Preparation method of N, N-dimethyl-1, 3-propane diamine

A technology of propylene diamine and dimethylamine, which is applied in the N field to achieve the effects of high efficiency, high conversion rate and few by-products

Pending Publication Date: 2021-11-09
CHINA TIANCHEN ENG
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Although the above-mentioned patent method provides a synthetic preparation method for DMAPA, there is still room for improvement in terms of raw material conversion rate, product yield, by-product selectivity, etc.

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  • Preparation method of N, N-dimethyl-1, 3-propane diamine

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preparation example Construction

[0043] Among the present invention, the preparation method of N,N-dimethyl-1,3-propanediamine comprises the following steps:

[0044] (1) After mixing acrylonitrile and dimethylamine solution in a certain proportion, inject the microchannel reaction device, carry out addition reaction under certain temperature and pressure conditions, obtain the first reaction solution containing dimethylaminopropionitrile, wherein The conversion rate of acrylonitrile is 100%, and the selectivity of dimethylaminopropionitrile is above 99.8%;

[0045] (2) The first reaction solution is mixed with hydrogen, and after preheating, it enters the continuous hydrogenation reactor 8 equipped with a Ni-based alloy hydrogenation catalyst for hydrogenation reaction to obtain a hydrogenation reaction containing N,N-dimethyl-1,3- Propylenediamine second reaction solution, wherein the conversion rate of dimethylaminopropionitrile is 100%, and the product selectivity is greater than 99.8%;

[0046] (3) The ...

Embodiment 1

[0049] Using the ethanol solution of acrylonitrile and 30% dimethylamine as raw materials, the addition reaction is carried out through a microchannel reaction device to obtain the addition reaction liquid, wherein the molar ratio of acrylonitrile and dimethylamine is 1:1.05, and the reaction temperature is 40°C , pressure 1bar, residence time 40s. The reaction product was collected from the outlet of the microchannel reaction device for analysis. The conversion rate of acrylonitrile was 100%, and the selectivity of dimethylaminopropionitrile was 99.82%. The above-mentioned addition reaction solution and hydrogen are mixed and preheated and then entered into a fixed-bed hydrogenation reactor, and a Ni-based alloy hydrogenation catalyst is installed in the reactor. The hydrogenation reaction temperature is 60°C, the pressure is 3 bar, and the residence time of the reaction liquid is 30 min. The preparation method of the hydrogenation catalyst is as follows: the alloy composed ...

Embodiment 2

[0051] Using the methanol solution of acrylonitrile and 35% dimethylamine as raw materials, the addition reaction is carried out through a microchannel reaction device to obtain the addition reaction solution, wherein the molar ratio of acrylonitrile and dimethylamine is 1:1.1, and the reaction temperature is 60°C , pressure 1.5bar, residence time 30s. The reaction product was collected from the outlet of the microchannel reaction device for analysis. The conversion rate of acrylonitrile was 100%, and the selectivity of dimethylaminopropionitrile was 99.80%. The above-mentioned addition reaction liquid and hydrogen are mixed and preheated, and then enter a trickle bed hydrogenation reactor, and a Ni-based alloy hydrogenation catalyst is installed in the reactor. The hydrogenation reaction temperature is 40°C, the pressure is 4 bar, and the residence time of the reaction liquid is 30 min. The preparation method of the hydrogenation catalyst is as follows: the alloy composed of...

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Abstract

The invention provides a preparation method of N, N-dimethyl-1, 3-propane diamine, which comprises the following steps: mixing acrylonitrile and a dimethylamine solution, injecting the mixture into a micro-channel reaction device for addition reaction, mixing the reaction liquid with hydrogen, preheating the mixture, feeding the preheated mixture into a continuous hydrogenation reactor filled with a Ni-based alloy hydrogenation catalyst, carrying out hydrogenation reaction and carrying out vacuum rectification separating to obtain the required product. According to the preparation method disclosed by the invention, the microchannel reactor has the advantages of continuity, high mass and heat transfer efficiency, narrow residence time distribution, no amplification effect and the like, so that the addition reaction of acrylonitrile and dimethylamine has the characteristics of high efficiency, high conversion rate and few byproducts; and the hydrogenation reaction is carried out under extremely mild reaction conditions by using the novel Ni-based alloy catalyst, and meanwhile, very high conversion rate and product selectivity are obtained, so that the whole reaction system has the advantages of continuous production, convenience in operation, high resource utilization rate and the like.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of N,N-dimethyl-1,3-propanediamine. Background technique [0002] Dimethylaminopropylamine, full name N,N-dimethyl-1,3-propanediamine (DMAPA), is one of the most important varieties of lower aliphatic diamine compounds. It is polar, chemically active, and can form hydrogen bonds. At the same time, there are lone pairs of electrons on the N atom, which has nucleophilic ability and is easy to react with electrophilic compounds. DMAPA is mainly used in the fields of daily chemicals, pesticides, dyes, oil fields, water treatment, resins and other additives, and has a wide range of uses. At present, the vast majority of DMAPA products are used to produce amide betaine, and the remaining small part of DMAPA products are used as polyurethane catalysts, epoxy resin curing agents and accelerators, and the production of dyes and propamocarb. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/11C07C209/48C07C255/24C07C253/30B01J23/755B01J19/00B01J8/00
CPCC07C209/48C07C253/30B01J23/755B01J19/0093B01J8/00C07C211/11C07C255/24Y02P20/10Y02P20/52
Inventor 史文涛王聪冯传密崔艳杰吴昊崔志国
Owner CHINA TIANCHEN ENG
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