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Ethyl 3-ethoxypropionate preparation method

A technology of ethyl ethoxy propionate and ethyl acrylate, applied in the field of preparing ethyl 3-ethoxy propionate, can solve the problems of high cost, many side reactions, affecting production efficiency and the like

Inactive Publication Date: 2018-09-25
XIAN GERUIDE NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[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, there are many side reactions, and the cost is too high
Literature [Tetrahedroletters, 46(19), 3279-3282: 2005] using aluminum oxide-supported potassium fluoride as a catalyst to synthesize ethyl 3-ethoxypropionate with ethanol and ethyl acrylate, using acetonitrile as a solvent in the process , the yield is 90%, but a large amount of solvent needs to be recovered, and the reaction time is 20 hours, which is too long and affects production efficiency
[0004] 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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  • Ethyl 3-ethoxypropionate preparation method
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Examples

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specific Embodiment 1

[0042] 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

[0043] 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 disch...

specific Embodiment 3

[0044]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 dischar...

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Abstract

The invention discloses an ethyl 3-ethoxypropionate preparation method, wherein the raw materials comprise anhydrous ethanol and ethyl acrylate, and the catalyst is ethyl acrylate accounting for 0.1-20% of the weight. According to the present invention, the method has advantages of simple synthesis, mild conditions, less side reactions, substantially-simplified separation process, convenient continuous production and the like, wherein the catalyst can be recycled without the damage, and can be regenerated.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for preparing 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. Literature [Tetrahedroletters, 46(19), 3279-3282: 2005] using aluminum oxide-supported potassium fluoride as a catalyst to synthesize ethyl 3-ethoxypropionate with ethanol and ethyl acrylate, using aceton...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/708
CPCC07C67/31C07C69/708Y02P20/584
Inventor 孙蓓林泽欣
Owner XIAN GERUIDE NEW CHEM MATERIALS CO LTD
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