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Halogenation reaction method

A technology of halogenation reaction and halogenation agent, applied in the direction of organic chemical methods, chemical instruments and methods, organic halogenation, etc., can solve problems such as uneven stirring, many side reactions, and long halogenation time, and achieve the effect of avoiding side reactions

Inactive Publication Date: 2017-02-15
北京化工大学苏州(相城)研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the fast reaction rate of the halogenation reaction, ordinary stirred tanks have always had the problem of uneven stirring, and it is almost impossible to achieve uniform mixing of liquid-liquid and gas-liquid during the process of halogenation reaction, which leads to overhalogenation and long halogenation time. , many side reactions, subsequent separation energy consumption and many other defects occur

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 uses a packed supergravity reactor as the core reactor device, and sets the supergravity level to 200g. Toluene and catalyst FeCl 3 The solution enters the supergravity reactor through the liquid inlet pipe, and the chlorine gas enters the supergravity reactor through the gas inlet pipe. The materials are efficiently mixed and halogenated in the supergravity reactor, and the reacted liquid materials leave from the liquid outlet of the supergravity reactor. In the supergravity reactor, the reacted gaseous substances leave the supergravity reactor through the gas outlet pipe. Wherein the molar ratio of toluene to chlorine is 1:0.9, the mass content of the catalyst in toluene is 0.02wt%, and the reaction body temperature is 20°C. After analysis and detection, the content of polyhalogenated by-products is 0.09%, and the yield of monochlorotoluene is 99.6%.

Embodiment 2

[0033] Example 2 uses a spiral channel type supergravity reactor as the core reactor device, and sets the supergravity level to 800g. Using acid catalysis, mix acetone and 35% hydrochloric acid and enter the high gravity reactor through the liquid inlet pipe, chlorine gas enters the high gravity reactor through the gas inlet pipe, and the materials are efficiently mixed and halogenated in the high gravity reactor. The final liquid material leaves the supergravity reactor from the liquid outlet of the supergravity reactor, and the reacted gaseous substance leaves the supergravity reactor through the gas outlet pipe. Wherein, the feeding molar ratio is acetone:chlorine:hydrochloric acid=4.5:1:0.01, and the reaction body temperature is 20°C. After analysis and detection, the content of monochloroacetone in the product is 98.9%, and the content of 1,1-dichloroacetone is 0.08%.

Embodiment 3

[0034] Embodiment 3 uses a stator-rotor type supergravity reactor as the core reactor device, and sets the supergravity level to 5g-10g. Ethyl acetoacetate and sulfuryl chloride are input into the supergravity reactor through the liquid inlet pipe and the liquid inlet pipe at the same time. The materials are mixed efficiently in the supergravity reactor and halogenated. The outlet leaves the high-gravity reactor, and the reacted gaseous substances leave the high-gravity reactor through the gas outlet pipe. The molar ratio of ethyl acetoacetate to sulfuryl chloride is 1.1:05, and the temperature of the reaction body is 12-18°C. After analysis and detection, the content of polyhalogenated by-products is 0.01 wt%, and the yield of ethyl 2-chloroacetoacetate is 97.8%.

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PUM

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Abstract

The present invention discloses a halogenation reaction method, which comprises: mixing at least an organic compound to be halogenated, a halogenating agent and a solvent capable of being optionally added or being not added and / or a diluent in a super gravity reactor to form a liquid-state reaction system, and carrying out a halogenation reaction to produce the halogenated product, preferably the super gravity level of the super gravity reaction is 5-800 g during the halogenation reaction. According to the present invention, the super gravity reactor such as the super gravity rotating bed reactor is used to perform the halogenation reaction, such that the rapid and microscopic mixing between the organic compound to be halogenated and the halogenating agent can be achieved, various kinds of side reactions caused by the too high local concentration can be effectively avoided, and the yield and the quality of the product can be significantly improved.

Description

technical field [0001] The invention relates to a halogenation reaction method, in particular to a method for utilizing a high-gravity reactor to carry out the halogenation reaction. [0002] technical background [0003] The organic halides prepared by the halogenation reaction of organic compounds are an important class of organic intermediates, mainly because organic halides can undergo both electrophilic substitution reactions and nucleophilic substitution reactions under certain conditions. Therefore, at present, the halogenation reaction is a very important organic unit reaction in the production process of many important pesticides, pharmaceutical intermediates and fine chemicals such as dyes and pigments. [0004] The industrial halogenation reaction process is mostly carried out by catalyst initiation or thermal initiation in a stirred tank. Due to the fast reaction rate of the halogenation reaction, ordinary stirred tanks have always had the problem of uneven stirr...

Claims

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Application Information

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IPC IPC(8): C07B39/00C07C25/02C07C17/12C07C49/16C07C45/63C07C69/716C07C67/307C07C19/075C07C17/16C07C211/52C07C209/74C07C43/303C07C41/52C07C39/28C07C37/62C07C23/10C07C17/02C07C17/14C07C22/04
Inventor 陈建峰何海赵宏高立东初广文
Owner 北京化工大学苏州(相城)研究院
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