CN1408707A - Process for recovering sodium mercaptoacetate from production of thia amino-ester waste liquid - Google Patents
Process for recovering sodium mercaptoacetate from production of thia amino-ester waste liquid Download PDFInfo
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- CN1408707A CN1408707A CN 01131727 CN01131727A CN1408707A CN 1408707 A CN1408707 A CN 1408707A CN 01131727 CN01131727 CN 01131727 CN 01131727 A CN01131727 A CN 01131727A CN 1408707 A CN1408707 A CN 1408707A
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- thioglycolic acid
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Abstract
Recovering sodium mercaptoacetate from waste liquid of thia-amino-ester production can eliminate the environmental pollution caused by the waste liquid and reduce the production cost of sodium mercaptoacetate. The recovering process includes extraction from the waste liquid, alkalization, letting stand and filtering to obtain sodium mercaptoacetate.
Description
The present invention relates to a kind of recoverying and utilizing method of chemical waste liquid, especially relate to a kind of method that from the waste liquid of producing thiourethane, reclaims Thioglycolic acid sodium salt.
In the background technology, thiourethane is international a kind of high-efficient collecting agent, and it is widely used in nonferrous metal mines such as copper, cobalt, nickel, gold, replaces with serious pollution xanthate, and has obtained good economic benefit and social benefit.Although thiourethane is a kind of new and effective mining collecting agent, the but a large amount of waste water (1: 6) of output in manufacturing processed.As not handling, can cause severe environmental pollution, therefore how to handle so a large amount of waste water, become the key of thiourethane existence.General in the world chloroactic acid method is adopted in the production of thiourethane at present, promptly utilize Mono Chloro Acetic Acid, soda ash, sec.-propyl xanthate, Monomethylamine or four kinds of industrial chemicals outputs of monoethylamine thiourethane, the a large amount of waste liquids of output mainly contain Thioglycolic acid sodium salt in the waste liquid simultaneously, and content is 8%～20%.And Thioglycolic acid sodium salt has been utilized as copper(greening)inhibitor in copper-molybdenum separation by mines such as molybdenum, copper, to replace violent in toxicity-sodium cyanide and the sodium sulphite that conventional method was adopted in the past fully.And Thioglycolic acid sodium salt adopts " hypo method " to produce more at present, and cost is higher, and the ton cost is about 1.6 ten thousand yuan.How Thioglycolic acid sodium salt is extracted from waste liquid, be not resolved always.
The objective of the invention is to overcome the weak point in the above-mentioned background technology, a kind of method that reclaims Thioglycolic acid sodium salt from the waste liquid of producing thiourethane is provided, adopt this method can from waste liquid, extract Thioglycolic acid sodium salt, both eliminated the pollution of waste liquid, greatly reduced the production cost of Thioglycolic acid sodium salt again environment.
For achieving the above object, the technical solution that the present invention adopts is as follows:
A kind of method that from the waste liquid of producing thiourethane, reclaims Thioglycolic acid sodium salt, its special character is: will produce the waste liquid that Thiovanic acid receives that contains that is produced in the thiourethane process and extract, back waste liquid and impure extraction agent obtain after leaving standstill coming together, the back waste liquid that will come together then alkalizes and through after leaving standstill, filtering, obtains the Thioglycolic acid sodium salt finished product.
Above-mentioned alkalization process can comprise once alkalization and double alkalisation.
Above-mentioned can passing through through the extraction agent that contains small amount of impurities that obtains after extracting and leaving standstill washed and be left standstill, and obtain the absolute extract agent.
Above-mentioned extraction agent can comprise ethers, alcohols, ester class, benzene class, ketone.
The additive that uses in the alkalization process can comprise sodium hydroxide, yellow soda ash, sodium bicarbonate, calcium oxide, calcium hydroxide, lime carbonate.
Above-mentioned extraction agent can be an ether, and the weight ratio of itself and waste liquid is 1: 6.
