CN1644523A - Recovery of alcohol diisopropylamine from waste liquid of pharmaceutical industry - Google Patents
Recovery of alcohol diisopropylamine from waste liquid of pharmaceutical industry Download PDFInfo
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- CN1644523A CN1644523A CN 200410044139 CN200410044139A CN1644523A CN 1644523 A CN1644523 A CN 1644523A CN 200410044139 CN200410044139 CN 200410044139 CN 200410044139 A CN200410044139 A CN 200410044139A CN 1644523 A CN1644523 A CN 1644523A
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Abstract
Production of recovering alcohol and diisopropylamine from pharmaceutical effluent liquor is carried out by mixing pharmaceutical effluent liquor containing alcohol 40-90%, diisopropylamine 3-30%, and water 7-30% with acid matter, separating and recovering alcohol by acid extracting and rectifying technology, adding solid basic matter into the distilled raffinate at pan bottom, making solution value below 12, rectifying, and obtaining diisopropylamine product for pharmaceutical production. It achieves simple production, high separating efficient and no environmental pollution.
Description
Technical field
The invention discloses a kind of method that from pharmaceutical waste liquor, reclaims ethanol and Diisopropylamine.
Background technology
Ethanol is a kind of widely used chemical reagent and organic solvent, be the raw material of many important Chemicals and medicine intermediate, it all has a wide range of applications in chemical industry, dyestuff, paint, cosmetics production, medicine industry, electronic industry, national defense industry and other industrial production.Diisopropylamine is a kind of Organic Chemicals, is mainly used in synthetic medicine, agricultural chemicals (as weedicide etc.), synthetic dyestuff, thiofide, tensio-active agent, washing composition and defoamer etc.
In the cephalosporin analog antibiotic production process, need to use a large amount of organic solvents that medicine is purified, produce a large amount of organic liquid wastes after purifying, a kind of waste liquid wherein is the organic solvent component that contains recyclable utilizations such as ethanol, Diisopropylamine, ethanol content is 80%～90%, Diisopropylamine content 3%～5%, all the other are water and a small amount of high boiling substance.Process for separating and recovering research about this pharmaceutical waste liquor yet there are no relevant report both domestic and external.This waste liquid if can be reclaimed usefulness again, can not only be reduced production costs, improve economic benefit of enterprises, also can be reduced environmental pollution, limited resources is reused, realized sustainable development of resource.
The alcoholic acid boiling point is 78 ℃ in the component that contains in this pharmaceutical waste, 83 ℃ of Diisopropylamine boiling points, and both boiling points are more approaching, and can both form binary azeotrope with water, therefore are difficult to the three is thoroughly separated by traditional direct rectificating method.
Summary of the invention
The invention discloses a kind of method that from pharmaceutical waste liquor, reclaims ethanol and Diisopropylamine, it is characterized in that pharmaceutical waste liquor consists of ethanol 40%～90%, Diisopropylamine 3%～30%, water is 7%～30%, this waste liquid is mixed with acidic substance, acidic substance are the concentrated hydrochloric acid or the vitriol oil, the vitriol oil preferably, stir after 0.5～3 hour, the pH value of solution adjusts to 1～3, distillation, obtain the alcohol-water overhead product, this overhead product can obtain the alcohol product of purity more than 95% by the conventional rectification technology, or obtains the dehydrated alcohol product by the extractive distillation with salt technology; In addition, cauldron bottom residue after the distillation is added the solid alkaline material, and alkaline matter is sodium hydroxide or potassium hydroxide, stirs 0.5～2 hour, the pH value that makes solution is more than 12, static 0.5～2 hour, two-layer about being divided into, separate, the upper strata is that Diisopropylamine is main solution, this solution is carried out rectifying in rectifying tower, reflux ratio 3～15: 1, obtain can be used for the Diisopropylamine product that pharmaceutical industry uses.
The present invention reclaims the method for ethanol and Diisopropylamine from pharmaceutical waste liquor, adopt effectively separating alcohol-Diisopropylamine-water mixed system of acid extraction, alkali neutralization and distillation technology, obtain ethanol and Diisopropylamine product simultaneously, technical process is simple, the separation efficiency height, simple to operate, can reduce environmental pollution, valuable resource is reused.
