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A kind of method preparing 3-aminopropionitrile under supercritical condition

An aminopropionitrile and supercritical technology, which is applied in the preparation of carboxylic acid nitriles, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as complex processes, limited development, and increased costs, so as to avoid separation difficulties and shorten the reaction time. time, the effect of reducing energy consumption

Active Publication Date: 2020-04-07
ZHEJIANG NHU CO LTD +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] In the above report, when synthesizing 3-aminopropionitrile, using alcohol as a solvent can reduce the amount of ammonia, speed up the reaction rate, and improve the selectivity of the main product. Nitrile is difficult to separate from the product, thus limiting its development in industry
The use of catalysts can effectively increase the product yield, but at the same time it also increases the cost. In the production process, the invalid catalyst needs to be replaced, which makes the operation complicated
To produce 3-aminopropionitrile by continuous reaction in a fixed-bed tubular reactor, it is necessary to recycle the by-product iminodipropionitrile and further react with ammonia to form the product, which makes the process complicated and consumes a lot of energy.

Method used

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  • A kind of method preparing 3-aminopropionitrile under supercritical condition
  • A kind of method preparing 3-aminopropionitrile under supercritical condition
  • A kind of method preparing 3-aminopropionitrile under supercritical condition

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Experimental program
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Effect test

Embodiment 1

[0040] by such as figure 1 As shown in the reaction flow chart, turn on metering pump 1, pump in acrylonitrile at a constant rate of 2ml / min, set the temperature of the vaporizer at 90°C, turn on liquid ammonia metering pump 2, and pump in liquid ammonia at a constant rate of 9ml / min , The temperature of the supercritical pipeline reactor is set at 160°C, the high-precision reverse pressure controller after the condenser is adjusted, the pressure is controlled at 15±1MPa, and the reaction residence time is 20min. After the reaction was completed, the reaction solution was collected, the organic layer was separated, and analyzed by gas chromatography. It was calculated that the conversion rate of acrylonitrile was 100%, and the selectivity of 3-aminopropionitrile was 90.2%.

Embodiment 2-22

[0042] According to the operation method of embodiment 1, change reaction conditions: liquid ammonia flow rate, reactor temperature, reaction pressure, residence time, obtain reaction liquid, its reaction conditions and reaction result are as shown in table 1.

[0043] The reaction condition and reaction result of table 1 embodiment 2~22

[0044]

[0045]

[0046] As can be seen from the results in Table 2, under the supercritical conditions of the present invention, without adding additional catalyst and solvent, the reaction can also obtain better conversion and selectivity.

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Abstract

The invention discloses a method for preparing 3-aminopropionitrile under a supercritical condition. According to the method, liquid ammonia and acrylonitrile are used as raw materials which are subjected to direct addition reaction in a pipeline reactor without adding a catalyst and a solvent to obtain 3-aminopropionitrile. The reaction according to the invention is carried out under a supercritical condition of the liquid ammonia, thus avoiding the use of a catalysts and a solvent when the liquid ammonia is used in reports in the past; a product can be obtained through continuous rectification; unreacted raw materials can be directly used; the process is safe and environmentally friendly, substances of non-reactive raw materials are not introduced, and the method accords with a concept of green chemistry. The conversion rate of acrylonitrile can reach 99.5-100.0%, and the selectivity can reach 85.5-95.8%, so that the acrylonitrile has a high industrial application value.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for preparing 3-aminopropionitrile under supercritical conditions. Background technique [0002] 3-aminopropionitrile, also known as β-aminopropionitrile (β-amino propionitrile, C 3 h 6 N 2 , Molecular Weight: 70.11, CAS No.: 151-18-8), colorless liquid, with ammonia odor, is an intermediate in the synthesis of alanine and pantothenic acid; 1,3-diaminopropane can be obtained by reduction; and phosgene The reaction can produce isocyanate, and the reaction with p-nitroaniline can produce a sweetener, which is also used as a pharmaceutical intermediate. [0003] The main synthetic method of 3-aminopropionitrile is obtained by the addition reaction of acrylonitrile and ammonia, and the reaction formula is as follows: [0004] CH 2 =CHCN+NH 3 →NH 2 CH 2 CH 2 CN [0005] The main by-product is that 3-aminopropionitrile continues to react with acrylonitrile to obtain 3,3...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/24C07C253/18
CPCC07C253/18C07C255/24Y02P20/54
Inventor 王钰谢海英彭俊华倪海江吴晓东李观兵石清爱
Owner ZHEJIANG NHU CO LTD
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