CN1105702C - Process for preparing monochloroacetic acid - Google Patents
Process for preparing monochloroacetic acid Download PDFInfo
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- CN1105702C CN1105702C CN00112627A CN00112627A CN1105702C CN 1105702 C CN1105702 C CN 1105702C CN 00112627 A CN00112627 A CN 00112627A CN 00112627 A CN00112627 A CN 00112627A CN 1105702 C CN1105702 C CN 1105702C
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- gas
- tower
- acetyl chloride
- chloride gas
- acid
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Abstract
The present invention relates to a technology for preparing chloroacetic acid, which comprises the following technological steps: (1) chlorine gas is led in the mixed acetic acid and mixed sulfur at the temperature of 90 to 100 DEG C; (2) after being led out of a condenser, the obtained acetyl chloride gas is in a liquid state and is absorbed by cold acetic acid for spare use; (3) liquid materials generated from step (1) and step (2) are proportionally mixed and are preheated; (4) the mixed liquid materials in step (3) are continuously put in a chlorinating reaction tower in a high position, and the chlorine gas is simultaneously led in the chlorinating reaction tower. After being condensed, chloro-acetyl chloride gas and acetyl chloride gas which are generated in the chlorinating reaction tower are recovered to circularly generate the crude product of chloroacetic acid. The technology of the present invention has the advantages of high chlorinating reaction speed, liquid state mixing, simple and convenient method, etc. The technology is suitable for continuous tower-type hydrogenizing reaction operation, and uses the existing production devices and the existing production conditions during preparation.
Description
The present invention relates to a process for preparing monochloroacetic acid.
At present, solid sulfur (S) is used as a catalyst in the chlorination reaction for preparing monochloroacetic acid domestically, is used for chlorination reaction in an intermittent enamel reaction kettle, is not suitable for tower-type continuous chlorination reaction, has too low reaction speed and poor catalytic effect, and is used for preparing acetic anhydride [ (CH) for monochloroacetic acid by individual enterprises at home and abroad and in China3CO)2O]As a catalyst, the acetic anhydride is more than one time higher than acetic acid, and the dosage is large, thus being uneconomical. Acetic anhydride belongs to an intermediate of a drug, and has complex management and monitoring relation and inconvenient use.
The invention aims to provide a process for preparing monochloroacetic acid, which is particularly suitable for tower-type continuous chlorination operation, and has good catalytic effect and high reaction speed.
The above object of the present invention is achieved by a technical solution of a process for preparing monochloroacetic acid, characterized in that: the method comprises thefollowing steps:
1. adding acetic acid and sulfur into an enamel reaction kettle according to the ratio of 25-35: 0.5-1.5, introducing chlorine gas at the temperature of 90-100 ℃, and keeping the reaction time as follows: generating gases such as acetyl chloride and the like within 7-9 hours;
2. leading out the gas in the reaction kettle, cooling the gas by a condenser to obtain liquid acetyl chloride, and then leading the liquid acetyl chloride and the residual gaseous acetyl chloride into another enamel kettle to be absorbed by cold acetic acid for later use;
3. preparing the liquid materials generated in the step 1 and the step 2 in a preparation kettle according to the proportion of 2: 1, and preheating at the temperature of about 60 ℃;
4. continuously placing the liquid material prepared in the step 3 into a chlorination reaction tower from the top at a high position, introducing chlorine gas into the bottom of the reaction tower, maintaining the temperature in the tower at 90-120 ℃, discharging generated hydrogen chloride gas, recovering the chlorine chloride gas after the chlorine chloride gas is changed into liquid through a condenser, and reacting the liquid material with acetic acid in the tower to generate a monochloroacetic acid crude productAnd the generated acetyl chloride gas reacts with chlorine gas to generate chloroacetyl chloride gas, and the chloroacetyl chloride gas is condensed and then is circulated in the tower to generate monochloroacetic acid. The reaction formula is as follows:
the attached drawing is a block diagram of the process steps of the invention.
Referring to the drawings: a preferred embodiment of the present invention is: adding acetic acid and solid sulfur into an initial material reaction kettle according to the ratio of 30: 1, and then introducing chlorine for 8 hours; the temperature in the continuous chlorination reaction column was chosen to be 100 ℃.
