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Synthetic method of propiolic acid

A synthesis method and technology of propynoic acid, applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation and other directions, can solve the problems of high price of propargyl alcohol, high production process cost, unfriendly environment, 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

[0006] The current production process uses corrosive sulfuric acid and chromic anhydride, and the process is not environmentally friendly
And the price of propynyl alcohol is higher, causes the cost height of production process

Method used

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  • Synthetic method of propiolic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 160ml (3mol) of acetonitrile, 53g (0.5mol) of sodium carbonate and 54g (0.5mol) of phenolic resin microspheres into the reaction kettle and stir evenly. Then 32g (0.5mol) of calcium carbide and 7.9g (3%) of cuprous iodide were added to the reactor, and the reactor was filled with carbon dioxide. Heat and pressurize the reaction. Reaction temperature is 60 ℃, and reaction pressure is 2MPa. The reaction time was 18 hours. After the reaction, the mixture was filtered to separate the liquid, and then acidified with sulfonic acid resin to obtain the product. The product was analyzed by liquid chromatography, and the yield of propiolic acid was 96 mol%.

Embodiment 2

[0029] Put 320ml (6mol) of acetonitrile, 27g (0.25mol) of sodium carbonate and 27g (0.25mol) of phenolic resin microspheres into the reaction kettle and stir evenly. Then 16g (0.25mol) of calcium carbide and 5.9g (3%) of cuprous iodide were added to the reactor, and the reactor was filled with carbon dioxide. Heat and pressurize the reaction. Reaction temperature is 60 ℃, and reaction pressure is 2MPa. The reaction time was 18 hours. After the reaction, the mixture was filtered to separate the liquid, and then acidified with sulfonic acid resin to obtain the product. The product was analyzed by liquid chromatography, and the yield of propiolic acid was 95% mol.

Embodiment 3

[0031] Put 160ml (3mol) of acetonitrile, 159g (0.75mol) of sodium carbonate and 162g (0.75mol) of phenolic resin microspheres into the reaction kettle and stir evenly. Then add 96g (0.75mol) of calcium carbide and 10g (1.5%) of cuprous iodide into the reactor, and fill the reactor with carbon dioxide. Heat and pressurize the reaction. Reaction temperature is 60 ℃, and reaction pressure is 2MPa. The reaction time was 18 hours. After the reaction, the mixture was filtered to separate the liquid, and then acidified with sulfonic acid resin to obtain the product. The product was analyzed by liquid chromatography, and the yield of propiolic acid was 97 mol %.

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Abstract

The invention discloses a synthetic method of propiolic acid. The method comprises the following steps of: putting calcium carbide, a hydrogen donor, a solvent, a catalyst and an auxiliary agent intoa reaction kettle, introducing carbon dioxide into the reaction kettle, and heating and pressurizing to react, wherein the reaction temperature is 30-80 DEG C, the reaction pressure is 1-6 MPa, and the reaction time is 12-24 hours; separating a liquid and a hydrogen donor from the mixture after the reaction, and acidifying the liquid mixture to obtain a product. The propiolic acid synthesis methoddisclosed by the invention is relatively environment-friendly and low in production cost.

Description

technical field [0001] The invention relates to a method for synthesizing propiolic acid, in particular to a method for synthesizing propiolic acid from calcium carbide (calcium carbide) and carbon dioxide. Background technique [0002] Propiolic acid is a colorless liquid at room temperature. Miscible with water, ethanol, ether and chloroform. Propiolic acid is used as an intermediate in organic synthesis, and can be catalyzed with methanol to generate propiolic acid methyl ester, which is the raw material for the production of antiviral drug iodine. It can be used to prepare propionic acid, trimesic acid, halogenated acrylic acid, dihalogenated acrylic acid, diacetylene dicarboxylic acid, ethyl propiolate, pyrazolone, dibromocrotonic acid, ethoxycrotonic acid, etc. Propiolic acid can also be used in the synthesis of transition metal complexes, haloalkyl propiolates, and haloacrylates. With the deepening of its research and the development of new uses, the demand for pro...

Claims

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Application Information

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IPC IPC(8): C07C51/02C07C57/20C07C51/15
CPCC07C51/02C07C51/15C07C57/20
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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