Method for preparing 3-aminopropionitrile from waste liquid containing 3,3-iminodipropionitrile

A technology of iminodipropionitrile and aminopropionitrile, applied in the field of preparation of 3-aminopropionitrile, which can solve the problems of high risk, increased environmental treatment costs, waste of resources, etc.

Inactive Publication Date: 2021-04-20
HANGZHOU XINFU TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, a large amount of by-product 3,3-iminodipropionitrile is produced through the acrylonitrile ammoniation reaction. For this part of the by-product, the usual treatment method is incineration or thermal cracking. This method not only increases the cost of environmental governance, It is a waste of resources and a high degree of danger

Method used

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  • Method for preparing 3-aminopropionitrile from waste liquid containing 3,3-iminodipropionitrile
  • Method for preparing 3-aminopropionitrile from waste liquid containing 3,3-iminodipropionitrile

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Experimental program
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Effect test

Embodiment 1

[0018] First take by weighing 40% 3,3-iminodipropionitrile waste liquid 260g and 30% ammoniacal liquor 600g for subsequent use, adjust the reaction pressure of microchannel flow reactor to be 4.0MPa, and reaction temperature is 168 ℃, then by metering pump Ammonia water with a volumetric flow rate of 10ml / min and 40% 3,3-iminodipropionitrile aqueous solution were poured into the microchannel flow reactor at a speed of 1.6ml / min, and reacted for 20min. Distilled to obtain 98.7g of rectified propionitrile, the molar yield was 82.2%.

[0019] GC detection conditions: chromatographic column Agilent DB-624-08, inlet temperature 250°C, carrier gas (nitrogen) flow rate 2ml / min, detector temperature 300°C, column temperature 70-240°C;

[0020] Use GC to sample the product, see figure 1 , the peak position of β-aminopropionitrile is at 5.635min, for figure 1 The analysis results are as follows: the mass content of β-aminopropionitrile in the rectified propionitrile is 98.6%, the mass...

Embodiment 2

[0023] According to the treatment method of Example 1, the difference is that the reaction temperature is 130°C.

[0024] The product was distilled with ammonia water, and then rectified to obtain 56.2 g of rectified propionitrile, with a molar yield of 46.8%.

[0025] The product was sampled and detected by GC, and the results were as follows: the mass content of β-aminopropionitrile in the rectified propionitrile was 98.5%, the mass content of iminodipropionitrile was 0.1%, and the mass content of water was 1.4%.

Embodiment 3

[0027] According to the treatment method of Example 1, the difference is that the ammonia concentration is 33.5%, and the reaction temperature is 175°C.

[0028] The product was distilled with ammonia water, and then rectified to obtain 110.7 g of rectified propionitrile, with a molar yield of 92.0%.

[0029] Using GC to sample and detect the product, the results are as follows: the mass content of β-aminopropionitrile in the rectified propionitrile is 98.4%, the mass content of iminodipropionitrile is 0.1%, and the mass content of water is 1.5%.

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Abstract

The invention provides a method for preparing 3-aminopropionitrile from a waste liquid containing 3,3-iminodipropionitrile, wherein the method comprises the following steps: respectively introducing the waste liquid containing 3,3-iminodipropionitrile and an ammonia water solution into a micro-channel reactor to react, to obtain a reaction feed liquid; and carrying out deamination and distillation on the reaction feed liquid to obtain 3-aminopropionitrile. Firstly, the treatment method for preparing the 3-aminopropionitrile from the 3,3-iminodipropionitrile in the 3,3-iminodipropionitrile waste liquid can effectively realize reutilization of resources, and the yield of the 3-aminopropionitrile is relatively high; and secondly, the micro-channel reactor is adopted to strengthen mass and heat transfer in the reaction process, improve the reaction efficiency and realize continuous synthesis of the process, so that the high-temperature residence time can be shortened, the whole process is easy to control, the reutilization of beta-aminopropionitrile byproducts is improved favourably, and the consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of waste liquid reuse, in particular to a method for preparing 3-aminopropionitrile from waste liquid containing 3,3-iminodipropionitrile. Background technique [0002] β-aminopropionitrile is an intermediate for the synthesis of aminoalanine and pantothenic acid; 1,3-diaminopropane can be obtained by reduction; isocyanate can be obtained by reacting with phosgene, and further reacted with p-nitroaniline, A sweetener can be prepared, which is 350 times sweeter than sugar; the hydrogen on ammonia can be replaced by aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons and heterocyclic rings to generate corresponding alkylaminopropionitriles; it is also used as a synthetic pharmaceutical intermediate Such as vitamin B1 and vitamin B5. [0003] In the prior art, a large amount of by-product 3,3-iminodipropionitrile is produced through the acrylonitrile ammoniation reaction. For this part of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C253/34C07C255/24
Inventor 伊滨刘学愚朱继荣余建新姜伟林贺光巍娄波沈汉军陈琦白彦兵汪军朱松青胡益辉
Owner HANGZHOU XINFU TECH CO LTD
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