The invention has the following advantages due to the process:
1. the catalytic effect is good, the chlorination reaction speed is high and is not lower than that of acetic anhydride;
2. liquid state mixing, no caking or hole blockage phenomenon, and suitability for tower type continuous chlorination reaction operation;
3. the preparation of the catalyst utilizes the existing production equipment and conditions;
4. the method is simple and convenient for local job making in the production process;
5. the condensation and recycling of gases such as acetyl chloride and the like in the process are cheaper than acetic anhydride and other catalysts, and the economical efficiency is good.
Claims (1)
1. A process for preparing monochloroacetic acid is characterized in that: the method comprises the following steps:
(1) introducing chlorine gas into an enamel reaction kettle according to the ratio of 25-35: 0.5-1.5 of acetic acid and sulfuric acid at the temperature of 90-100 ℃ for the following time: generating acetyl chloride gas within 7-9 hours;
(2) leading out the gas in the reaction kettle, cooling the gas by a condenser to obtain liquid acetyl chloride, and then leading theliquid acetyl chloride and the residual gaseous acetyl chloride into another enamel kettle to be absorbed by cold acetic acid for standby;
(3) preparing the liquid materials generated in the step 1 and the step 2 in a preparation kettle according to the ratio of 2: 1, and preheating at the temperature of 60 ℃;
(4) and (3) continuously placing the liquid material prepared in the step (3) into a chlorination reaction tower from the top at a high position, introducing chlorine gas into the bottom of the reaction tower, maintaining the temperature in the tower at 90-120 ℃, discharging the generated hydrogen chloride gas, recovering the chloroacetyl chloride gas after the chloroacetyl chloride gas is changed into liquid through a condenser, reacting with acetic acid in the tower to generate a monochloroacetic acid crude product, leading out the chloroacetic acid crude product, reacting the generated acetyl chloride gas with the chlorine gas, then regenerating chloroacetyl chloride gas, condensing the chloroacetic chloride gas and then circularly producing monochloroacetic acid in the tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00112627A CN1105702C (en) | 2000-01-14 | 2000-01-14 | Process for preparing monochloroacetic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00112627A CN1105702C (en) | 2000-01-14 | 2000-01-14 | Process for preparing monochloroacetic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1264697A CN1264697A (en) | 2000-08-30 |
| CN1105702C true CN1105702C (en) | 2003-04-16 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00112627A Expired - Fee Related CN1105702C (en) | 2000-01-14 | 2000-01-14 | Process for preparing monochloroacetic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1105702C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL208653B1 (en) * | 2002-10-11 | 2011-05-31 | Akzo Nobel Nv | A process for the preparation of monochloroacetic acid |
| CN101386574B (en) * | 2007-09-10 | 2013-01-23 | 张天德 | Method for preparing chloracetic acid using acetyl chloride as catalyst |
| CN102976921A (en) * | 2012-11-30 | 2013-03-20 | 江苏省格林艾普化工股份有限公司 | Chlorinating liquid draining system for chloroacetic acid production |
| CN106242961B (en) * | 2016-07-29 | 2018-10-19 | 河北科技大学 | Production of chloroacetic acid equipment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063677A (en) * | 1991-01-31 | 1992-08-19 | 翟超进 | Produce the method for Monochloro Acetic Acid |
| CN1070183A (en) * | 1992-07-10 | 1993-03-24 | 何正� | Preparation process for chloroacetic acid |
-
2000
- 2000-01-14 CN CN00112627A patent/CN1105702C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063677A (en) * | 1991-01-31 | 1992-08-19 | 翟超进 | Produce the method for Monochloro Acetic Acid |
| CN1070183A (en) * | 1992-07-10 | 1993-03-24 | 何正� | Preparation process for chloroacetic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1264697A (en) | 2000-08-30 |
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Owner name: CHONGQING CHANGYUAN CHEMICAL INDUSTRY CO., LTD. Free format text: FORMER NAME: CHONGQING JIALING CHEMICAL PRODUCTS COD., LTD. |
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| CP01 | Change in the name or title of a patent holder |
Address after: Chongqing Jiangbei District No. 151 Dong River Patentee after: Chongqing Changyuan Chemical Corporation Limited Address before: Chongqing Jiangbei District No. 151 Dong River Patentee before: Jialing Chemical Products Co Ltd, Chongqing |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20030416 Termination date: 20170114 |