CN1425649A - Process for preparing mercaptoacetic acid - Google Patents
Process for preparing mercaptoacetic acid Download PDFInfo
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- CN1425649A CN1425649A CN 02157244 CN02157244A CN1425649A CN 1425649 A CN1425649 A CN 1425649A CN 02157244 CN02157244 CN 02157244 CN 02157244 A CN02157244 A CN 02157244A CN 1425649 A CN1425649 A CN 1425649A
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Abstract
The present invention belongs to the field of chemical technology. The material for synthesizing mercaptoacetic acid is sodium bisulfide and chloroacetic acid. Under normal temperature and normal pressure, chloroacetic acid solution is dropped into sodium bisulfide solution while certain amount of H2S gas is introduced. The said process has high yield and synthesis converting rate over 90% but simple equipment and technological process and low material material cost.
Description
Technical field: the invention belongs to field of chemical technology, be used to produce Thiovanic acid.
Background technology: generally, the main path that adopts sodium hydrosulfide to produce Thiovanic acid has two kinds :-kind be low temperature process, a kind of is high-pressure process.
In low temperature process, Sodium sulfhydrate and Mono Chloro Acetic Acid initial reaction temperature are 5～10 ℃, 1 hour dropping time.Drip that temperature rises to about 20 ℃ after 1 hour, and then be warming up to 35 ℃ through 1 hour, insulation to reaction is finished under this temperature.Because of this reaction starting stage will react for some time at low temperatures, so be unfavorable for production operation.This kind method reaction times is also longer.Therefore, this technological process is implemented relatively difficulty in suitability for industrialized production.
In high-pressure process, owing to building-up reactions will be carried out under certain pressure, and reaction raw materials has very strong corrodibility, and therefore the material to reactor just has very high requirement.In industrial production, adopt this technology can increase facility investment, and in the production run process, have potential safety hazard.
Summary of the invention: in the present invention, the building-up reactions of Thiovanic acid is carried out at normal temperatures and pressures, and the characteristics of this method are to realize industrialization easily, and flow process is simple, operating safety.
Concrete technological process is: the sodium hydrosulfide that adds concentration about 15% earlier in reactor, in sodium hydrosulfide, drip about 20% chloroacetic acid solution of concentration again, about 1 hour of dropping time, temperature of reaction is 15～25 ℃, reacted again about 1 hour after dripping end, continue in conversion zone, to feed hydrogen sulfide in the reaction process.
In reaction process, after the reaction of Mono Chloro Acetic Acid and Sodium sulfhydrate generates Thioglycolic acid sodium salt, Thioglycolic acid sodium salt can continue with reaction solution in Sodium sulfhydrate react, generate by product NaSCH
2COONa emits hydrogen sulfide simultaneously.Therefore, if there is a large amount of hydrogen sulfide in the reaction system, can help suppressing the generation of side reaction.Because side reaction all can take place when reinforced and behind reinforced the finishing, so need to continue to feed hydrogen sulfide.There is hydrogen sulfide to generate in Sodium sulfhydrate and the chloroacetate reaction process, this part collection and confinement of gases can be used at the basin internal recycle.
In above-mentioned reaction, sodium hydrosulfide concentration is about 15%, chloroacetic acid solution concentration about 20%.Reactant concn is too high, and Synthesis conversion descends; Reactant concn is low excessively, can make the resultant density loss, increases the loss in the subsequent processes.
Embodiment:
Embodiment 1
Be reflected in the 1L four-hole boiling flask that stirring arm, thermometer and dropping funnel are housed and carry out, temperature of reaction is controlled by water-bath.Sodium hydrosulfide 467 grams of preparation 15% earlier, 20% chloroacetic acid solution 237 grams.Sodium sulfhydrate is all put into four-hole boiling flask, in dropping funnel, add chloroacetic acid solution, Mono Chloro Acetic Acid is dripped in sodium hydrosulfide, about 25 ℃ of temperature of reaction, 1 hour dropping time, dropwise, reaction soln was warming up to 35 ℃ in 0.5 hour.In entire reaction course, in conversion zone, feed hydrogen sulfide, the about 0.4～0.6L/min of tolerance.
It is 2 that above-mentioned reaction solution is acidified to the pH value with concentrated hydrochloric acid, with the extraction agent extraction, steams solvent under normal pressure, and the cut under 104～110 ℃/2.13kPa is collected in underpressure distillation again, and the yield of product is greater than 90%, and purity is greater than 99%.
Embodiment 2
Solution preparation and dropping process are with embodiment 1.About 25 ℃ of dropping temperature dropwises, and continues about 1 hour of reaction under the same temperature.In entire reaction course, in conversion zone, feed hydrogen sulfide, the about 0.4～.06L/min of tolerance.
Acidifying, extraction, still-process are the same, and the yield of product is greater than 90%, and purity is greater than 99%.
Claims (4)
1, a kind of method of producing Thiovanic acid is characterized in that at normal temperatures and pressures chloroacetic acid solution being dripped in sodium hydrosulfide, and stirs, and feeds H simultaneously in conversion zone
2S gas, reacted solution obtain the Thiovanic acid product through acidifying, extraction, distillation.