Embodiment
Embodiment 1:
Pharmaceutical waste liquor is formed: the alcoholic acid massfraction is 82.5%, and the massfraction of Diisopropylamine is 3.7%, and the massfraction of water is 13.8%.The massfraction of each component is identical in the pharmaceutical waste liquor of following examples, and all represents with massfraction.
The hydrochloric acid 24ml of adding 33% stirred 1 hour in the 200ml pharmaceutical waste liquor, and the pH value of adjusting solution is 1.2, distill, obtain the overhead product of 197ml, the overhead product after the gas chromatographic analysis consists of ethanol 79.57%, Diisopropylamine 0.05%, water 20.38%, ethanol yield 95.0%.
Embodiment 2:
The hydrochloric acid 20ml of adding 33% stirred 2 hours in the 200ml pharmaceutical waste liquor, and the pH value of solution is 2.1, distilled, and obtained the overhead product of 193ml, and overhead product consists of ethanol 80.19%, Diisopropylamine 0.09%, water 19.72%, ethanol yield 93.8%.
Embodiment 3:
The sulfuric acid 12ml of adding 98% stirred 2 hours in the 200ml pharmaceutical waste liquor, and the pH value of solution is 1.1, distilled, and obtained the overhead product of 182ml, and overhead product consists of ethanol 86.6%, water 13.4%, and Diisopropylamine does not detect, ethanol yield 95.5%.
Embodiment 4:
The sulfuric acid 10ml of adding 98% stirred 1 hour in the 200ml pharmaceutical waste liquor, and the pH value of solution is 2.0, distilled, and obtained the overhead product of 181ml, and overhead product consists of ethanol 86.3%, water 13.7%, and Diisopropylamine does not detect, ethanol yield 94.7%.
Overhead product among the embodiment 1～4 just can obtain the alcohol product of purity more than 95% by the conventional rectification technology, or can obtain the dehydrated alcohol product by the extractive distillation with salt technology.
Embodiment 5:
Get the cauldron bottom residue 100ml after the distillation among the embodiment 1～2, add solid sodium hydroxide 20g, stirred 1 hour, pH value with pH test paper test soln is about 14, static 1 hour, is divided into two-layer up and down, separate, the upper strata is main solution for the 83ml Diisopropylamine, and gas chromatographic analysis consists of Diisopropylamine 92.3%, ethanol 3.2%, water 4.5 carries out rectifying, reflux ratio 10: 1 with this solution in rectifying tower, obtain the Diisopropylamine product 61ml of purity 96.6%, yield 77.0%.
Embodiment 6:
Get the cauldron bottom residue 100ml after the distillation among the embodiment 3～4, add solid potassium hydroxide 20g, stirred 40 minutes, pH value with pH test paper test soln is more than 14, static 1.5 hours, is divided into two-layer up and down, separate, the upper strata is main solution for the 85ml Diisopropylamine, and gas chromatographic analysis consists of Diisopropylamine 94.2%, ethanol 4.3%, water 1.5 carries out rectifying, reflux ratio 10: 1 with this solution in rectifying tower, obtain the Diisopropylamine product 65ml of purity 97.8%, yield 79.4%.
Embodiment 5～6 products can be used further to use in the pharmaceutical manufacturing.
By the foregoing description as seen, adopt effectively separating alcohol-Diisopropylamine-water mixed system of acid extraction, alkali neutralization and distillation technology, technical process is simple, and the separation efficiency height is simple to operate, can reduce environmental pollution, and valuable resource is reused.
