Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

One process of using two fixed bed reactors to continuously catalyze the N-methyl-1,3-propyleneramine

A fixed-bed reactor and catalytic reaction technology, which is applied in the preparation of amino compounds, organic compounds, carboxylic acid nitriles, etc., can solve the problems of many by-products, complicated product distillation and purification operations, and difficult product separation, etc., and achieve The effect of low cost and easy serial production

Active Publication Date: 2022-05-27
DALIAN UNIV OF TECH
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • One process of using two fixed bed reactors to continuously catalyze the N-methyl-1,3-propyleneramine
  • One process of using two fixed bed reactors to continuously catalyze the N-methyl-1,3-propyleneramine
  • One process of using two fixed bed reactors to continuously catalyze the N-methyl-1,3-propyleneramine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) First, the reactor 11 and the reactor 17 are loaded with catalyst 4A molecular sieve and Raney-Ni respectively. (2) Open the nitrogen cylinder, purge the entire system, discharge air, set the pressure of 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: 4MPa, and the mass flow controller 18 controls the hydrogen flow rate, and the temperature controller 16 sets the temperature to 65°C. (3) Two double-piston micro-pumps were respectively used to transport monomethylamine ethanol solution (40%) and acrylonitrile (99%) in a ratio of 7 molar ratios of 1.1:1 to a fixed bed reactor filled with 4A type molecular sieve catalyst 11 reactions at a space velocity of 0.8h -1 Under certain conditions, the reaction solution containing 3-methylaminopropionitri...

Embodiment 2-12

[0028]

[0029]

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a process for preparing N-methyl-1,3-propylenediamine through continuous catalytic reaction in two fixed-bed reactors, which belongs to the technical field of organic chemical industry. Using monomethylamine and acrylonitrile as raw materials, first continuously pass through the first fixed-bed reactor to react to generate 3-methylaminopropionitrile intermediate, and then continuously enter the second fixed-bed hydrogenation reactor for catalytic hydrogenation Hydrogen to generate N-methyl-1, 3-propylenediamine, yield ≥ 99%. The process of the invention is continuous production, simple, less three wastes, energy saving, environmental protection, low cost, and easy to realize industrialization.

Description

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

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/11C07C209/48C07C255/24C07C253/30
CPCC07C253/30C07C209/48C07C255/24C07C211/11
Inventor 都健谭威孟庆伟卫源安
Owner DALIAN UNIV OF TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products