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Preparation methods of nitrile and corresponding amine

A manufacturing method and amide technology, applied in chemical instruments and methods, dehydration preparation of carboxylic acid amides, preparation of organic compounds, etc., can solve problems such as long reaction time, environmental pressure, reaction material loss and side reactions

Active Publication Date: 2015-11-04
SINOPEC YANGZI PETROCHEM +1
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AI Technical Summary

Problems solved by technology

[0005] But, the inventor of the present invention finds by research, and prior art is when producing corresponding aliphatic polyhydric nitrile by aliphatic polycarboxylic acid ammoniation method, in order to make ammoniation reaction fully carry out, this technology must be in the whole carboxylic acid During the ammoniation process or during a long reaction time, the ammonia source (ammonia gas) is continuously supplied (introduced) into the reaction system as a raw material, so the amount of ammonia gas is huge, resulting in the actual amount of ammonia gas far exceeding the ammoniation reaction. The amount used may be tens of millions of times the actual reaction requirement, resulting in extremely low utilization of ammonia gas
In addition, due to the extremely low utilization rate of ammonia, the ammonification reaction produces a large amount of waste ammonia water but cannot be recycled. After discharge, it will cause huge pressure on the environment, which is inconsistent with the current green production concept.
Moreover, since the ammoniation reaction of this technology adopts an overall higher reaction temperature (for example, exceeding 300° C.) and an overall longer reaction time, the energy consumption is higher, resulting in higher production costs, and there are also reactions during the reaction process. Severe material loss (for example, the reaction material is entrained out of the reaction system due to the continuous feeding of ammonia gas flow) and many side reactions, which make it difficult to effectively improve the quality and yield of nitrile products, etc.

Method used

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  • Preparation methods of nitrile and corresponding amine
  • Preparation methods of nitrile and corresponding amine
  • Preparation methods of nitrile and corresponding amine

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Embodiment

[0123] The following examples will be used to illustrate the present invention in further detail, but the present invention is not limited to these examples.

[0124] Preparation example of amide intermediate

[0125] Add 500g carboxylic acid raw material (chemically pure) in 1L open reactor, open and stir (600r / min), constantly pass into ammonia gas (chemically pure, water content is 5.1wt% in the carboxylic acid raw material from the reactor bottom, flow rate is 100g / min). Make the reaction at the reaction temperature T A T C After 1 hour, the ammonia gas was stopped. The contents of the reactor were sampled for 1H NMR and elemental analysis to characterize the amide intermediate. The specific reaction conditions and characterization results are shown in the following Table A-1, Table A-2, Table A-3, Table A-4 and Table A-5. These characterization results show that the obtained amide intermediate has extremely high purity (over 99%).

[0126] Table A-1

[0127]

[...

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Abstract

The invention relates to a preparation method of nitrile. Compared with the prior art, the preparation method has the characteristics of obvious reduction of the usage amount of ammonia sources, low environmental pressure, low energy consumption, low production cost, high purity and yields of nitrile products, and the like, and can be used for obtaining nitrile with a more complex structure. The invention also relates to a method for preparing corresponding amine with nitrile.

Description

technical field [0001] The invention relates to a process for the production of nitriles and a process for producing corresponding amines from the nitriles. Background technique [0002] Alicyclic polyhydric nitriles such as alicyclic dibasic nitriles are very important chemical intermediates. It and its derivatives have a very wide range of uses. For example, alicyclic diamines, one of its derivatives, have special properties , It is widely used in dyes, medicines, curing agents and high molecular polymers. [0003] The preparation methods of cycloaliphatic divalent nitriles are basically obtained by taking existing simple nitrile compounds as raw materials through certain reactions. The range of substrates applicable to these methods is very narrow and the reaction conditions are harsh, so they are not suitable for industrial production. [0004] At present, the preparation method of aliphatic polyvalent nitrile mainly adopts carboxylic acid ammoniation method, but there ...

Claims

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Application Information

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IPC IPC(8): C07B43/08C07B43/04C07C253/20C07C255/46C07C255/47C07D203/06C07D305/08C07D261/18C07D309/32C07D333/38C07D279/12C07C209/48C07C211/18C07C211/25
Inventor 孙海龙魏延雨陈新华缪军李娜高以龙阚林柏基业陈韶辉杨爱武许岳兴
Owner SINOPEC YANGZI PETROCHEM
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