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Preparation method for synthesis of ethyl 3-ethoxypropionate

A technology of ethyl ethoxy propionate and ethyl acrylate, applied in the field of preparation of synthesizing ethyl 3-ethoxy propionate, can solve the difficulty of increasing separation steps, increasing side reactions, and increasing organic salts to purify products And other issues

Inactive Publication Date: 2014-09-03
SHENZHEN PRECHEM FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Patent CN200810061996.1 uses alkali metals such as sodium metal or alkali metal alkoxides as catalysts to synthesize ethyl 3-ethoxypropionate with absolute ethanol and ethyl acrylate, the reaction time is shortened to less than 3 hours, and the highest yield can reach 96%, but there are also catalysts that are extremely sensitive to acid and water, once they encounter water or acid, they will be destroyed and cannot be regenerated, and after the reaction, it is necessary to use acid to destroy the catalyst to make the system neutral or even acidic, which increases the separation steps, and The formation of organic salts in the reaction increases the difficulty of product purification, and the highly exothermic process of neutralization increases side reactions

Method used

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  • Preparation method for synthesis of ethyl 3-ethoxypropionate
  • Preparation method for synthesis of ethyl 3-ethoxypropionate
  • Preparation method for synthesis of ethyl 3-ethoxypropionate

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specific Embodiment 1

[0047] Specific Example 1: In a fixed-bed reactor with a radius of 2.5 centimeters and a height of 75 centimeters, the catalyst is fixed inside, and the catalyst is first cleaned with absolute ethanol, then purged with nitrogen, then washed with deionized water, and then again Purged with nitrogen, then treated with 2-10% lye, washed with water after treatment, then filled with nitrogen, then washed with fresh ethanol or a mixture of ethanol and ethyl acrylate under nitrogen, and then filled with nitrogen Wash with ethanol until the water content of the cleaned ethanol in the system is not more than 0.1%. In the batching tank, the mass ratio of absolute ethanol and ethyl acrylate is 85:15, and the catalyst is about 15% of ethyl acrylate. Cool to The temperature is between 9-13 degrees, and it is passed into the fixed bed reactor according to the dilution rate of 2.1. The temperature of the reactor is controlled at 26±2 degrees. The material in the tank is rectified through the...

specific Embodiment 2

[0048]Specific embodiment 2: on the fixed-bed reactor surface of above embodiment 1, fix catalyst, clean and dry as embodiment 1, be 85:15 by the mass ratio of dehydrated alcohol and ethyl acrylate in batching tank, catalyst It is about 15% of ethyl acrylate, cooled to a temperature between 19-20 degrees, passed into a fixed bed reactor at a dilution rate of 2.0, the temperature of the reactor is controlled at 28±2 degrees, and the reacted material enters the receiving tank , measure the content of ethyl acrylate inside, the material in the receiving tank is rectified by the rectification tower, the EEP with a purity of 99% is collected as the product, and the yield is calculated, the excess ethanol and unreacted ethyl acrylate and a small amount of entrainment Return EEP to the batching tank and add fresh absolute ethanol and ethyl acrylate to adjust to 85:15, and enter the fixed bed circulation reaction. After continuous operation for 105 hours, 0.3% of ethyl acrylate discha...

specific Embodiment 3

[0049] Specific embodiment 3: on the fixed-bed reactor surface of above embodiment 1, fix catalyst, clean and dry as embodiment 1, be 85:15 by the mass ratio of dehydrated alcohol and ethyl acrylate in batching tank, catalyst It is about 15% of ethyl acrylate, cooled to a temperature between 13-15 degrees, passed into a fixed bed reactor at a dilution rate of 2.0, the temperature of the reactor is controlled at 28±2 degrees, and the reacted material enters the receiving tank , measure the content of ethyl acrylate inside, the material in the receiving tank is rectified by the rectification tower, the EEP with a purity of 99% is collected as the product, and the yield is calculated, the excess ethanol and unreacted ethyl acrylate and a small amount of entrainment Return EEP to the batching tank and add fresh absolute ethanol and ethyl acrylate to adjust to 85:15, and enter the fixed bed circulation reaction. After continuous operation for 90 hours, 0.8% of ethyl acrylate discha...

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Abstract

The invention relates to the technical field of chemical synthesis, and particularly relates to a preparation method for synthesis of ethyl 3-ethoxypropionate; the ethyl 3-ethoxypropionate is synthesized by addition reaction of absolute ethanol and ethyl acrylate in the presence of a catalyst in a tubular reactor, the molar ratio of absolute ethanol to ethyl acrylate is 3: 1 to 100: 1, the catalyst weight accounting for 0.1% to 20% of the weight of the ethyl acrylate; the catalyst is anion exchange resin, and the method has the advantages of simple synthesis, mild condition, less side reaction, recycling and regeneration of the catalyst without damage, great simplification of the separation process, easy continuous production and the like.

Description

【Technical field】 [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method for synthesizing ethyl 3-ethoxypropionate. 【Background technique】 [0002] Ethyl 3-ethoxypropionate is an important organic solvent and organic synthesis intermediate, widely used in the coating industry, electronics industry and the synthesis of pharmaceutical intermediates. [0003] U.S. Patent No. 5,081,285 uses ethanol and ethyl acrylate to obtain ethyl 3-ethoxypropionate under the catalysis of methanesulfonic acid. The reaction temperature is 120-130 degrees, and the yield is 41%. This scheme needs to be reacted under pressure, which is not convenient for production. And the reaction temperature is high, the side reactions are many, and the cost is too high. [0004] Literature [Tetrahedro letters, 46 (19), 3279-3282: 2005] adopts potassium fluoride supported by aluminum oxide as a catalyst to synthesize 3-ethoxy ethyl propionate with ethan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/708C07C67/31
CPCY02P20/584C07C67/31
Inventor 罗鑫鹏吴小强
Owner SHENZHEN PRECHEM FINE CHEM CO LTD
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