Method for preparing 2-ethylhexyl chloroformate

A technology of ethylhexyl ester and chloroformic acid, which is applied in the purification/separation of carbonate/haloformate, the chemical method of reacting liquid and gaseous medium, and the method of chemically changing substances by using atmospheric pressure, etc. , can solve the problems of phosgene utilization rate of only 64%, long reaction time, high energy consumption of desolventization, etc., and achieve the effect of solving hydrogen chloride transfer, reducing reaction time and increasing reaction rate

Pending Publication Date: 2020-06-19
JIANGSU YANGNONG CHEM GROUP +3
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, because liquid phosgene is difficult to control and operate in the production process, there are many unsafe factors, and it is difficult to carry out industrial production
[0004] In 2008, Wang Chaohui and others disclosed that phosgene and isooctanol were used as raw materials to prepare chloroesters (referring to "Pilot Test Research on the Production Technology of Chloroformic Acid-2-Ethylhexyl Ester", Wang Chaohui, etc., Sichuan Chemical Industry, Volume 11, No. 3rd period, page 35-37), this method adopts photochemical reactor to react, but phosgene utilization rate only has 64%, and the gained chloroester content is 93%, and this method reaction time is up to 16h, and phosgene utilization rate is low
However, this method has low phosgene utilization rate, large amount of catalyst and high energy consumption for desolvation.
[0006] In summary, the existing synthesis method of 2-ethylhexyl chloroformate has the problems that hydrogen chloride cannot be discharged from the reaction system in time, the utilization rate of phosgene is low, the reaction time is long, the energy consumption is high, and the product purity is low.

Method used

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  • Method for preparing 2-ethylhexyl chloroformate
  • Method for preparing 2-ethylhexyl chloroformate
  • Method for preparing 2-ethylhexyl chloroformate

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Embodiment 1

[0051] The present embodiment provides a kind of method for preparing 2-ethylhexyl chloroformate, described method adopts the reaction kettle of two stages in series, specifically comprises the following steps:

[0052] (1) add isooctyl alcohol 1000g, 800g respectively in first stage, second stage reactor, phosgene passes through the reactor of two stages in series successively, reacts with the isooctyl alcohol in described reactor, makes chloroformic acid -2-Ethylhexyl ester; control the reaction temperature in each stage of reactor to be 10°C, the flow rate of phosgene to be 14g / min, and the degree of vacuum to be 200mmHg;

[0053] After the phosgene passes through the second-stage reaction kettle, it is passed into the sodium hydroxide solution for tail gas absorption. When the conversion rate of isooctyl alcohol in the first-stage reaction kettle is >99wt%, stop feeding phosgene, and directly inject the phosgene into the second-stage reaction kettle. Feed phosgene, and so ...

Embodiment 2

[0056] The present embodiment provides a method for preparing 2-ethylhexyl chloroformate, the method uses a three-stage series reaction kettle, and its schematic flow diagram is as follows figure 1 As shown, it specifically includes the following steps:

[0057] (1) Add isooctyl alcohol 1000g, 800g and 800g to the first-stage reactor 2, the second-stage reactor 3, and the third-stage reactor 4 respectively, and the phosgene passes through the three-stage successively through the phosgene feeding pipeline 1 Reactors connected in series react with the isooctanol in the reactor to produce chloroformic acid-2-ethylhexyl; controlling the reaction temperature in each grade of reactor is 0°C, and the flow rate of phosgene is 3.8g / min, Vacuum degree is 450mmHg;

[0058] Phosgene is passed into the potassium hydroxide solution of tail gas absorption tank 5 after the third stage reaction kettle 3 and carries out tail gas absorption, stops feeding phosgene when the isooctyl alcohol conv...

Embodiment 3

[0061] The present embodiment provides a kind of method for preparing 2-ethylhexyl chloroformate, described method adopts the reactor of four stages in series, specifically comprises the following steps:

[0062] (1) Add isooctyl alcohol 1000g, 800g, 800g, 800g to the first stage, second stage, third stage, and fourth stage reactor respectively, and phosgene passes through the reactor of four stages in series successively, and reacts with the React the isooctyl alcohol in the kettle to prepare 2-ethylhexyl chloroformate; control the reaction temperature in each stage of the reactor to be 30°C, the phosgene flow rate to be 5.9g / min, and the vacuum degree to be 600mmHg;

[0063] After the phosgene is passed through the fourth-stage reactor, it is passed into the sodium carbonate solution for tail gas absorption. When the conversion rate of isooctyl alcohol in the first-stage reactor is >99wt%, stop feeding phosgene, and directly pass it into the second-stage reactor. Enter phosg...

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Abstract

The invention provides a method for preparing 2-ethylhexyl chloroformate. The method comprises a step of reacting isooctyl alcohol with phosgene by using multiple stages of reaction kettles which areconnected in series. By adopting a micro-negative pressure system, hydrogen chloride generated by the reaction can be transferred in time, and unreacted phosgene in one reaction kettle can enter the next-stage reaction kettle for further reaction, so the utilization rate of phosgene and the conversion rate of isooctyl alcohol are improved, reaction time is greatly shortened, and 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. Background technique [0002] 2-Ethylhexyl chloroformate can be used to synthesize bis(2-ethyl)hexyl peroxydicarbonate (abbreviated as EHP), which is a colorless and transparent liquid, and EHP is a highly active initiator. Compared with dicarbonate initiators, its transportation and storage stability are better. Because it is insoluble in water, it is not easy to produce water phase polymers when initiating polymerization reactions, the tendency of sticking to the kettle is small, and the heat release of polymerization reactions is uniform Easy to obtain uniform reaction. Therefore, EHP has become one of the most promising initiators, and is widely used as polyethylene, polyvinyl chloride, polyvinyl acetate, polyacrylate, polyacrylonitrile and thermoplastic polyurethane, polyurethane vinyl chloride composite materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/02C07C68/08C07C69/96B01J19/18B01J3/00B01J10/00
CPCC07C68/02C07C68/08B01J19/1862B01J3/006B01J10/00C07C69/96
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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