Process for continuously producing chloroacetic acid through acetic anhydride catalytic method

A technology of chloroacetic acid and acetic anhydride, which is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid compounds, etc. It can solve the problem of poor quality of by-product hydrochloric acid, large equipment footprint, and difficult purification and purification, etc. Problems, to achieve the effect of being beneficial to downstream use, occupying a large area, and improving the level of automation

Pending Publication Date: 2019-06-07
HUBEI TAISHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 2. Due to the use of sulfur as a catalyst, the chloroacetic acid product contains elemental sulfur and its compounds, resulting in many impurities in the product chloroacetic acid, which affects downstream use
[0008] 3. The by-product hydrochloric acid contains elemental sulfur, sulfuric acid, sulfurous acid and other compounds, resulting in poor quality of by-product hydrochloric acid, and the purification is difficult and costly, and it is difficult to use downstream, and the environmental protection hazard is relatively large
[0009] 4. The device occupies a large area and has a low degree of automation
[0010] Some chloroacetic acid plants in China are produced by the acetic anhydride catalytic batch method, and the quality of the main product chloroacetic acid and by-product hydrochloric acid has improved, but due to the single-pot batch method, the device occupies a large area and has a low degree of automation

Method used

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  • Process for continuously producing chloroacetic acid through acetic anhydride catalytic method
  • Process for continuously producing chloroacetic acid through acetic anhydride catalytic method

Examples

Experimental program
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Effect test

Embodiment 1

[0050] 1) Take acetic acid and chlorine as raw materials, use acetic anhydride as a catalyst, control the temperature of the feed liquid at 98°C in the primary chlorination reaction main kettle, and make the concentration of monochloroacetic acid in the reaction solution reach 73% by the chlorine reaction, pump the The reaction liquid is delivered to the secondary chlorination reaction main kettle;

[0051] 2) In the secondary chlorination reaction main kettle, keep the temperature of the feed liquid at 97 ° C, continue to feed chlorine so that the concentration of monochloroacetic acid in the reaction solution reaches 88%, and terminate the chlorination reaction, pump the secondary chlorination reaction main kettle The reaction solution in the tank is transported to the hydrolysis tank;

[0052] 3) Raise the temperature of the reaction solution in the hydrolysis tank to 110°C, add an appropriate amount of water in the hydrolysis tank, control the water content in the reaction...

Embodiment 2

[0058] 1) Take acetic acid and chlorine as raw materials, use acetic anhydride as a catalyst, control the temperature of the feed liquid at 97°C in the primary chlorination reaction main kettle, and the chlorine reaction makes the concentration of monochloroacetic acid in the reaction solution reach 71%. The reaction liquid is delivered to the secondary chlorination reaction main kettle;

[0059] 2) In the secondary chlorination reaction main kettle, keep the temperature of the feed liquid at 99 ° C, continue to feed chlorine so that the concentration of monochloroacetic acid in the reaction solution reaches 87%, and terminate the chlorination reaction, pump the secondary chlorination reaction main kettle The reaction solution in the tank is transported to the hydrolysis tank;

[0060] 3) Raise the temperature of the reaction solution in the hydrolysis tank to 112°C, add an appropriate amount of water in the hydrolysis tank, control the water content in the reaction solution a...

Embodiment 3

[0066] 1) Take acetic acid and chlorine as raw materials, use acetic anhydride as a catalyst, control the temperature of the feed liquid at 100°C in the primary chlorination reaction main kettle, and make the concentration of monochloroacetic acid in the reaction solution reach 74% by the chlorine reaction, and pump the The reaction liquid is delivered to the secondary chlorination reaction main kettle;

[0067] 2) In the secondary chlorination reaction main kettle, keep the temperature of the feed liquid at 102 ° C, continue to feed chlorine so that the concentration of monochloroacetic acid in the reaction solution reaches 89%, and terminate the chlorination reaction, pump the secondary chlorination reaction main kettle The reaction solution in the tank is transported to the hydrolysis tank;

[0068] 3) Raise the temperature of the reaction solution in the hydrolysis tank to 114°C, add an appropriate amount of water in the hydrolysis tank, control the water content in the re...

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Abstract

The invention discloses a process for continuously producing chloroacetic acid through an acetic anhydride catalytic method. The production process comprises the steps: using acetic acid and chlorineas raw materials, using acetic anhydride as a catalyst, introducing chlorine for a reaction in a first-stage chlorination main kettle, conveying a reaction liquid to a second-stage chlorination main kettle through a pump, introducing chlorine for a reaction continuously in the second-stage chlorination main kettle, conveying the reaction liquid in the second-stage chlorination main kettle to a hydrolysis kettle through a pump, adding an appropriate amount of water to the hydrolysis kettle, removing unreacted intermediate products through a hydrolysis reaction, conveying the hydrolyzed reactionliquid to a rectification column through a pump, introducing steam into a reboiler of the rectification column for material heating, and separating the light component acetic acid and the heavy component chloroacetic acid from the reaction liquid; and condensing liquid foam in the reaction gas of the chlorination reaction kettles through a first-stage condenser and a second-stage condenser, returning the condensed liquid foam to the chlorination reaction kettles through reflux pipes separately, and sending the reaction gas condensed by the condensers to an exhaust gas treatment process for further treatment.

Description

technical field [0001] The invention relates to the production technology of chloroacetic acid, in particular to a new process of the catalyzed continuous method of chloroacetic acetic anhydride. Background technique [0002] Using acetic acid and chlorine as raw materials to produce chloroacetic acid, the chemical reaction formula is as follows: [0003] [0004] In the process of producing chloroacetic acid with glacial acetic acid and chlorine as raw materials, various production processes are derived according to the catalyst used in the reaction and whether the process is continuous. Among them, according to the catalyst used, it is divided into two types: sulfur catalysis method and acetic anhydride catalysis method, and according to whether the production process is continuous or not, it is divided into two types: batch method and continuous method. At present, the production process of chloroacetic acid in the domestic chloroacetic acid industry mainly includes t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/363C07C51/42C07C51/44C07C51/487C07C53/16
Inventor 赵信文田义群余义明
Owner HUBEI TAISHENG CHEM
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