Method and device for continuously preparing chloropivaloyl chloride by using micro-channel

A technology of chloropivaloyl chloride and pivaloyl chloride, applied in separation methods, carboxylate preparation, chemical instruments and methods, etc., can solve the problem of poor separation effect of impurities in the rectifying section, poor product quality stability, and poor control of reaction conditions. and other problems, to achieve the effect of enhancing the photochlorination reaction efficiency, less impurities, and short reaction time.

Active Publication Date: 2020-02-21
山东民基新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The photochlorination reaction equipment in the above-mentioned patents has low reaction efficiency, long reaction time, and high unit consumption; the impurity separation effect in the rectification section is poor, and poor control of reaction conditions leads to poor product quality stability

Method used

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  • Method and device for continuously preparing chloropivaloyl chloride by using micro-channel

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The pivaloyl chloride in the pivaloyl chloride storage tank is mixed with the pivaloyl chloride delivery pump at a flow rate of 500kg / h and the chlorine gas is mixed with the chlorine gas delivery pump at a flow rate of 278kg / h at the same time into the pipeline before the preprocessor, and enters the inner wall with MnS- The pretreatment of the ZnS composite catalyst pretreatment, the preprocessor controls the normal pressure, the temperature is 60 ℃, and the reaction residence time is 10s; the thickness of the MnS-ZnS composite catalyst on the inner wall of the preconditioner is 4.5mm; after that, it enters the microchannel photochlorination In the reactor, under the condition of ultraviolet light irradiation with a wavelength of 350nm, the reaction temperature is controlled at 75°C and the reaction residence time is 30s to obtain the chloropivaloyl chloride reaction liquid, and then the chloropivaloyl chloride reaction liquid enters the front distillation tower in a va...

Embodiment 2

[0035] The pivaloyl chloride in the pivaloyl chloride storage tank is mixed with the pivaloyl chloride delivery pump at a flow rate of 500kg / h and the chlorine gas is mixed with the chlorine gas delivery pump at a flow rate of 294kg / h at the same time into the pipeline before the preprocessor, and enters the inner wall with MnS- The pretreatment of the ZnS composite catalyst pretreatment, the preprocessor controls the normal pressure, the temperature is 50 ℃, and the reaction residence time is 15s; the thickness of the MnS-ZnS composite catalyst on the inner wall of the preconditioner is 5.0mm; after that, it enters the microchannel photochlorination In the reactor, under the condition of ultraviolet light irradiation with a wavelength of 340nm, the reaction temperature is controlled at 60°C and the reaction residence time is 30s to obtain the chloropivaloyl chloride reaction liquid, and then the chloropivaloyl chloride reaction liquid enters the front distillation tower in a va...

Embodiment 3

[0037] The pivaloyl chloride in the pivaloyl chloride storage tank is mixed with the pivaloyl chloride delivery pump at a flow rate of 500kg / h and the chlorine gas is mixed with the chlorine gas delivery pump at a flow rate of 250kg / h into the pipeline before the preprocessor, and enters the inner wall with MnS- The pretreatment of the ZnS composite catalyst pretreatment, the preconditioner controls the normal pressure, the temperature is 35 ℃, and the reaction residence time is 10s; the thickness of the MnS-ZnS composite catalyst on the inner wall of the preconditioner is 2.5mm; after that, it enters the microchannel photochlorination In the reactor, under the condition of ultraviolet light irradiation with a wavelength of 360nm, the reaction temperature is controlled at 80°C and the reaction residence time is 30s to obtain the chloropivaloyl chloride reaction liquid, and then the chloropivaloyl chloride reaction liquid enters the front distillation tower in a vacuum Control t...

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a method and device for continuously preparing chloropivaloyl chloride by using a micro-channel. The method comprises the steps: mixing pivaloyl chloride and chlorine, then adding the mixture to a preprocessor with a composite photocatalyst attached to the inner wall, pretreating, allowing the pretreated mixture to enter a micro-channel photochlorination reactor, carrying out a photochlorination reaction under an ultraviolet irradiation condition to prepare a chloropivaloyl chloride reaction solution, and rectifying the chloropivaloyl chloride reaction solution to obtain the chloropivaloyl chloride finished product. The inner wall of the preprocessor is lined with a nano MnS-ZnS composite photocatalyst to enhance the photochlorination reaction efficiency; the multi-wave band ultraviolet lamp adopts a surrounding mode, so that the harm of light diffusion to the surrounding environment is reduced while the utilization efficiency of ultraviolet light is enhanced; by adopting the micro-channel photochlorination reactor, the reaction time is shorter, the reaction is more thorough, and the impurities are fewer; a middle distillation tower is added in the rectification section, so that middle distillation impurities are separated more thoroughly, and the product quality is higher.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method and a device for continuously preparing chloropivaloyl chloride by using a microchannel. Background technique [0002] The synthetic technique of chloropivaloyl chloride has had many reports, and its main industrial production technique has following several: one is to prepare pivalic acid with isobutylene and carbon monoxide as initial raw material, react it with chlorinating agent, generate Pivaloyl chloride is produced by photochlorination; the second is to prepare pivalic acid with tert-butyl chloride and formic acid as starting materials, and react it with a chlorinating agent to generate pivaloyl chloride by photochlorination. Generate chloropivaloyl chloride; the third is to use tert-butyl chloride and carbon monoxide as raw materials, carbonylate pivaloyl chloride in the presence of a catalyst, and then chlorinate to obtain chloropivaloyl c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/62C07C53/50B01D3/14B01J19/00B01J19/12
CPCC07C51/62B01J19/0093B01J19/123B01D3/143C07C53/50Y02P20/584
Inventor 韦兵张海朋毛民基孙连付李建军黄超鹏杨中原郭勇杨承周晓倩成晓露
Owner 山东民基新材料科技有限公司
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