In the back waste liquid alkalization process of will coming together, can add calcium oxide when once alkalizing, its weight ratio is 5%, can add sodium hydroxide when carrying out double alkalisation, its weight ratio is 8%～9%.
Above-mentioned extraction process can carry out under the room temperature normal pressure and stir 0.5 hour, leaves standstill then 1 hour.
once alkalize and the double alkalisation process in, can under the room temperature normal pressure, stir 1 hour, behind the double alkalisation and left standstill press filtration then 36 hours.
A kind of method that from the waste liquid of producing thiourethane, reclaims Thioglycolic acid sodium salt, its special character is: will produce the waste liquid adding hydrochloric acid that contains Thioglycolic acid sodium salt that is produced in the thiourethane process earlier and carry out acidifying, adding ether then extracts, obtain organic phase and collection tail, organic phase is added the sodium hydroxide back extraction, obtain the Thioglycolic acid sodium salt finished product through leaving standstill.
Below the present invention is described in further detail:
Method one: will produce the waste liquid adding ether that contains Thioglycolic acid sodium salt that is produced in the thiourethane process and extract, the weight ratio of ether and waste liquid is 1: 6, stirred 0.5 hour under atmospheric pressure at room and left standstill 1 hour, back waste liquid and the ether that contains ELI obtain coming together.Add lime then in the waste liquid of collection back and once alkalize, once alkalization is carried out at normal temperatures and pressures, and the lime add-on is 5%, stirred 1 hour, and added sodium hydroxide again and carry out double alkalisation, double alkalisation carries out at normal temperatures and pressures, addition amount of sodium hydroxide is 8%～9%, add the back and stirred 1 hour, left standstill then 36 hours, obtain Thioglycolic acid sodium salt finished product and throw out, the throw out composition is calcium hydroxide and water glass, amount is few, has only 0.1 ‰, and the Thiovanic acid sodium content is about 25%.The sodium hydroxide solution that will contain the ether adding 0.5% of ELI simultaneously washs, the weight ratio of sodium hydroxide solution and ether is 1: 1, adding the back stirred 30 minutes, left standstill then 1 hour, obtain wash water and pure ether, wash water can return use, and ether can return extraction and use, and the above-mentioned washing and the process that leaves standstill are all carried out at normal temperatures and pressures.
Method two: will produce the waste liquid that contains Thioglycolic acid sodium salt that is produced in the thiourethane process and add hydrochloric acid and carry out acidifying, the PH=1 of solution during acidifying stirred 1 hour, left standstill then 0.5 hour, above-mentioned acidifying, stirred, left standstill process and all carry out at normal temperatures and pressures.Leave standstill back adding ether in solution and extract, the weight ratio of ether and waste liquid is 1: 2, stirs 1 hour, leaves standstill then 0.5 hour, obtains organic phase and collection tail, and the above-mentioned extraction and the process that leaves standstill are carried out at normal temperatures and pressures.The tail that will come together discards, and adds sodium hydroxide and carry out back extraction in organic phase, and addition amount of sodium hydroxide is 10%, temperature during back extraction≤30 ℃, and pressure is normal pressure.Add the back and stirred 1 hour, left standstill then 0.5 hour, obtain Thioglycolic acid sodium salt finished product and ether, ether can return use.
Compared with prior art, the advantage and the effect that have of the present invention is as follows:
1. the present invention has solved produced the waste water pollution problem that produces in the thiourethane process fully, does not appoint What discharge of wastewater, say from environmental angle significant, the sodium thioglycolate of recyclable high added value again simultaneously Product has significant Social benefit and economic benefit;
The present invention with produce sodium thioglycolate with " hypo method " and compare, production cost significantly reduces, Its ton cost only has 0.3 ten thousand yuan/tons, for numerous molybdenums, copper mine replace toxic articles cyanide and vulcanized sodium Created advantage;
3. remarkable in economical benefits of the present invention, its profits tax total value can reach 1.5 ten thousand yuan/tons, has wide city The field prospect.
