Method for preparing 2-ethylhexyl chloroformate through continuous flow of micro-channel reactor

A microchannel reactor, a technology of channel reactors, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, preparation of phosgene or haloformate, etc., can solve the content of by-product diisooctyl carbonate High and low purity of chlorinated ester products, inability to transfer heat in time, etc., to achieve high industrial application value, improve phosgene utilization rate and ensure the effect of phosgene utilization rate

Inactive Publication Date: 2020-06-12
JIANGSU YANGNONG CHEM GROUP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has low phosgene utilization rate, large amount of catalyst and high energy consumption for desolvation.
[0004] US06919471B2 discloses a method of using phosgene and isooctyl alcohol as raw materials to carry out batch reaction to prepare chloroesters. The reaction time of this method is as long as 16h, and the utilization rate of phosgene is low.
[0005] Indian patent 946 / MUM / 2010A discloses a technology for the continuous synthesis of chloroesters in a continuous film reactor. This method uses a tower reaction. Although the tower reaction is more suitable for industrial continuous production, the control of the reaction temperature depends on external Physical cooling to achieve a reasonable reaction temperature range, the excess heat cannot be transferred in time, the by-product diisooctyl carbonate content is high, and the final chlorinated ester product has a low purity
[0006] In summary: the synthesis of 2-ethylhexyl chloroformate is mainly based on kettle-type and tower-type reactions, the reaction time is long, the utilization rate of phosgene is low, and the production cost is high. The content of by-product diisooctyl carbonate is too high, which affects product quality

Method used

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  • Method for preparing 2-ethylhexyl chloroformate through continuous flow of micro-channel reactor
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  • Method for preparing 2-ethylhexyl chloroformate through continuous flow of micro-channel reactor

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Embodiment 1

[0056] The present embodiment provides a kind of method that microchannel reactor continuous flow prepares -2-ethylhexyl chloroformate, and described method comprises the steps:

[0057] (1) According to the molar ratio 1.2:1, phosgene and isooctyl alcohol are passed into the microchannel reactor independently to react, by adjusting the back pressure valve at the reactor outlet, keep the reaction system pressure at 0.1MPa, pass through the heat exchanger To control the temperature to be 40°C, the residence time is 80s, and 2-ethylhexyl chloroformate is obtained to obtain the reaction mixture;

[0058] (2) The reaction mixture is passed into the lightening kettle, stirred and fed into nitrogen, and carried out lightening treatment to remove phosgene and hydrogen chloride until the phosgene content<50ppm, to obtain the 2-ethylhexyl chloroformate product ;

[0059] (3) Passing the tail gas after the lightening treatment into the sodium hydroxide solution for tail gas absorption,...

Embodiment 2

[0061] The present embodiment provides a kind of method that microchannel reactor continuous flow prepares -2-ethylhexyl chloroformate, and described method comprises the steps:

[0062] (1) According to the molar ratio 1.5:1, phosgene and isooctyl alcohol are passed into the microchannel reactor independently to react, by adjusting the back pressure valve at the reactor outlet, keep the reaction system pressure at 0.3MPa, pass through the heat exchanger To control the temperature to be 20°C, the residence time is 120s, and 2-ethylhexyl chloroformate is obtained to obtain the reaction mixture;

[0063] (2) The reaction mixture is passed into the lightening kettle, stirred and fed into nitrogen and argon, and carried out lightening treatment to remove phosgene and hydrogen chloride until the phosgene content<50ppm, to obtain chloroformic acid-2-ethyl Hexyl ester products;

[0064] (3) Pass the tail gas after the light removal treatment into the potassium hydroxide solution to ...

Embodiment 3

[0066] The present embodiment provides a kind of method that microchannel reactor continuous flow prepares -2-ethylhexyl chloroformate, and described method comprises the steps:

[0067] (1) According to the molar ratio 1.1:1, phosgene and isooctyl alcohol are passed into the microchannel reactor independently to react, by adjusting the back pressure valve at the reactor outlet, keep the reaction system pressure at 0.2MPa, pass through the heat exchanger To control the temperature to be 0°C, the residence time is 30s, and 2-ethylhexyl chloroformate is obtained to obtain the reaction mixture;

[0068] (2) The reaction mixture is passed into the lightening kettle, stirred and fed into nitrogen, and carried out lightening treatment to remove phosgene and hydrogen chloride until the phosgene content<50ppm, to obtain the 2-ethylhexyl chloroformate product ;

[0069] (3) passing the tail gas after the lightening treatment into the sodium carbonate solution for tail gas absorption, ...

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Abstract

The invention provides a method for preparing 2-ethylhexyl chloroformate through continuous flow of a micro-channel reactor. According to the method, isooctanol and phosgene react by adopting the micro-channel reactor. The reaction conditions can be accurately controlled, the phosgene utilization rate is high, the reaction time is short, the yield and selectivity of 2-ethylhexyl chloroformate arehigh, and the industrial application value is relatively high.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing 2-ethylhexyl chloroformate in continuous flow in a microchannel reactor. Background technique [0002] 2-ethylhexyl chloroformate, commonly known as chloroester, is mainly used to produce 2-ethylhexyl peroxydicarbonate. 2-ethylhexyl peroxydicarbonate, referred to as EHP, is mainly used as an initiator in the preparation of polyvinyl chloride. Among them, chloroester is prepared from isooctyl alcohol and phosgene (or solid light) through nucleophilic substitution reaction. [0003] CN101602667A discloses a production method of using solid phosgene and isooctyl alcohol as raw materials to prepare chloroesters. Toluene is used as a solvent and DMF is used as a catalyst to synthesize chloroesters by batch reaction. However, this method has low phosgene utilization rate, large amount of catalyst and high energy consumption for desolventization. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/02C07C69/96B01J19/00
CPCC07C68/02B01J19/0093C07C69/96
Inventor 孙诚徐林丁克鸿王怡明李幸霏刘越
Owner JIANGSU YANGNONG CHEM GROUP
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