Supported carboxylation catalyst as well as preparation method and application thereof

A carboxylation catalyst and catalyst technology, applied in the direction of physical/chemical process catalyst, carboxylate preparation, molecular sieve catalyst, etc., can solve the problems of high loss rate of catalyst reuse, short service life of catalyst, high energy consumption of catalyst separation, and achieve The effect of reducing the content of impurities, prolonging the service life, and reducing production costs

Active Publication Date: 2021-07-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The catalyst used in the above reaction has high energy consumption for separation, difficulty in separation and reuse, high lo

Method used

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  • Supported carboxylation catalyst as well as preparation method and application thereof
  • Supported carboxylation catalyst as well as preparation method and application thereof
  • Supported carboxylation catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Prepare a 0.2mol / L cesium carbonate solution, use the cesium carbonate solution to perform ion exchange with hydrotalcite, the solid-to-liquid ratio is 1:10g / L, and exchange at 70°C for 2 hours. It was then filtered, washed and dried at 40°C. Repeat once. Finally, it was fired at 350° C. for 2 hours in air.

[0043] (2) Prepare a 1mol / L cesium chloride solution, use the cesium chloride solution to perform ion exchange with NaY molecular sieves, the solid-liquid ratio is 1:5 g / L, and exchange at 70°C for 2 hours. It was then filtered, washed, dried at 40°C, and finally calcined at 550°C for 2 hours in air. Repeat once.

[0044] (3) Mix 20g of modified hydrotalcite obtained in step (1), 40g of ion-exchange molecular sieve obtained in step (2), and 4g of SB powder, 0.4g of citric acid, 0.4g of nitric acid, and 20g of water in proportion, extrude, and dry Roasting to obtain a catalyst support.

[0045] (4) Prepare 2.6mol / L silver nitrate solution, immerse 50g catal...

Embodiment 2

[0047] (1) Prepare a 0.2mol / L cesium carbonate solution, use the cesium carbonate solution to perform ion exchange with hydrotalcite, the solid-to-liquid ratio is 1:10g / L, and exchange at 70°C for 2 hours. It was then filtered, washed and dried at 40°C. Repeat once. Finally, it was fired at 350° C. for 3 hours.

[0048] (2) Prepare a 1mol / L cesium chloride solution, use the cesium chloride solution to perform ion exchange with NaY molecular sieves, the solid-liquid ratio is 1:5 g / L, and exchange at 70°C for 2 hours. Then filter, wash, dry at 40°C, and finally bake at 550°C for 2 hours. Repeat once.

[0049] (3) Mix 40g of modified hydrotalcite obtained in step (1), 20g of ion-exchange molecular sieve obtained in step (2), and 8g of SB powder, 0.8g of citric acid, 0.8g of nitric acid, and 32g of water in proportion, extrude, and dry Roasting to obtain a catalyst support.

[0050] (4) Prepare 1mol / L silver nitrate solution, immerse 50g catalyst support in 20mL silver nitrat...

Embodiment 3

[0052] (1) Prepare a 0.2mol / L cesium carbonate solution, use the cesium carbonate solution to perform ion exchange with hydrotalcite, the solid-to-liquid ratio is 1:10g / L, and exchange at 70°C for 2 hours. It was then filtered, washed and dried at 40°C. Repeat once. Finally, bake at 350°C for 2 hours.

[0053] (2) Prepare 1 mol / L cesium chloride solution, use the cesium chloride solution to perform ion exchange with NaZSM-5 molecular sieve, the solid-liquid ratio is 1:5 g / L, and exchange at 70°C for 2 hours. Then filter, wash, dry at 40°C, and finally bake at 550°C for 2 hours. Repeat once.

[0054] (3) Mix 20g of modified hydrotalcite obtained in step (1), 80g of ion-exchange molecular sieve obtained in step (2), and 6g of SB powder, 1.2g of citric acid, 1.2g of nitric acid, and 60g of water in proportion, extrude, and dry Roasting to obtain a catalyst support.

[0055] (4) Prepare 1mol / L silver nitrate solution, immerse 50g catalyst support in 12mL silver nitrate soluti...

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Abstract

The invention discloses a supported carboxylation catalyst for synthesizing phenylpropiolic acid. The catalyst comprises a catalyst supporter and a supported active component; the catalyst supporter comprises modified hydrotalcite, a modified molecular sieve and aluminum oxide; the charge balance anion of the modified hydrotalcite is carbonate; the modified molecular sieve is a cation modified molecular sieve, and the cation is at least one of lithium, sodium, potassium and cesium; and the active component is selected from at least one of metal salts AgI, AgBr, AgCl, CuI, CuBr and CuCl. According to the invention, carbonate ions are utilized to modify hydrotalcite, so that the content of carbonate ions in hydrotalcite is increased; and the molecular sieve is modified by using soluble salt of assistant ions, and assistant metal ions are loaded on the molecular sieve. The catalyst disclosed by the invention has the characteristic that active components and auxiliary components are not easy to lose, the service life of the catalyst can be prolonged, and the utilization rate of the catalyst is greatly improved.

Description

technical field [0001] The invention relates to a supported carboxylation catalyst, its preparation method and application. Background technique [0002] Phenylpropiolic acid is an important raw material for the preparation of substituted alkynes by decarboxylation cross-coupling reactions. It is widely used in the synthesis of heterocyclic compounds in the organic synthesis of macromolecules, and is an important intermediate for pharmaceutical molecules. Therefore, the synthesis method of phenylpropiolic acid compounds has been widely concerned. The industrial synthesis method of phenylpropiolic acid compounds uses formaldehyde as a carboxylation reagent to carry out oxidative carboxylation reaction with phenylacetylene. However, the price of formaldehyde is relatively expensive and there are disadvantages such as inconvenient operation, so the application of the method is limited. As for the method of using Grignard reagents to prepare phenylpropiolic acid compounds, th...

Claims

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Application Information

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IPC IPC(8): B01J27/232B01J29/12B01J29/14B01J29/44C07C51/15C07C57/42
CPCB01J29/126B01J29/44B01J29/146B01J27/232C07C51/15B01J2229/20C07C57/42Y02P20/584
Inventor 张志智王陶孙潇磊韩照明刘全杰张喜文
Owner CHINA PETROLEUM & CHEM CORP
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