Manufacturing method of nitrile and corresponding amine thereof

A manufacturing method and amide technology, which are applied in chemical instruments and methods, dehydration preparation of carboxylic acid amides, preparation of organic compounds, etc., can solve the problems of inconsistent production concepts, loss of reaction materials, side reactions, and high production costs.

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For this reason, 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 in the whole ammoniation process of carboxylic acid or in longer During the reaction time, ammonia gas is continuously fed 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 amount required for the ammoniation reaction, which may be tens of millions of times the amount required for the actual reaction. The utilization rate of ammonia gas is extremely low
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 (such as 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 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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  • 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
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Effect test

Embodiment

[0137] The following examples will be used to illustrate the present invention in further detail, but the present invention is not limited to these examples.

[0138] Amide Intermediate Preparation Example A

[0139] 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%).

[0140] In this embodime...

preparation Embodiment A

[0154] 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

[0169]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, A1-11 and A1-12. These characterization results show that the obtained nitrile product has a high purity (above 92%).

[0170] In these nitrile product preparation examples, opt...

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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] Nitrile compounds are a class of organic compounds containing cyano group (-CN), and are important intermediates in organic synthesis. Due to the high reactivity of the cyano group, the corresponding amine compounds can be prepared through hydrogenation reaction, which is an important raw material for the manufacture of medicines, pesticides, dyes, spices, surfactants, etc., and is widely used in various fields of the national economy . For example, aliphatic monoamine, one of its derivatives, is the basic raw material for the production of cationic, zwitterionic and nonionic surfactants. [0003] Aliphatic monoamines are divided into low-carbon aliphatic monoamines and high-carbon aliphatic monoamines. Representatives of low-carbon aliphatic monoamines include methylamine, ethylamine, and...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/03C07C255/33C07C255/34C07C255/13C07C255/07C07C255/25C07C255/10C07C255/17C07C255/35C07C255/31C07D213/57C07D209/18C07D333/24C07D317/60C07D233/64C07D307/54C07D307/16C07C323/52C07C319/12C07C209/48C07C211/03C07C211/27C07C211/17C07C217/16C07C213/02C07D213/38C07D401/04
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 CHINA PETROLEUM & CHEM CORP
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