample was obtained, which was named KAPs-Py; then 200 mg of KAPs-Py carrier was weighed, added to 20 mL of acetonitrile, and dispersed uniformly by ultrasonic at room temperature. Then 1 mL of AgTCM (0.5 mg) in acetonitrile was added, and 2 mL of NaBH was added under stirring 4 (50 mg) solution, and continued stirring at room temperature for 10 min. After the suspension is separated and washed, the solid product is dried ...

Embodiment 3

[0027] Preparation of Ag* / KAPs-Py catalyst:

[0028] First in the powdered SiO containing pyrrole (3.5mL, 50mmol), 15nm 2 (6g), in 300mL dichloroethane of FDA (9mL, 100mmol), add FeCl 3 (16.2g, 100mmol); after stirring evenly at room temperature, the temperature was raised to 80°C, and reacted for 12h under the protection of argon; after the reaction, washed 3 times with methanol, extracted with methanol for 24h; and dried at 120°C until constant Heavy, and then etched with 4M HF solution to remove the hard template SiO 2 , and finally a black solid powder sample was obtained, which was named KAPs-Py; then 200 mg of KAPs-Py carrier was weighed, added to 20 mL of acetonitrile, and dispersed uniformly by ultrasonic at room temperature. Then add 1 mL of AgNO 3 (0.45mg) acetonitrile water (V乙腈 :V 水 =9:1) solution, and add 2mL of NaBH under the condition of stirring 4 (50 mg) solution, and continued stirring at room temperature for 10 min. After the suspension is separated an...

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Abstract

The invention relates to a preparation method of a braided mesoporous polymer-supported silver catalyst and its application in CO 2 Applications in the synthesis of alkynoic acids. The catalyst uses a braided mesoporous polymer as a carrier and nanoscale Ag as an active component, and its mass content is 0.01%-1.0%. The catalyst can efficiently catalyze CO under mild conditions 2 reaction with alkynes and CO 2 into alkynoic acid. The catalyst of the present invention has the characteristics of easy preparation, high activity and high stability, wherein the yield of phenylpropiolic acid is as high as 92%, and the initial conversion number (TON) of phenylpropiolic acid is as high as 9936, providing a catalyst for the efficient synthesis of alkynoic acid. A method with good application prospects.

Description

technical field [0001] The present invention relates to industrial emissions of CO 2 chemical conversion technology, especially a PPh 3 Preparation of modified braided mesoporous polymer-supported silver catalysts. Background technique [0002] Since alkynoic acid can be used as an important intermediate in medicinal chemistry and organic synthesis, secondly, through this technology, the emission reduction of greenhouse gases can be realized, and the CO 2 resource utilization, so CO 2 The synthesis of alkynoic acids with alkynes has attracted widespread interest. If you can break through the CO 2 The technical problem of efficient immobilization under mild conditions, and alkynes can be obtained from renewable energy sources (wind energy, solar energy, biomass energy, etc.) on a large scale, will further increase CO 2 Economic and technical feasibility of synthesizing alkynoic acids by carboxylation with alkynes. Therefore, the preparation of highly active and stable c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28C07C51/15C07C57/42C07B41/08
CPCB01J31/0267B01J31/28B01J35/006B01J37/0201B01J37/16C07B41/08C07C51/15C07C57/42
Inventor 黄延强吴志连杨小峰叶雪张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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