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Preparation method for ethyl formate

A technology of ethyl formate and carbon monoxide, applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of not meeting the environmental protection requirements of green chemical technology, not obtaining simple and easy treatment methods, unfavorable separation of products, etc., to achieve Reduce equipment requirements, increase productivity, and facilitate post-processing effects

Active Publication Date: 2012-10-24
LINHAI LIANSHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the existing technology, since a large amount of water is produced during the esterification reaction between formic acid and ethanol, and ethyl formate is easy to hydrolyze, a large amount of desiccant is required for product post-treatment to dehydrate, which not only increases the production cost, but also the product is not It is beneficial to the separation, which has always been the key problem solved by relevant literature at home and abroad, but so far has not obtained a simple and easy processing method.
In addition, strong acids such as sulfuric acid need to be used as catalysts in the reaction process, which not only causes corrosion to the equipment, but also requires a relatively large amount of catalysts, which does not meet the environmental protection requirements of green chemical processes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The alkali metal alkoxide of the catalyst is sodium methoxide.

[0028] Add 300g of absolute ethanol and 5g of sodium methoxide (that is, absolute ethanol and sodium methoxide with a molar ratio of 1000:14.2) into an autoclave equipped with an electric stirring device and a thermometer, and raise the temperature to the reaction temperature while stirring At 60°C, feed carbon monoxide to react with absolute ethanol to generate ethyl formate, and the reaction pressure is 4.0Mpa.

[0029] After the reaction was finished, the distilled fraction obtained was ethyl formate with a weight of 410 g.

[0030] The yield of ethyl formate is 85.0%, and the content is greater than 98.0%.

Embodiment 2

[0032] The alkali metal alkoxide of the catalyst is selected from sodium ethylate.

[0033] Add 300g of absolute ethanol and 6g of sodium ethylate (that is, absolute alcohol and sodium ethylate with a molar ratio of 1000:13.5) into an autoclave equipped with an electric stirring device and a thermometer, and raise the reaction temperature to 50°C while stirring , feed carbon monoxide to react with absolute ethanol to generate ethyl formate, and the reaction pressure is 3.0Mpa.

[0034] After the reaction was finished, the distilled fraction obtained was ethyl formate with a weight of 410 g.

[0035] The yield of ethyl formate is 85.0%, and the content is greater than 98.0%.

Embodiment 3

[0037] The alkali metal alkoxide of the catalyst is potassium methylate.

[0038] Add 300g of absolute ethanol and 6g of potassium methylate (that is, absolute ethanol and potassium methylate with a molar ratio of 1000:13.1) into an autoclave equipped with an electric stirring device and a thermometer, and raise the reaction temperature to 70°C while stirring , feed carbon monoxide to react with absolute ethanol to generate ethyl formate, and the reaction pressure is 9.0Mpa.

[0039] After the reaction was finished, the distilled fraction obtained was ethyl formate with a weight of 390 g.

[0040] The yield of ethyl formate is 80.8%, and the content is greater than 98.0%.

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Abstract

The invention relates to a preparation method for ethyl formate. The method does not generate a great quantity of water and does not need to take sulfuric acid as a catalyst. The ethyl formate can be prepared by reacting anhydrous ethanol with carbonic oxide under the action of a basic catalyst. By the technical scheme, equipment requirements can be lowered, cost of raw materials is reduced, hydrolysis of the ethyl formate is avoided, and yield and acceptance rate of the ethyl formate are increased.

Description

technical field [0001] The invention belongs to the field of chemical material synthesis, and relates to a method for preparing ethyl formate, in particular to a method for preparing ethyl formate through hydroxylation. Background technique [0002] Ethyl formate (molecular formula is C 3 h 6 o 2 , the structural formula is HCOOCH 2 CH 3 , simplified to ) is a colorless transparent liquid with a pungent smell similar to ethyl acetate and a pineapple-like aroma with a slightly bitter taste. Ethyl formate is slightly soluble in water, soluble in most organic solvents such as benzene, ethanol, ether, and insoluble in glycerin, with a boiling point of about 53.4-54.4°C. [0003] Ethyl formate is an important organic solvent and organic synthesis intermediate, which can be used in pharmaceuticals, such as for the manufacture of antineoplastic drugs Fuxeridine, vitamin B1, and the production of houttuyonin, tongjingning, anadrol, thiophene It can also be used as a solvent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/06C07C67/36
Inventor 邓一建黄卫国胡海波
Owner LINHAI LIANSHENG CHEM
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