Method for producing epoxy chloropropane

A technology of epichlorohydrin and its production method, which is applied in the direction of organic chemistry, and can solve problems such as explosion hazards, safety hazards, and development hindrances

Inactive Publication Date: 2011-03-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of hydrogen peroxide as the oxygen source in the reaction raw materials has brought dangers that the traditional process does not have to the process.
Under the action of the catalyst, a small amount of hydrogen peroxide decomposes ineffectively during the reaction process, which easily causes the gas phase of the reactor to form an explosive mixed gas, which brings new safety hazards to the new process of direct epoxidation of allyl chloride. hindered the further development of the process route

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Add chloroform, 3-chloropropene, and catalyst to the reactor first, stir and heat up to the reaction temperature, then add hydrogen peroxide at a uniform speed within 1 hour, and the total reaction time is 2 hours. Feed mass ratio, chloroform: chloropropene: 50% (mass ratio) hydrogen peroxide: catalyst is 1: 1: 0.26: 0.08.

[0010] During the reaction process, the highest gas phase oxygen concentration is 1.3%, the conversion rate of allyl chloride is 29.6%, and the selectivity is 97.8%.

Embodiment 2

[0012] Add chloroform, 3-chloropropene, and catalyst to the reactor first, stir and heat up to the reaction temperature, then add hydrogen peroxide at a uniform speed within 30 minutes, and the total reaction time is 1.5 hours. The mass ratio of feed, chloroform: chloropropene: 50% hydrogen peroxide: catalyst is 1:1:0.26:0.08.

[0013] During the reaction process, the highest gas phase oxygen concentration is 3.8%, the conversion rate of allyl chloride is 30.2%, and the selectivity is 98.2%.

[0014] The mass ratio of 50% hydrogen peroxide to 3-chloropropene can be controlled to be 0.21-0.27:1.

[0015] A zirconia-type oxygen analyzer can be used, and the zirconia oxygen sensor is arranged above the gas phase of the reactor to monitor the oxygen concentration in the gas phase of the reactor online.

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Abstract

The invention relates to a method for producing epoxy chloropropane which is produced by using with 3-chloropropene as a raw material, phosphotungstic acid quaternary ammonium salt as a catalyst, hydrogen peroxide as an oxidizing agent and chloroform as a solvent by utilizing a phase transfer method. The method comprises the following steps of: adding the chloroform, the 3-chloropropene and the phosphotungstic acid quaternary ammonium salt into a reactor; stirring and raising temperature to a reaction temperature; adding the hydrogen peroxide to react at a bubble point temperature; and condensing, reflowing and taking away reaction heat in the reaction process through organic vapor. The oxygen concentration of reactor gas phase is controlled in the range of 0-6%; and the reaction temperature is the bubble point temperature, and the starting reaction temperature is 52-54 DEG C. Because the hydrogen peroxide decomposes in the reaction process, a blasting mixture is easily formed by the generated oxygen in the reactor gas phase and the organic vapor. The method is characterized in that the mixed gas in the reactor does not blast in the range, therefore, the blasting danger of the reactor gas is effectively eliminated.

Description

technical field [0001] The invention relates to a production method of epichlorohydrin, in particular to a method for controlling the oxygen concentration of a reactor in the production process of epichlorohydrin. Background technique [0002] Epichlorohydrin is an important organic chemical raw material and fine chemical product with a wide range of uses. The traditional epichlorohydrin production process is mainly propylene high-temperature chlorination method and propylene acetate method, and there is a large amount of "three wastes" pollution control problems in the process of saponification sewage discharge. With the advancement of the sustainable development strategy, the green synthesis route of epichlorohydrin with industrial value has become the focus of research in the industry. The current research mainly focuses on the exploration of the direct epoxidation process route of allyl chloride, using titanium silicon molecular sieve or phosphorus Tungstate is used as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/12
Inventor 姜杰谢传欣石宁张宏哲张晨王振刚徐伟孟庭宇王慧欣孙峰黄飞张铁郑俊鹤
Owner CHINA PETROLEUM & CHEM CORP
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