Process system and process for preparing chloropinacolone

A technology of a process system and pinatone, which is applied in the field of a process system for preparing monochloropinatone, can solve the problems of affecting yield and purity, and high local concentration, so as to avoid excessive chlorine concentration, reduce chlorine content, and realize The effect of subsequent processing

Pending Publication Date: 2021-03-02
HUBEI SHANSHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But because there will be excessive local concentration when passing through chlorine gas, cause generation dichloropinatone impurity, secondly, when distilling and purifying, material can be because of material residence time too long, methanol and hydrogen chloride react, produce more moisture, and Water will further react with chloropinatone, affecting yield and purity

Method used

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  • Process system and process for preparing chloropinacolone
  • Process system and process for preparing chloropinacolone
  • Process system and process for preparing chloropinacolone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The process system for preparing chloropinatone comprises:

[0047] The sequentially connected feeding unit A, reaction unit B, purification unit C and post-processing unit D;

[0048] The feeding unit A includes: a gas feeding device 1 and a liquid feeding device 2, the gas feeding device 1 includes a gas mixing tank 3, a first gas storage 101 and a second gas storage 102, the gas mixing tank 3 and The first gas storage 101 and the second gas storage 102 are respectively connected, and the liquid feeding device 2 includes a first liquid storage bottle 201 and a second liquid storage bottle 202;

[0049] The reaction unit B includes a reaction kettle 4, and the reaction kettle 4 is connected to the gas mixing kettle 3, the first liquid storage bottle 201 and the second liquid storage bottle 202 respectively;

[0050] The purification unit C comprises a distillation still 5 and a condenser 6 connected in sequence;

[0051] The post-processing unit D includes a gas abso...

Embodiment 2

[0059] Utilize the technique of embodiment 1 system to prepare monochloropinatone:

[0060] Pinatone is stored in the first liquid storage bottle, methanol is stored in the second liquid storage bottle, chlorine is stored in the first gas storage, and nitrogen is stored in the second gas storage.

[0061] Step S1: add pinacolone and methanol into the reaction kettle, mix and cool down to -3°C (cool the frozen brine that is passed into the jacket of the reaction kettle), and obtain a liquid mixed raw material;

[0062] Step S2: pass chlorine and nitrogen into the gas mixing tank and mix to obtain reaction gas. The flow rate of reaction gas is 50m3 / min, and then feed liquid mixed raw materials. When chlorine reaches the input amount, stop feeding reaction gas. Reaction under the condition of ℃-5℃, after the reaction, the reaction product is obtained;

[0063] In the reaction process, sampling and detection from time to time, when the content of monochloropinatone was 50% of the...

Embodiment 3

[0069] Chloropinatone was prepared according to the steps of Example 2, except that the ratio of the amount of pinacolone to chlorine gas was 3:1.

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Abstract

The invention provides a process system and process for preparing chloropinacolone. The process system comprises a feeding unit, a reaction unit, a purification unit and a post-treatment unit which are connected in sequence, wherein the feeding unit comprises a gas feeding device and a liquid feeding device, the gas feeding device comprises a gas mixing kettle, a first gas storage device and a second gas storage device, the gas mixing kettle is respectively connected with the first gas storage device and the second gas storage device, and the liquid feeding device comprises a first liquid storage bottle and a second liquid storage bottle. The process system has the advantages that reaction and purification of pinacolone and chlorine can be achieved, subsequent treatment of pollutants is achieved, nitrogen can be introduced into the device to dilute chlorine in the reaction period, and what is avoided is that the concentration of chlorine is too large, and by-products are generated.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a process system and process for preparing monochloropinatone. Background technique [0002] As early as the 1930s, there were explorations on the synthesis method of chloropinatone at home and abroad. The room temperature chlorination method with pinacolone as raw material and chloroform, carbon tetrachloride and carbon disulfide as solvents has a low yield. The yield of pinatone gas phase chlorination is improved, but a large amount of by-products are produced. Pinatone and chlorine are reacted at 0°C without using any solvent. The disadvantage of this process is that the conversion rate of pinatone is low and the yield is not ideal. [0003] In order to solve the problem of low conversion rate and selectivity in the above-mentioned chlorination process, improved methods have been proposed successively. At present, most processes use methanol as a solvent, and pi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/63C07C45/82C07C45/81C07C49/16
CPCC07C45/63C07C45/82C07C45/81C07C49/16
Inventor 曾晓兵李立生
Owner HUBEI SHANSHUI CHEM
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