Efficient and safe adipic acid synthesis method

A synthesis method and technology of adipic acid, applied in chemical instruments and methods, carboxylate preparation, oxidation preparation of carboxylic acid, etc., can solve the problems of good mixing effect, low reaction liquid holdup, short residence time, etc. The effect of high yield and selectivity, low reaction liquid holdup, and improved safety factor

Pending Publication Date: 2021-10-29
NINGXIA RUITAI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the insufficient mixing of raw materials during the continuous synthesis of adipic acid in kettle, local easy back-mixing and overheating, large reaction liquid holding capacity and high reaction risk; system gas volume in the reaction process of tubular reactor and microchannel reactor large, the gas cannot be discharged from the reaction system in time, the actual residence time is short, and the device is complicated. An efficient and safe adipic acid synthesis method is provided. When it is applied, the process uses a microchannel reactor to achieve sufficient raw materials at a lower temperature. Mixing, the mixing process is liquid-liquid mixing (no gas generation), the mixing effect is much better than the kettle type and tubular type, which is beneficial to the subsequent synthesis reaction; this process completes the adipic acid synthesis reaction in the falling film reactor, and there is no return during the reaction process Mixed, the specific surface area of ​​the liquid film is large, and the gas generated by the reaction overflows from the film surface in time, which is conducive to the positive reaction, and the reaction yield and selectivity are high; Low, good mixing effect, greatly improved safety factor

Method used

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  • Efficient and safe adipic acid synthesis method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Such as figure 1 As shown, cyclohexanol and 50% nitric acid (copper 0.25%, vanadium 0.05%) dissolved in catalyst are used as raw materials, and the molar ratio of nitric acid:cyclohexanol is 5:1. The two streams of materials are pumped into the microchannel reactor through the pump, the mixing temperature is 30°C, and the mixing residence time is 20s. The discharged material enters the falling film reactor, the reaction temperature is 80°C, the reaction residence time is 20min, and the reaction pressure is 0.1MPa. The composition of the reaction solution was analyzed by HPLC. The discharged material was cooled, crystallized, suction filtered, and dried to obtain adipic acid. The conversion rate of raw materials was 100%, the selectivity was 96.2%, the content of adipic acid was 99.6%, and the yield of adipic acid was 95.8%.

Embodiment 2

[0030] Such as figure 1 As shown, cyclohexanol and 70% nitric acid (copper 0.25%, vanadium 0.05%) dissolved in catalyst are used as raw materials, and the molar ratio of nitric acid:cyclohexanol is 10:1. The two streams of materials are pumped into the microchannel reactor through the pump, the mixing temperature is 20°C, and the mixing residence time is 40s. The discharged material enters the falling film reactor, the reaction temperature is 80°C, the reaction residence time is 10min, and the reaction is carried out under normal pressure. The composition of the reaction solution was analyzed by HPLC. The discharged material was cooled, crystallized, suction filtered, and dried to obtain adipic acid. The conversion rate of raw materials was 100%, the selectivity was 93.2%, the content of adipic acid was 99.3%, and the yield of adipic acid was 92.5%.

Embodiment 3

[0032] Such as figure 1 As shown, cyclohexanone and 40% nitric acid (copper 0.5%, vanadium 0.25%) dissolved in catalyst are used as raw materials, and the molar ratio of nitric acid:cyclohexanone is 8:1. The two streams of materials are pumped into the microchannel reactor through the pump, the mixing temperature is 10°C, and the mixing residence time is 10s. The discharged material enters the falling film reactor, the reaction temperature is 80°C, the reaction residence time is 30min, and the reaction is carried out under normal pressure. The composition of the reaction solution was analyzed by HPLC, and the discharged material was cooled, crystallized, filtered and dried to obtain adipic acid. The conversion rate of raw materials was 100%, the selectivity was 95.2%, the content of adipic acid was 99.5%, and the yield of adipic acid was 94.7%.

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Abstract

The invention discloses an efficient and safe adipic acid synthesis method. The method comprises the following steps:raw materials containing a catalyst are fully mixed in a microchannel reactor; and the mixed material enters a falling film reactor, is heated to a reaction temperature, forms a liquid film after flow guiding, realizes adipic acid synthesis in the film, and the generated gas overflows from the surface of the film in time and then enters a tail gas post-treatment device through a gas phase pipeline. The micro-channel reactor is adopted to realize full mixing of raw materials at a lower temperature, the mixing process is liquid-liquid mixing (no gas is generated), the mixing effect is greatly superior to that of a kettle type and a tube type, the subsequent synthesis reaction is facilitated, the adipic acid synthesis reaction is completed in the falling film reactor, back mixing is avoided in the reaction process, and the specific surface area of a liquid film is large; and gas generated by the reaction overflows from the surface of the film in time, so that the reaction can be carried out forwards, the reaction yield and selectivity are high, continuous production of adipic acid is realized, the retention time is short, the reaction liquid holdup is low, the mixing effect is good, and the safety coefficient is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis applications, and specifically relates to a method for preparing adipic acid by using cyclohexanol / cyclohexanone as raw materials, fully mixing in a microchannel reactor, and performing oxidation reaction in a falling film reactor. Background technique [0002] Adipic acid, also known as fatty acid, is one of the most valuable dibasic acids among aliphatic dibasic acids. The application of adipic acid is mainly divided into two categories, namely nylon and non-nylon. The application of adipic acid in nylon products is mainly to manufacture nylon 66 salt (complex), polycondensation of nylon 66 salt to produce nylon 66 resin and nylon 66 fiber; the application in non-nylon is mainly to produce polyester polyol, and then produce Polyurethane products. In addition, adipic acid is also widely used in medicine, spices, pesticides, coatings, food, adhesives and dyes. The adipic acid process i...

Claims

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Application Information

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IPC IPC(8): C07C51/27C07C51/31C07C55/14
CPCC07C51/316C07C51/27C07C55/14
Inventor 石苏洋林洋严绘廖强孟海娟王明晨亢玉荣马荣慧
Owner NINGXIA RUITAI TECH
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