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Preparation process method of N-methyl-1, 3-propane diamine

A preparation process and technology of propylene diamine are applied in the preparation of amino compounds, the preparation of organic compounds, the preparation of carboxylic acid nitrile, etc., and can solve the problems of complicated rectification and purification operations, low production efficiency, and low product yield, etc. Achieve the effect of reducing the probability of deterioration, improving hydrogenation efficiency, and high resource utilization

Active Publication Date: 2020-07-28
DALIAN UNIV OF TECH +1
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The 1,3-propylenediamine route is a non-mainstream synthetic route, which is obtained by the ammoniation reaction of 1,3-propylenediamine and methanol, usually accompanied by many ammoniated by-products, the actual production efficiency is not high, and it is difficult to industrialize
[0004] The acrylonitrile route is to generate 3-methylaminopropionitrile by reacting acrylonitrile and monomethylamine, and then obtain N-methyl-1,3-propanediamine by hydrogenation reduction of 3-methylaminopropionitrile. The method route is simple and direct , the reaction conversion rate is high, which is the mainstream synthetic route; however, most domestic factories use batch reaction equipment, so that the intermediate 3-methylaminopropionitrile and the product N-methyl-1,3-propanediamine are often Deterioration occurs during the reaction process, resulting in a low yield of the final product and complex distillation and purification operations

Method used

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  • Preparation process method of N-methyl-1, 3-propane diamine

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Experimental program
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Effect test

Embodiment 1

[0030] Through the metering pump, acrylonitrile and 40% monomethylamine aqueous solution are passed into the preheating pipeline at a molar ratio of 1:1, and the acrylonitrile and monomethylamine aqueous solution are preheated to 40°C respectively, and then the raw material liquid enters the first A microchannel reactor carries out addition reaction, reaction temperature 40 ℃, reaction time 90s, reaction pressure 0.5MPa, the reaction feed liquid containing intermediate 3-methylaminopropionitrile and water obtained after the completion of the reaction; the reaction feed liquid is directly Mix evenly with water containing sodium hydroxide through a T-type mixer, then heat the feed liquid to 100°C through a preheating pipeline, and pass it into the second microchannel reactor with a mixing ratio of 1:150 (v / v) with hydrogen Mix, then enter the fixed bed filled with Ranny-Ni for hydrogenation reaction, the content of 3-methylaminopropionitrile in the hydrogenation raw material liqu...

Embodiment 2

[0032] Using the production method of Example 1, the difference is to use a monomethylamine-methanol solution with a concentration of 80%, the molar ratio of acrylonitrile and monomethylamine is 1:2, the reaction temperature is 100°C, the reaction time is 50s, and the reaction pressure is 1.5MPa The hydrogenation solvent is methanol, the hydrogenation aid catalyst is monomethylamine, the content of 3-methylaminopropionitrile in the hydrogenation raw material liquid is 20%, the content of monomethylamine is 2%, the reaction temperature is 70°C, the reaction time is 5min, and the final product The yield is 93.5%.

Embodiment 3

[0034] Using the production method of Example 1, the difference is that the concentration of 95% monomethylamine aqueous solution is used, the molar ratio of acrylonitrile and monomethylamine is 1:1.3, the reaction temperature is 120°C, the reaction time is 30s, and the reaction pressure is 2.2MPa; The hydrogen solvent is water, and the hydrogenation-promoting catalyst is sodium carbonate and monomethylamine. The 3-methylaminopropionitrile content is 40% in the hydrogenation raw material liquid, and the co-catalyst content is 2%. The fixed bed is filled with Pd-C, and the hydrogenation reaction temperature is 90°C, the reaction time is 10min, and the yield of the final product is 95%.

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Abstract

The invention discloses a preparation process method of N-methyl-1, 3-propane diamine, and belongs to the technical field of organic synthesis. According to the method, monomethylamine and acrylonitrile are used as raw materials, an intermediate 3-methylaminopropionitrile is generated through a reaction in a micro-channel reactor, the intermediate is mixed with hydrogen and enters a catalyst fixedbed for a hydrogenation reaction, and finally the product N-methyl-1, 3-propane diamine is obtained. According to the preparation process method of N-methyl-1, 3-propane diamine, the method is simple, continuous production can be achieved, the reaction time is short, the side reaction occurrence probability is low, the product yield reaches 90-95%, and the productivity is improved.

Description

technical field [0001] The invention relates to a preparation process of N-methyl-1,3-propanediamine, which belongs to the field of organic synthesis. Background technique [0002] N-methyl-1,3-propanediamine, also known as 3-methylaminopropylamine, is an important chemical synthesis intermediate, widely used in medicine, feed, food and other fields. [0003] Currently, industrial chemical synthesis routes mainly include acrylonitrile route and 1,3-propanediamine route, among which the present invention adopts acrylonitrile route, which is the mainstream synthesis route. The 1,3-propanediamine route is a non-mainstream synthetic route, which is obtained by the ammoniation reaction of 1,3-propylenediamine and methanol, usually accompanied by many ammoniated by-products, the actual production efficiency is not high, and it is difficult to industrialize . [0004] The acrylonitrile route is to generate 3-methylaminopropionitrile by reacting acrylonitrile and monomethylamine, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/48C07C211/09B01J19/00
CPCC07C209/48C07C253/30B01J19/0093C07C211/09C07C255/24Y02P20/584
Inventor 高岩曾伟滕坤尹航
Owner DALIAN UNIV OF TECH
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