Manufacturing method of nitrile and corresponding amine thereof

A manufacturing method and amide technology, applied in chemical instruments and methods, carboxylic acid amide dehydration preparation, organic compound preparation, etc., can solve the problems of inability to recycle, side reaction of reaction material loss, low selectivity of alkyl mononitriles, etc. question

Active Publication Date: 2015-04-29
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this ammoxidation method has the advantages of cheap and easy-to-get raw materials, short reaction route, and easy handling of products, there are four serious problems below: (1) In order to improve the yield, NH 3 The consumption is too large; (2) a large amount of waste ammonia water is produced in the reaction process, which causes great pressure on the environment and aftertreatment; (3) the reaction substrate range is narrow, and the selectivity is low when preparing alkyl mononitriles; (4) the reaction The temperature is high (above 410°C), and the requirements for catalyst preparation are very high
[0005] But, the inventor of the present invention finds by research, and prior art is when producing nitrile by carboxylic acid ammoniation method, in order to make ammoniation reaction fully carry out, require Ammonia gas is continuously fed into the reaction system as a raw material during the entire ammoniation process of carboxylic acid or within a long reaction time, so the amount of ammonia gas is huge, resulting in the actual a

Method used

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  • Manufacturing method of nitrile and corresponding amine thereof
  • Manufacturing method of nitrile and corresponding amine thereof
  • Manufacturing method of nitrile and corresponding amine thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0133] The following examples are used to illustrate the present invention in further detail, but the present invention is not limited to these

[0134] Example.

[0135] Amide Intermediate Preparation Example A

[0136] 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, Table A-5 and Table A-6. These characterization results show that the obtained amide intermediate has extremely high purity (over 99%).

[0137] In this emb...

preparation Embodiment A

[0151] Example A was prepared following the amide intermediate. Close described reaction kettle (when the boiling point of amide intermediate at normal pressure is equal to or lower than following reaction temperature T B ) or keep the reactor open (when the boiling point of the amide intermediate at normal pressure is higher than the following reaction temperature T B time), continue to stir (600r / min), change the reaction temperature to T B , at the reaction temperature T B keep T down D After 1 hour, the reaction was essentially complete. Then, close the reactor and connect the vacuum pump to make the vacuum in the reactor reach 20-50mbar (adjust accordingly according to the difference of the nitrile product type), and use the distillate as the nitrile product. Calculate the yield of the nitrile product, and take a sample for proton nuclear magnetic spectrum and elemental analysis to characterize the obtained nitrile product. The specific reaction conditions and charac...

preparation Embodiment A1

[0164] Example A was prepared following the amide intermediate. Seal described reactor, open stirring (600r / min), temperature of reaction is changed to T B . The reactor was connected to a vacuum pump, and the vacuum in the reactor was gradually reduced from 500 mbar until a trace amount (up to about 0.5 wt %) of the amide intermediate was detected in the effluent. Maintain the vacuum degree, the reaction time T D After 1 hour, the reaction was essentially complete. The distillate was taken as the nitrile product. Calculate the yield of the nitrile product, and take a sample for proton nuclear magnetic spectrum and elemental analysis to characterize the obtained nitrile product. The specific reaction conditions and characterization results are shown in the following Tables A1-7, A1-8, A1-9, A1-10 and A1-11. These characterization results show that the obtained nitrile product has a high purity (above 92%).

[0165] In these nitrile product preparation examples, optionall...

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Abstract

The invention relates to a manufacturing method of nitrile. Compared with the prior art, the manufacturing method has the characteristics of significantly reduced using amount of an ammonia source, low environmental pressure, low energy consumption, low production cost, high purity and yield of a nitrile product and the like, and nitrile with a more complex structure can be obtained. The invention also relates to a method for manufacturing corresponding amine from 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] Aromatic monohydric nitrile has a wide range of uses, and the demand for it in domestic and foreign markets has increased year by year in recent years. For example, benzonitrile is an important intermediate for the synthesis of chemicals such as pesticides and aromatic amines, an intermediate for advanced coatings such as benzomelamine, and a solvent for resin polymers, nitrile rubber and coatings. O-methylbenzonitrile can be used to synthesize the agricultural fungicides kresoxim-methyl, methamine, fluoramide and so on. m-Toluonitrile is an important pesticide, pharmaceutical and dye intermediate, widely used in the production of fine chemicals. p-Toluonitrile is one of the main raw materials of optical brighteners, and is also widely used in the synthesis of drugs, dyes and other fine ch...

Claims

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Application Information

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IPC IPC(8): C07B43/08C07B43/04C07C253/20C07C255/50C07C255/52C07C255/28C07C255/53C07C255/54C07C255/51C07C209/48C07C211/27C07C211/30C07C211/29C07C211/49C07C211/50C07C213/02C07C215/50C07C217/58C07C319/20C07C323/62C07C323/32C07D213/84C07D213/38C07D307/68C07D307/52C07D333/38C07D333/20C07D213/85C07D215/48C07D215/12C07D241/24C07D241/12C07D231/14C07D231/12C07D241/44C07D241/42C07D277/56C07D277/28C07D277/32
Inventor 孙海龙魏延雨高以龙陈新华缪军李娜阚林柏基业陈韶辉杨爱武许岳兴
Owner SINOPEC YANGZI PETROCHEM
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