Method and device for preparing adiponitrile

A technology for adiponitrile and pentene nitrile is applied in the field of devices for preparing adiponitrile, and can solve the problems such as the inability to monitor the inventory content of active catalysts

Active Publication Date: 2020-11-27
ZHEJIANG NHU CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This invention only monitors the hydrocyanic acid in the reaction effluent material, and cannot monitor the inventory of the active catalyst in the hydrocyanation reaction system, the residue of hydrocyanic acid and the content of the by-product 2-methyl-3-butenenitrile

Method used

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  • Method and device for preparing adiponitrile
  • Method and device for preparing adiponitrile
  • Method and device for preparing adiponitrile

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Experimental program
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preparation example Construction

[0125] The invention provides a kind of preparation method of adiponitrile, comprising:

[0126] Step 1: Hydrocyanic acid and butadiene carry out the first hydrocyanation reaction in the presence of the first catalyst to form a compound containing 3-pentenenitrile (3PN), 2-methyl-3-butenenitrile (2M3BN), The first stream of the first catalyst and butadiene, the concentration of hydrocyanic acid in the detection system is regulated by adjusting the ratio of raw materials, reaction temperature, reaction residence time or a combination of the above methods, so that the hydrogen in the final first stream is The residue of cyanic acid is less than 10ppm, and the molar ratio of the total amount of hydrocyanic acid to the amount of butadiene in the first hydrocyanation reaction is 0.75-1.0;

[0127] Step 2: the first stream obtained in step 1 is subjected to an isomerization reaction to obtain mononitriles comprising 2-pentenenitriles (2PN), 3-pentenenitriles (3PN) and 4-pentenenitri...

Embodiment 1

[0234] (1) The first hydrocyanation reaction

[0235] In the reactor R1, continuously feed the stream 101 of Cat1 (ligand: formula I, the molar ratio of total phosphorus ligand and zero-valent nickel is 12:1, impurity mass content 3.6%, 3.5Kg / h), BD The stream 102 (1.76Kg / h) and the stream 103 (0.50Kg / h) of HCN are passed into the stirred tank reactor R1 for reaction, the reaction temperature is 75°C, the reaction pressure is 2.0MPa, and the reaction residence time is 0.30h.

[0236] The R1 effluent stream 106 was monitored by online Raman spectroscopy, and the HCN content was 230 ppm. The stream 106 is continuously fed into the stirred tank reactor R2, and the stream 104 (0.25Kg / h) of HCN is continuously fed into R2, the reaction temperature is 75° C., the reaction pressure is 2.0 MPa, and the reaction residence time is 0.30 h.

[0237] The R2 effluent stream 107 was monitored by online Raman spectroscopy, and the HCN content was 160 ppm. The stream 107 is continuously fed ...

Embodiment 2-6

[0255] Continue the method shown in embodiment 1, reaction condition is identical, obtains following result:

[0256] Example Running time / h ADN yield / kg Cat1 loss rate / % Cat2 loss rate / % 2 10 27.1 3.9 3.0 3 50 135.5 3.8 2.8 4 100 270.9 3.8 2.7 5 200 541.8 3.8 2.7 6 500 1357.3 3.7 2.8

[0257] *The above Cat1 and Cat2 loss rates are the average loss rate per hour.

[0258]

[0259]

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Abstract

The invention provides a method and a device for preparing adiponitrile. The preparation method comprises the steps of a first hydrocyanation reaction, an isomerization reaction and a second hydrocyanation reaction. According to the method, the contents of specific components in a system is detected by adopting an online Raman spectrum, and reaction conditions are regulated and controlled based ona detection result, so accurate control on materials in each step in the reaction system is realized. The method provided by the invention can reduce the consumption of butadiene, and lower subsequent butadiene recovery energy consumption and equipment investment in the reaction; the content of hydrocyanic acid is monitored in real time, so hydrocyanic acid residues are reduced to a relatively low level, and the operation safety and the stability of a catalyst in the reaction process are improved; and the loss of the catalyst is reduced.

Description

technical field [0001] The invention relates to a method for preparing and separating chemical products, in particular to a method for preparing and separating adiponitrile and a device for preparing adiponitrile. Background technique [0002] Adiponitrile (ADN, adiponitrile), colorless and transparent oily liquid, slightly bitter, flammable, molecular formula NC(CH 2 ) 4 CN is an important organic chemical intermediate. It is mainly used in industry to produce hexamethylenediamine by hydrogenation, and then to produce polyhexamethylene adipamide (nylon 66) by polymerization reaction of hexamethylenediamine and adipic acid. Its material is similar to that of nylon Compared with 6, it has better strength, heat resistance, crystallinity, wear resistance and lower water absorption, and is widely used in automobiles, machinery industry, electronic appliances, precision instruments and other fields. In addition, adiponitrile synthesizes melamine-urea amino resin through guanami...

Claims

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Application Information

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IPC IPC(8): C07C255/04C07C253/10C07C253/34B01D3/06B01D3/42B01J4/00B01J4/02
CPCC07C253/10C07C253/34C07C253/00B01J4/008B01J4/02B01D3/06B01D3/42C07C2531/22C07C255/04C07C255/07B01D3/143B01D3/10C07C2531/24
Inventor 陈志荣吴文彬周贵阳丰明石兴兴马滔封智超张雄伟孙青徐勇
Owner ZHEJIANG NHU CO LTD
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