4. utilize the inventive method can adopt four kinds of industrial chemicals be monoxone, soda ash, isopropyl xanthate, Monomethyl amine or monoethyl amine produce chemical products thiourethane and the sodium thioglycolate of two kinds of high added values, simultaneously not Produce any pollution.
Claims (10)
1. method that from the waste liquid of producing thiourethane, reclaims Thioglycolic acid sodium salt, it is characterized in that: will produce the waste liquid that contains Thioglycolic acid sodium salt that is produced in the thiourethane process and extract, back waste liquid and impure extraction agent obtain after leaving standstill coming together, the back waste liquid that will come together then alkalizes and through after leaving standstill, filtering, obtains the Thioglycolic acid sodium salt finished product.
2. the method that reclaims Thioglycolic acid sodium salt from the waste liquid of producing thiourethane according to claim 1 is characterized in that: described alkalization process comprises once alkalization and double alkalisation.
3. the method that reclaims Thioglycolic acid sodium salt from the waste liquid of producing thiourethane according to claim 1 and 2 is characterized in that: will wash and leave standstill through the extraction agent process that contains small amount of impurities that obtains after extracting and leaving standstill, and obtain the absolute extract agent.
4. the method that reclaims Thioglycolic acid sodium salt from the waste liquid of producing thiourethane according to claim 3, it is characterized in that: described extraction agent comprises ethers, ester class, alcohols, benzene class, ketone.
5. the method that reclaims Thioglycolic acid sodium salt from the waste liquid of producing thiourethane according to claim 4, it is characterized in that: the additive that uses in the alkalization process comprises sodium hydroxide, yellow soda ash, sodium bicarbonate, calcium oxide, calcium hydroxide, lime carbonate.
6. the method that from the waste liquid of producing thiourethane, reclaims Thioglycolic acid sodium salt according to claim 5, it is characterized in that: described extraction agent is an ether, the weight ratio of itself and waste liquid is 1: 6.
7. the method that from the waste liquid of producing thiourethane, reclaims Thioglycolic acid sodium salt according to claim 6, it is characterized in that: in the back waste liquid alkalization process of will coming together, add calcium oxide when once alkalizing, its weight ratio is 5%, add sodium hydroxide when carrying out double alkalisation, its weight ratio is 8%～9%.
8. the method that reclaims Thioglycolic acid sodium salt from the waste liquid of producing thiourethane according to claim 7, it is characterized in that: described extraction process carries out under the room temperature normal pressure and stirred 0.5 hour, leaves standstill then 1 hour.
9. the method that from the waste liquid of producing thiourethane, reclaims Thioglycolic acid sodium salt according to claim 8, it is characterized in that: once alkalize and the double alkalisation process in, all need at room temperature stir 1 hour, behind the double alkalisation and left standstill press filtration then 36 hours.
