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Continuous preparation method of 1-cyano-2-propenyl acetate

A technology of acryl acetate and cyano, which is applied in the field of continuous preparation of 1-cyano-2-propenyl acetate, can solve the problems of unfavorable industrial production, hidden safety hazards, and high production costs, and achieve labor Reduced strength, small footprint, and high production efficiency

Active Publication Date: 2020-12-15
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent US4336206 discloses a preparation method of 1-cyano-2-propenyl acetate, which will produce a large amount of cyanide-containing wastewater in the later stage, and more impurities will be produced during the reaction process, and the product needs to be distilled to improve the purity Carry out follow-up reaction again, simultaneously this method uses a large amount of carcinogenic solvent dichloromethane in order to improve yield, and on-site environment is bad, also has greatly influenced production capacity, and reaction liquid is in post-treatment desolvation and distillation process, and 1-cyano- 2-propenyl acetate is very easy to polymerize at high temperature, and there are safety hazards while the industrial production cost is high, so it is not conducive to industrial production

Method used

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  • Continuous preparation method of 1-cyano-2-propenyl acetate

Examples

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Effect test

Embodiment 1

[0043] 56g of acrolein and 102g of acetic anhydride are made into a mixed solution of acrolein and acetic anhydride for use, 49g of sodium cyanide and 114.3g of water are made into a 30% aqueous solution of sodium cyanide for use, and the temperature of the microchannel plate jacket oil is adjusted to -10°C, after the oil temperature stabilizes to -10°C, use the metering pump 1 to inject the sodium cyanide aqueous solution into the pre-cooling module of the microchannel reactor, then enter the reaction module, and use the metering pump 2 to mix the acetic anhydride and acrolein liquid into the reaction module of the microchannel reactor, wherein the feed rate of acetic anhydride and acrolein mixed solution is 10g / min (acrolein 0.0633mol / min, acetic anhydride 0.0633mol / min), and the feed rate of sodium cyanide aqueous solution is 10.339g / min (sodium cyanide 0.0633mol / min), the residence time of the reaction solution in the reactor is 96s, feed 10min, collect the microchannel eff...

Embodiment 2

[0045] 56g of acrolein and 102g of acetic anhydride are made into a mixed solution of acrolein and acetic anhydride for use, 49g of sodium cyanide and 114.3g of water are made into a 30% aqueous solution of sodium cyanide for use, and the temperature of the microchannel plate jacket oil is adjusted to 0°C, after the oil temperature stabilizes to 0°C, use the metering pump 1 to pump the sodium cyanide aqueous solution into the pre-cooling module of the microchannel reactor, then enter the reaction module, and use the metering pump 2 to pump the mixed solution of acetic anhydride and acrolein Enter the reaction module of microchannel reactor, wherein the feed rate of acetic anhydride and acrolein mixed solution is 10g / min (acrolein 0.0633mol / min, acetic anhydride 0.0633mol / min), the sodium cyanide aqueous solution feed rate is 10.339g / min (sodium cyanide 0.0633mol / min), the residence time of the reaction solution in the reactor is 96s, and the feed is 10min, and the microchannel...

Embodiment 3

[0047]56g of acrolein and 102g of acetic anhydride are made into a mixed solution of acrolein and acetic anhydride for use, 49g of sodium cyanide and 114.3g of water are made into a 30% aqueous solution of sodium cyanide for use, and the temperature of the microchannel plate jacket oil is adjusted to -10°C, after the oil temperature stabilizes to -10°C, use the metering pump 1 to inject the sodium cyanide aqueous solution into the pre-cooling module of the microchannel reactor, then enter the reaction module, and use the metering pump 2 to mix the acetic anhydride and acrolein liquid into the reaction module of the microchannel reactor, wherein the feed rate of acetic anhydride and acrolein mixed solution is 20g / min (acrolein 0.1266mol / min, acetic anhydride 0.1266mol / min), and the feed rate of sodium cyanide aqueous solution is 20.678g / min (sodium cyanide 0.1266mol / min), the residence time of the reaction solution in the reactor is 48s, the feed is 5min, the microchannel efflue...

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Abstract

The invention relates to a continuous preparation method of 1-cyan-2-propenyl acetate. Acrolein, acetic anhydride and sodium cyanide react to obtain the 1-cyano-2-propenyl acetate, wherein the reaction is carried out in a micro-channel continuous flow reactor. The preparation method disclosed by the invention is high in productivity and high in yield; According to the method, complete reaction canbe achieved under a solvent-free condition and a condition that the molar ratio of acrolein to acetic anhydride to sodium cyanide is 1:1:1, meanwhile, impurities are effectively reduced, the reactionselectivity is improved, a high-quality product can be obtained only through oil-water separation without distillation, no organic solvent is used in the whole reaction process, the green and environment-friendly requirements are met, and meanwhile, the cost is reduced.

Description

technical field [0001] The invention specifically relates to a continuous preparation method of 1-cyano-2-propenyl acetate. Background technique [0002] 1-cyano-2-propenyl acetate is mainly used as an intermediate in the production of the pesticide glufosinate-ammonium. [0003] Patent US4336206 discloses a preparation method of 1-cyano-2-propenyl acetate, which will produce a large amount of cyanide-containing wastewater in the later stage, and more impurities will be produced during the reaction process, and the product needs to be distilled to improve the purity Carry out follow-up reaction again, simultaneously this method uses a large amount of carcinogenic solvent dichloromethane in order to improve yield, and on-site environment is bad, also has greatly influenced production capacity, and reaction liquid is in post-treatment desolvation and distillation process, and 1-cyano- 2-propenyl acetate is very easy to polymerize at high temperature, and there are safety haza...

Claims

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Application Information

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IPC IPC(8): C07C253/00C07C255/16B01J19/00
CPCC07C253/00B01J19/0093C07C255/16
Inventor 蔡军义周炜周彬杨卓陈极
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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