Process for preparing N-methyl-1,3-propane diamine through continuous catalytic reaction by using two fixed bed reactors

A fixed-bed reactor and catalytic reaction technology, applied in the preparation of amino compounds, organic compounds, carboxylic acid nitriles, etc., can solve the complex distillation and purification of products, many by-products, and difficult to achieve large-scale industrialization and other problems, to achieve the effect of easy continuous production and low cost

Active Publication Date: 2021-06-15
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] There are two main synthetic routes of N-methyl-1,3-propanediamine, the first is to use acrylonitrile and monomethylamine as raw materials to prepare N-methyl-1,3-propanediamine, which is At present, the mainstream synthetic route of the industry, wherein the present invention adopts this synthetic route; the other is to use 1,3-propanediamine and methanol as raw materials, and methylation reaction occurs to prepare N-methyl-1,3-propanediamine, Although the process flow is simple, the products obtained from this reaction are mostly mixtures of secondary and tertiary amines, which have many by-products and the disadvantages of difficult product separation, making it difficult to realize large-scale industrial applications.
[0004] The first method takes acrylonitrile and monomethylamine as raw material reaction to generate 3-methylaminopropionitrile, and then obtains N-methyl-1,3-propanediamine by hydrogenation reduction of 3-methylaminopropionitrile, the method route Simple and direct, the reaction conversion rate is high, but most domestic factories currently use batch reactor reaction equipment, so that the intermediate 3-methylaminopropionitrile and the product N-methyl-1,3-propanediamine are often reacted Deterioration occurs during the process, resulting in a low yield of the final product and complex distillation and purification of the product

Method used

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  • Process for preparing N-methyl-1,3-propane diamine through continuous catalytic reaction by using two fixed bed reactors
  • Process for preparing N-methyl-1,3-propane diamine through continuous catalytic reaction by using two fixed bed reactors
  • Process for preparing N-methyl-1,3-propane diamine through continuous catalytic reaction by using two fixed bed reactors

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Embodiment 1

[0026] (1) Firstly, the reactor 11 and the reactor 17 are filled with catalyst 4A type molecular sieve and Raney-Ni respectively. (2) Open the nitrogen cylinder, purge the whole system, discharge the air, set the pressure on the fixed bed reactor 11 through the nitrogen pressure reducing valve 14: 4MPa, and set the temperature by the temperature controller 16: 35°C. The pressure of the fixed bed reactor 17 is set by the hydrogen cylinder 19 through the pressure reducing valve 14 to the system to set the hydrogen pressure: 4MPa, and the hydrogen flow rate is controlled by the mass flow controller 18, and the temperature is set by the temperature controller 16 to 65°C. (3) Use two double-plunger micropumps 7 to transport monomethylamine ethanol solution (40%) and acrylonitrile (99%) to the fixed-bed reactor filled with 4A molecular sieve catalyst at a molar ratio of 1.1:1 11 reactions, at a space velocity of 0.8h -1 Under certain conditions, continuous reaction makes the reacti...

Embodiment 2-12

[0028]

[0029]

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Abstract

The invention discloses a process for preparing N-methyl-1,3-propane diamine through continuous catalytic reaction by using two fixed bed reactors, belonging to the technical field of organic chemical industry. According to the invention, monomethylamine and acrylonitrile are used as raw materials, a 3-methylaminopropionitrile intermediate is generated through continuous reaction in a first fixed bed reactor, and then the intermediate continuously enters a second fixed bed hydrogenation reactor for catalytic hydrogenation, so N-methyl-1,3-propane diamine is generated, and the yield is larger than or equal to 99%. The process disclosed by the invention is continuous in production, simple in process, less in three wastes, reduced in energy consumption, friendly to environment, low in cost and easy to industrialize.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry and relates to a process for continuously preparing N-methyl-1,3-propanediamine. Background technique [0002] N-methyl-1,3-propanediamine belongs to lower aliphatic diamine and is an important organic chemical intermediate, widely used in medicine, feed, food and other fields. [0003] There are two main synthetic routes of N-methyl-1,3-propanediamine, the first is to use acrylonitrile and monomethylamine as raw materials to prepare N-methyl-1,3-propanediamine, which is At present, the mainstream synthetic route of the industry, wherein the present invention adopts this synthetic route; the other is to use 1,3-propanediamine and methanol as raw materials, and methylation reaction occurs to prepare N-methyl-1,3-propanediamine, Although the technological process is simple, the products obtained from this reaction are mostly mixtures of secondary and tertiary amines, which have ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/11C07C209/48C07C255/24C07C253/30
CPCC07C253/30C07C209/48C07C255/24C07C211/11
Inventor 孟庆伟谭威卫源安都健
Owner DALIAN UNIV OF TECH
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