Application of microreactor for preparation of ethylicin and production process of ethylicin

A micro-reactor, the technology of ethalicin, applied in the direction of control/regulation process, chemical/physical/physical-chemical reactor, chemical instruments and methods, etc., can solve the difficulty of ethalicin production process and equipment to achieve high efficiency, environmental protection, It is difficult to achieve the effect of industrialization, and it is difficult to achieve the problems of industrial production, so as to achieve the effect of production process safety, efficiency improvement, and concentration improvement.

Pending Publication Date: 2020-02-07
HAINAN ZHENGYE ZHONGNONG HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The microreactor has the advantages of increased specific area, enhanced heat transfer process, enhanced mass transfer process, safe reaction and easy scale-up. However, in different chemical productions, some are difficult to achieve industrialization effects, and some can be achieved, but not. goals of industrial production
[0005] The currently disclosed and industrially applied acetolicin production processes and equipment are difficult to achieve high efficiency and environmental protection. The applicant of the present invention has realized the preparation of acetolicin by using microreactors on the one hand. Quality and yield requirements, on the other hand, explored the application of microreactors to prepare acetolicin process requirements, and the production of acetolicin is efficient, environmentally friendly and safe

Method used

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  • Application of microreactor for preparation of ethylicin and production process of ethylicin
  • Application of microreactor for preparation of ethylicin and production process of ethylicin
  • Application of microreactor for preparation of ethylicin and production process of ethylicin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Raw material is that the concentration is 85% diethyl disulfide solution, glacial acetic acid and 45% nitric acid solution, glacial acetic acid and diethyl disulfide solution (the weight ratio of glacial acetic acid and diethyl disulfide solution is 5: 95) mix, prepare mixed solution, mixed solution and nitric acid solution pass into microreactor respectively after check valve respectively, the speed that mixed solution enters microreactor is 500L / hour, and the speed that nitric acid solution enters microreactor is 705L / hour, the gas mixture after passing through the microreactor enters the gas-liquid separator, and continues to stir and react for 2 hours at a constant temperature of 80°C in the gas-liquid separator to obtain a solution containing acetoallin, which is then discharged into the liquid separation tank. After layering, the oil phase and the water phase are separated, the concentration of acetoallin in the oil phase is detected and the yield of acetoallin is...

Embodiment 2

[0046] Embodiment 2 carries out pipeline reaction by the gas-liquid mixing that microreactor obtains

[0047] Raw material is that the concentration is 85% diethyl disulfide solution, glacial acetic acid and 45% nitric acid solution, glacial acetic acid and diethyl disulfide solution (the weight ratio of glacial acetic acid and diethyl disulfide solution is 5: 95) mix, prepare mixed solution, mixed solution and nitric acid solution pass into microreactor respectively after passing through check valve and pressurizing device respectively, the speed that mixed solution enters microreactor is 500L / hour, and nitric acid solution enters microreactor The speed of the device is 710L / hour, the gas mixture after passing through the microreactor is carried out to the gas-liquid separator, and the liquid after the gas-liquid separation is passed into the coil (nominal diameter Dn=20) for tubular reaction, and the coil is cooled to 55 ℃ and maintain a constant temperature, enter the gas-...

Embodiment 3

[0051] The gas-liquid mixing that embodiment 3 obtains by microreactor carries out microchannel reaction again

[0052] (1) 2 microchannel reactions

[0053] Raw material is that the concentration is 85% diethyl disulfide solution, glacial acetic acid and 45% nitric acid solution, glacial acetic acid and diethyl disulfide solution (the weight ratio of glacial acetic acid and diethyl disulfide solution is 5: 95) mix, prepare mixed solution, mixed solution and nitric acid solution respectively pass into microreactor (the microreactor of experiment number A3) (the 1st microchannel reaction) after check valve and pressurizing device respectively, mix The speed at which the solution enters the microreactor is 500L / hour, and the speed at which the nitric acid solution enters the microreactor is 497L / hour (70% of the total amount of nitric acid). The final liquid is passed into the microreactor (the microreactor of the experiment number A3), and the nitric acid solution is added at ...

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Abstract

The invention relates to an application of a microreactor for preparation of ethylicin and a production process of the ethylicin. The process of preparing the ethylicin by using the microreactor comprises the following steps: liquid raw materials and gas raw materials, or a mixture of the gas raw materials and the liquid raw materials are used as the ethylicin raw materials for entering the microreactor, wherein the liquid raw materials include diethyl disulfide, a catalyst and liquid oxidizing raw materials, and the gas raw materials are gas oxidizing raw materials, the raw materials are conveyed to the microreactor, and gas-liquid separation is performed to prepare the ethylicin or after gas-liquid separation is performed, the reaction is continued to prepare the ethylicin. The microreactor is used to prepare the ethylicin for the first time, various feasible processes of using the microreactor to prepare the ethylicin are developed, the efficiency of preparing the ethylicin is improved, and the concentration of the ethylicin product is improved; and the most important thing is that the time for producing the ethylicin can be shortened by controlling the conditions in the reaction process, and the different methods of producing the ethylicin have unique process characteristics and process advantages.

Description

technical field [0001] The invention belongs to the field of pesticide preparation, and in particular relates to the use of a microreactor for preparing acetoallin and its production process. Background technique [0002] The pure product of ethyl allicin (ethyl ethyl thiosulfonate) is a colorless oily transparent liquid, which decomposes when heated to 130-140°C. Soluble in ether, chloroform, ethanol, glacial acetic acid and other organic solvents, the solubility in water at room temperature is 1.2%. The industrial product is light yellow oily transparent liquid with garlic odor. Moderately toxic to warm-blooded animals. Its acute oral LD50 is 80 mg / kg in mice and 140 mg / kg in rats. Irritating to the skin of rabbits and guinea pigs. It has a broad spectrum of sterilization, and at a concentration of 1-100 mg / L, it can inhibit cotton anthracnose, R. Gibberella, striae, Tilletia, apple anthracnose, cucumber vine and other fungi and bacteria. [0003] CN105523980A disclo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C381/04B01J19/00
CPCB01J19/002B01J19/0093B01J2219/00263C07C381/04
Inventor 薛照先何昆明林光东
Owner HAINAN ZHENGYE ZHONGNONG HIGH TECH
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