10. method that from the waste liquid of producing thiourethane, reclaims Thioglycolic acid sodium salt, it is characterized in that: will produce the waste liquid adding hydrochloric acid that contains Thioglycolic acid sodium salt that is produced in the thiourethane process earlier and carry out acidifying, adding ether then extracts, obtain organic phase and collection tail, organic phase is added the sodium hydroxide back extraction, obtain the Thioglycolic acid sodium salt finished product through leaving standstill.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01131727 CN1224613C (en) | 2001-09-20 | 2001-09-20 | Process for recovering sodium mercaptoacetate from production of thia amino-ester waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01131727 CN1224613C (en) | 2001-09-20 | 2001-09-20 | Process for recovering sodium mercaptoacetate from production of thia amino-ester waste liquid |
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| Publication Number | Publication Date |
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| CN1408707A true CN1408707A (en) | 2003-04-09 |
| CN1224613C CN1224613C (en) | 2005-10-26 |
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| CN 01131727 Expired - Fee Related CN1224613C (en) | 2001-09-20 | 2001-09-20 | Process for recovering sodium mercaptoacetate from production of thia amino-ester waste liquid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102513220A (en) * | 2011-12-21 | 2012-06-27 | 大冶有色设计研究院有限公司 | Chemical composition for recycling copper concentrate and molybdenum concentrate from copper and molybdenum mixed concentrate pulp |
| CN103360291A (en) * | 2013-06-21 | 2013-10-23 | 青岛联拓化工有限公司 | Method for preparing high-concentration mercaptoacetic acid from raffinate generated in production of O-alkyl-N-alkyl thinocarbamate |
| CN105237449A (en) * | 2015-11-09 | 2016-01-13 | 青岛联拓化工有限公司 | Method for preparing high-concentration mercaptoacetic acid from tail liquid of O-alkyl-N-alkyl thinocarbamate production |
| CN105254547A (en) * | 2015-11-05 | 2016-01-20 | 上海韬鸿化工科技有限公司 | Method for preparing high-quality mercaptoacetic acid from tail solution from O-alkyl-N-alkyl thinocarbamate production |
| CN110878037A (en) * | 2019-12-26 | 2020-03-13 | 山东科技大学 | High-value utilization method of tail liquid in thiourethane production |
| CN111689884A (en) * | 2020-07-24 | 2020-09-22 | 青岛联拓化工有限公司 | Method for preparing critical saturated aqueous solution of sodium thioglycolate by utilizing thiourethane tail liquid |
| CN112047867A (en) * | 2020-09-24 | 2020-12-08 | 湖北犇星新材料股份有限公司 | Method for purifying sodium thioglycolate |
-
2001
- 2001-09-20 CN CN 01131727 patent/CN1224613C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102513220A (en) * | 2011-12-21 | 2012-06-27 | 大冶有色设计研究院有限公司 | Chemical composition for recycling copper concentrate and molybdenum concentrate from copper and molybdenum mixed concentrate pulp |
| CN103360291A (en) * | 2013-06-21 | 2013-10-23 | 青岛联拓化工有限公司 | Method for preparing high-concentration mercaptoacetic acid from raffinate generated in production of O-alkyl-N-alkyl thinocarbamate |
| CN103360291B (en) * | 2013-06-21 | 2016-12-07 | 青岛联拓化工有限公司 | With producing the method that high concentration TGA prepared by the O-alkyl-N-alkyl sulfide tail washings by carbamate |
| CN105254547A (en) * | 2015-11-05 | 2016-01-20 | 上海韬鸿化工科技有限公司 | Method for preparing high-quality mercaptoacetic acid from tail solution from O-alkyl-N-alkyl thinocarbamate production |
| CN105254547B (en) * | 2015-11-05 | 2019-01-01 | 青岛联拓化工有限公司 | With production O- alkyl-N- alkyl sulfide by the method for the tail washings preparation high-quality thioacetic acid of carbamate |
| CN105237449A (en) * | 2015-11-09 | 2016-01-13 | 青岛联拓化工有限公司 | Method for preparing high-concentration mercaptoacetic acid from tail liquid of O-alkyl-N-alkyl thinocarbamate production |
| CN110878037A (en) * | 2019-12-26 | 2020-03-13 | 山东科技大学 | High-value utilization method of tail liquid in thiourethane production |
| CN111689884A (en) * | 2020-07-24 | 2020-09-22 | 青岛联拓化工有限公司 | Method for preparing critical saturated aqueous solution of sodium thioglycolate by utilizing thiourethane tail liquid |
| CN112047867A (en) * | 2020-09-24 | 2020-12-08 | 湖北犇星新材料股份有限公司 | Method for purifying sodium thioglycolate |
| CN112047867B (en) * | 2020-09-24 | 2023-02-03 | 湖北犇星新材料股份有限公司 | Method for purifying sodium thioglycolate |
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| Publication number | Publication date |
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| CN1224613C (en) | 2005-10-26 |
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Granted publication date: 20051026 Termination date: 20091020 |