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Method for preparing 3-methoxypropionitrile

A technology of methoxypropionitrile and acrylonitrile, which is applied in the field of 3-methoxypropionitrile preparation, can solve the problems of long activation time and complicated operation, and achieve the effects of reduced methanol consumption, simple process and easy separation

Pending Publication Date: 2021-10-29
山东汉鸿新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the follow-up process, the alkali metal hydroxide needs to be removed, and the operation is complicated;
[0008] The active site of this reaction is methoxyl, and sodium hydroxide is used as a catalyst. It takes a certain period of time to provide methoxyl ions, and the activation time is relatively long.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 106.6g of methanol into a four-neck flask, add about 2‰wt of sodium methoxide, heat in a water bath to 60°C and keep it warm for 30min, weigh 159.0g of acrylonitrile into the dropping funnel, add dropwise, and control the temperature at 60-65 Celsius, 2 hours after the dropwise addition, add 0.1066g of sodium dihydrogen phosphate after 2 hours of reaction, the remaining 0.3% of acrylonitrile is measured, the conversion rate is 99.68%, and 0.0954g of sodium dihydrogen phosphate is added.

Embodiment 2

[0024] Example 2: Weigh 105.6g of methanol into a four-neck flask, add about 3‰wt of sodium methoxide, heat it in a water bath to 60°C and keep it warm for 30min, weigh 159.0g of acrylonitrile into the dropping funnel, add it dropwise, and control the temperature At 60-65 degrees Celsius, the dropwise addition was completed in 2 hours. After 3 hours of reaction, add 0.8650 g of a mixture of phosphoric acid and sodium phosphate. It was measured that the remaining acrylonitrile was about 0.5%, and the conversion rate was 99.48%. Add 0.1200 g of a mixture of phosphoric acid and sodium phosphate.

Embodiment 3

[0025] Example 3: Weigh 101.8g of methanol into a four-neck flask, add about 2‰wt of sodium methoxide, heat it in a water bath to 50°C and keep it warm for 30min, weigh 159.0g of acrylonitrile into the dropping funnel, add it dropwise, and control the temperature At 50-60 degrees Celsius, the dropwise addition was completed in 2 hours, and 0.0687 g of sodium bisulfate was added after 2 hours of reaction. It was measured that the remaining acrylonitrile was about 0.75%, and the conversion rate was 99.22%, and 0.1458 g of sodium bisulfate was added.

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PUM

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Abstract

The invention discloses a method for preparing 3-methoxypropionitrile. The method is characterized by comprising the following steps of: (1) adding a methanol alkali metal compound into methanol, heating to 30-80 DEG C, and keeping the temperature for a period of time; (2) dropwise adding acrylonitrile, controlling the temperature at 30-80 DEG C, reacting for 2-8 hours after the acrylonitrile is dropwise added, adding a modification additive, modifying the reaction liquid for 30 minutes to obtain methoxypropionitrile, and enabling the residual acrylonitrile to be less than 0.5%; and (3) after the reaction is finished, supplementing the modification additive to generate a precipitate, and distilling to obtain the methoxypropionitrile. Compared with the prior art, the method does not need to operation of removing alkali metal hydroxide, shortens the activation time, and reduces the methanol consumption, and the temperature can meet the requirement in industrial cooling water; the method is simple and easy to operate; the conversion rate of the method is high; and in addition, in the process of adding the additive, the catalyst in the reaction liquid can be removed, and the generated precipitate is easy to separate, so that convenience is provided for the subsequent reaction.

Description

technical field [0001] The invention relates to the technical field of preparing 3-methoxypropionitrile, and more specifically relates to a method for preparing 3-methoxypropionitrile. Background technique [0002] The reaction of acrylonitrile with compounds containing active hydrogen atoms to generate cyanoethyl derivatives is called cyanoethylation reaction. The reaction takes place at 40°C under the condition of alkali, in which methanol reacts with acrylonitrile to generate 3-methoxypropionitrile, which can be used in organic synthesis and also as a good solvent for plastic polymers. 3-Methoxypropionitrile is hydrogenated to generate methoxypropylamine, which can be used as a catalyst in the production of polyurethane foam and epoxy resin, and can also be used as a detergent, emulsifier, wetting agent and corrosion inhibitor, etc. . [0003] In the prior art: [0004] ① In Japanese Patent No. 103505 / 1975, an alkali metal oxide is used as a catalyst to obtain methoxyp...

Claims

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Application Information

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IPC IPC(8): C07C255/13C07C253/30C07C253/34
CPCC07C253/30C07C253/34C07C255/13
Inventor 刘涛李福同冯新江祁超慧
Owner 山东汉鸿新材料科技有限公司
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