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Catalyst for synthesizing phenylpropiolic acid and preparation method and application of catalyst

A technology of phenylpropiolic acid and catalyst, which is applied in the direction of catalyst activation/preparation, organic compound preparation, carboxylate preparation, etc. It can solve the problems of restricting reaction economy, loss of catalyst and additives, short service life of catalyst, etc.

Active Publication Date: 2020-07-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, the catalyst and auxiliary agent used in the reaction are seriously lost, and the service life of the catalyst is very short, which seriously restricts the economy of the reaction

Method used

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  • Catalyst for synthesizing phenylpropiolic acid and preparation method and application of catalyst
  • Catalyst for synthesizing phenylpropiolic acid and preparation method and application of catalyst
  • Catalyst for synthesizing phenylpropiolic acid and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Prepare a 1mol / L silver nitrate solution, impregnate 50g of hydrotalcite in 20mL of silver nitrate solution, dry for 24 hours, and then bake at 200°C for 5 hours. Prepare 1mol / L sodium iodide solution, immerse the hydrotalcite loaded with silver nitrate in 20mL sodium iodide solution, dry for 24 hours, and then bake at 120°C for 24 hours.

[0048] (2) Prepare a 0.2 mol / L cesium carbonate solution, use the cesium carbonate solution to carry out ion exchange with silver iodide-loaded hydrotalcite, the solid-to-liquid ratio is 1:10 g / 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 150° C. for 2 hours.

[0049] (3) Prepare a 1 mol / 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. ...

Embodiment 2

[0052] (1) Prepare 2mol / L silver acetate solution, impregnate 50g hydrotalcite in 20mL silver acetate solution, dry for 24 hours, and then bake at 200°C for 5 hours. Prepare 2mol / L potassium chloride solution, immerse the hydrotalcite loaded with silver acetate in 20mL potassium chloride solution, dry for 24 hours, and then bake at 180°C for 8 hours.

[0053] (2) Prepare a 1 mol / L cesium carbonate solution, use the cesium carbonate solution to carry out ion exchange with silver chloride-loaded hydrotalcite, the solid-to-liquid ratio is 1:5 g / L, and exchange at 50°C for 6 hours. It was then filtered, washed and dried at 40°C. Repeat 2 times. Finally, it was fired at 150° C. for 2 hours.

[0054] (3) Prepare a 0.1mol / L cesium chloride solution, use the cesium chloride solution to perform ion exchange with NaY molecular sieves, the solid-liquid ratio is 1:10 g / L, and exchange at 40°C for 12 hours. Then filter, wash, dry at 40°C, and finally bake at 400°C for 12 hours. Repeat ...

Embodiment 3

[0057] (1) Prepare 1.5mol / L cuprous nitrate solution, immerse 50g hydrotalcite in 20mL cuprous nitrate solution, dry for 24 hours, and then bake at 200°C for 5 hours. A 1.5 mol / L cesium iodide solution was prepared, and the hydrotalcite loaded with cuprous nitrate was immersed in 20 mL of the cesium iodide solution, dried for 24 hours, and then calcined at 200°C for 2 hours.

[0058] (2) Prepare 0.6 mol / L sodium carbonate solution, use sodium carbonate solution to carry out ion exchange with cuprous iodide-loaded hydrotalcite, the solid-liquid ratio is 1:8 g / L, and exchange at 40°C for 10 hours. It was then filtered and dried at 40°C. Repeat once. Finally, it was fired at 150° C. for 2 hours.

[0059] (3) Prepare a 0.5mol / L cesium chloride solution, use the cesium chloride solution to perform ion exchange with NaY molecular sieves, the solid-liquid ratio is 1:6 g / L, and exchange at 70°C for 2 hours. It was then filtered, dried at 40°C, and finally calcined at 600°C for 4 ho...

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PUM

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Abstract

The invention discloses a catalyst for synthesizing phenylpropiolic acid. The catalyst comprises hydrotalcite loaded with active metal salt and an ion exchange type molecular sieve, wherein the activemetal salt is selected from at least one of AgI, AgBr, AgCl, CuI, CuBr and CuCl, the ion exchange type molecular sieve is a cation exchange type molecular sieve, and the cation is at least one of lithium, sodium, potassium and cesium. The catalyst disclosed by the invention has the characteristics of high active center dispersity and low possibility of loss, and is used in a phenylpropiolic acidsynthesis process, so that the content of impurities in a product is reduced, the difficulty of post-treatment such as separation and refining is reduced, and generated wastes are greatly reduced.

Description

technical field [0001] The invention relates to a catalyst for synthesizing phenylpropiolic acid, a preparation method and application thereof. Specifically, it is a heterogeneous catalyst that catalyzes phenylacetylene and CO 2 A method for preparing phenylpropiolic acid by carboxylation. Background technique [0002] Phenylpropiolic acid is a white crystalline powder at room temperature. It is an important intermediate for the synthesis of fine chemicals and pharmaceutical molecules, such as the synthesis of heterocyclic compounds such as coumarin and flavones through cycloaddition and other reactions; in addition, they are also one of the important raw materials for the preparation of substituted alkynes by decarboxylation cross-coupling reactions. Therefore, the synthesis of phenylpropylic acid compounds has been widely concerned. In the prior art, the method for synthesizing phenylpropiolic acid compounds is mainly the oxidative carboxylation reaction of phenylacetyl...

Claims

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Application Information

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IPC IPC(8): C07C51/15C07C57/42B01J29/03B01J29/04B01J29/12B01J29/14B01J29/46B01J29/76B01J37/02B01J37/08B01J37/30
CPCC07C51/15B01J37/0201B01J37/082B01J37/30B01J29/126B01J29/146B01J29/46B01J29/0325B01J29/043B01J29/7615B01J2229/18C07C57/42Y02P20/584
Inventor 张志智王陶孙潇磊尹泽群刘全杰方向晨
Owner CHINA PETROLEUM & CHEM CORP
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