2, the method for claim 1 is characterized in that 10 ℃～25 ℃ of temperature of reaction.
3, the method for claim 1, the sodium hydrosulfide concentration that it is characterized in that is 15%, chloroacetic acid solution concentration 20%, 1 hour dropping time, temperature of reaction is 15～25 ℃, dropping was reacted 1 hour after finishing again.
4, the method for claim 1 is characterized in that logical H in the conversion zone
2S gas is to feed continuously in dropping and subsequent reaction process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157244 CN1218939C (en) | 2002-12-25 | 2002-12-25 | Process for preparing mercaptoacetic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157244 CN1218939C (en) | 2002-12-25 | 2002-12-25 | Process for preparing mercaptoacetic acid |
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| CN1425649A true CN1425649A (en) | 2003-06-25 |
| CN1218939C CN1218939C (en) | 2005-09-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 02157244 Expired - Fee Related CN1218939C (en) | 2002-12-25 | 2002-12-25 | Process for preparing mercaptoacetic acid |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921217A (en) * | 2010-09-20 | 2010-12-22 | 锦西化工研究院 | Method for synthesizing thioglycolic acid |
| CN102153496A (en) * | 2011-01-20 | 2011-08-17 | 浙江海虹控股集团有限公司 | Method for producing mercaptoacetic acid by using solid-state reaction |
| CN102174004A (en) * | 2011-03-24 | 2011-09-07 | 江南大学 | Synthesis method of p-vinylbenzyl mercaptan |
| CN102229548A (en) * | 2011-05-16 | 2011-11-02 | 潍坊益华化工有限公司 | Method for producing thioglycollic acid |
| CN104059003A (en) * | 2014-06-06 | 2014-09-24 | 湖北犇星化工有限责任公司 | Preparation method of aqueous solution of thioglycollic acid |
| CN104370783A (en) * | 2014-10-30 | 2015-02-25 | 天津河清化学工业有限公司 | Hydrogen sulfide recycling method and hydrogen sulfide recycling system for continuously producing mercaptoacetic acid by adopting sodium hydrosulfide method |
| KR20170041732A (en) * | 2014-08-07 | 2017-04-17 | 알케마 인코포레이티드 | Synthesis of 2,2,2-trifluoroethanethiol |
| CN112538036A (en) * | 2020-12-15 | 2021-03-23 | 山东沾化金嘉利化工科技有限公司 | Method for producing methyl thioglycolate based on sodium hydrosulfide method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193658B (en) * | 2014-08-21 | 2016-12-07 | 湖南立新环保科技发展有限公司 | A kind of preparation method of TGA |
-
2002
- 2002-12-25 CN CN 02157244 patent/CN1218939C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921217A (en) * | 2010-09-20 | 2010-12-22 | 锦西化工研究院 | Method for synthesizing thioglycolic acid |
| CN101921217B (en) * | 2010-09-20 | 2013-06-26 | 锦西化工研究院有限公司 | Method for synthesizing thioglycolic acid |
| CN102153496A (en) * | 2011-01-20 | 2011-08-17 | 浙江海虹控股集团有限公司 | Method for producing mercaptoacetic acid by using solid-state reaction |
| CN102174004A (en) * | 2011-03-24 | 2011-09-07 | 江南大学 | Synthesis method of p-vinylbenzyl mercaptan |
| CN102229548A (en) * | 2011-05-16 | 2011-11-02 | 潍坊益华化工有限公司 | Method for producing thioglycollic acid |
| CN104059003A (en) * | 2014-06-06 | 2014-09-24 | 湖北犇星化工有限责任公司 | Preparation method of aqueous solution of thioglycollic acid |
| KR20170041732A (en) * | 2014-08-07 | 2017-04-17 | 알케마 인코포레이티드 | Synthesis of 2,2,2-trifluoroethanethiol |
| US10717707B2 (en) | 2014-08-07 | 2020-07-21 | Arkema Inc. | Synthesis of 2,2,2-trifluoroethanethiol |
| KR102417295B1 (en) * | 2014-08-07 | 2022-07-07 | 알케마 인코포레이티드 | Synthesis of 2,2,2-trifluoroethanethiol |
| CN104370783A (en) * | 2014-10-30 | 2015-02-25 | 天津河清化学工业有限公司 | Hydrogen sulfide recycling method and hydrogen sulfide recycling system for continuously producing mercaptoacetic acid by adopting sodium hydrosulfide method |
| CN112538036A (en) * | 2020-12-15 | 2021-03-23 | 山东沾化金嘉利化工科技有限公司 | Method for producing methyl thioglycolate based on sodium hydrosulfide method |
| CN112538036B (en) * | 2020-12-15 | 2022-12-06 | 山东沾化金嘉利化工科技有限公司 | Method for producing methyl thioglycolate based on sodium hydrosulfide method |
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| Publication number | Publication date |
|---|---|
| CN1218939C (en) | 2005-09-14 |
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Granted publication date: 20050914 Termination date: 20121225 |