Claims (3)
1. method that from pharmaceutical waste liquor, reclaims ethanol and Diisopropylamine, it is characterized in that utilizing contain that ethanol is 40%～90%, Diisopropylamine is 3%～30%, water is that 7%～30% pharmaceutical waste liquor mixes with acidic substance, stirred 0.5～3 hour, the pH value of solution adjusts to 1～3, distillation, obtain the alcohol-water overhead product, can obtain the alcohol product of purity more than 95%, or obtain the dehydrated alcohol product by the extractive distillation with salt technology by the conventional rectification technology; Cauldron bottom residue after the distillation is added the solid alkaline material, stirred 0.5～2 hour, the pH value of solution is more than 12, static 0.5～2 hour, two-layer about being divided into, separate, the upper strata is that Diisopropylamine is main solution, this solution is carried out rectifying in rectifying tower, reflux ratio 3～15: 1, obtain can be used for the Diisopropylamine product that pharmaceutical manufacturing is used.
2. the method that reclaims ethanol and Diisopropylamine from pharmaceutical waste liquor according to claim 1 is characterized in that described acidic substance can be concentrated hydrochloric acids, also can be the vitriol oil, the preferably vitriol oil.
3. the method that reclaims ethanol and Diisopropylamine from pharmaceutical waste liquor according to claim 1 is characterized in that described solid alkaline material can be sodium hydroxide or potassium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100441392A CN100391862C (en) | 2004-12-21 | 2004-12-21 | Recovery of alcohol diisopropylamine from waste liquid of pharmaceutical industry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100441392A CN100391862C (en) | 2004-12-21 | 2004-12-21 | Recovery of alcohol diisopropylamine from waste liquid of pharmaceutical industry |
Publications (2)
| Publication Number | Publication Date |
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| CN1644523A true CN1644523A (en) | 2005-07-27 |
| CN100391862C CN100391862C (en) | 2008-06-04 |
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| CNB2004100441392A Expired - Fee Related CN100391862C (en) | 2004-12-21 | 2004-12-21 | Recovery of alcohol diisopropylamine from waste liquid of pharmaceutical industry |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489043A (en) * | 2011-12-20 | 2012-06-13 | 湖南国发精细化工科技有限公司 | Recovery technology of methylamino avermectin benzoate amination solvent |
| CN105753677A (en) * | 2014-12-19 | 2016-07-13 | 蚌埠丰原涂山制药有限公司 | Method for recovering acetone and diethylamine from mother liquor obtained after propacetamol hydrochloride ammonification |
| CN106582060A (en) * | 2016-11-24 | 2017-04-26 | 北京航天试验技术研究所 | Vapor phase cleaning system and method of propellant tank |
| CN109608476A (en) * | 2018-12-28 | 2019-04-12 | 广州白云山医药集团股份有限公司白云山化学制药厂 | A kind of the production method for treating waste liquid and production method of cephalosporin analog antibiotic |
| CN112441929A (en) * | 2020-11-23 | 2021-03-05 | 浙江大学衢州研究院 | Method for separating mixture of diisopropylamine and ethanol by azeotropic distillation |
| CN117224988A (en) * | 2023-11-16 | 2023-12-15 | 内蒙古华欣药业有限公司 | Solvent recovery method and system |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58124578A (en) * | 1982-01-22 | 1983-07-25 | Jgc Corp | Distillation |
| CN1083802A (en) * | 1993-07-06 | 1994-03-16 | 兴城市化工总厂 | A kind of methanol sewage treatment technology |
| JPH07184628A (en) * | 1993-12-27 | 1995-07-25 | Mitsui Eng & Shipbuild Co Ltd | Treatment of fermentation waste liquid |
| CN1521133A (en) * | 2003-02-13 | 2004-08-18 | 宇 保 | Treatment method for waste water and waste residue in the production of diosgenin |
-
2004
- 2004-12-21 CN CNB2004100441392A patent/CN100391862C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489043A (en) * | 2011-12-20 | 2012-06-13 | 湖南国发精细化工科技有限公司 | Recovery technology of methylamino avermectin benzoate amination solvent |
| CN102489043B (en) * | 2011-12-20 | 2013-07-31 | 湖南国发精细化工科技有限公司 | Recovery technology of methylamino avermectin benzoate amination solvent |
| CN105753677A (en) * | 2014-12-19 | 2016-07-13 | 蚌埠丰原涂山制药有限公司 | Method for recovering acetone and diethylamine from mother liquor obtained after propacetamol hydrochloride ammonification |
| CN106582060A (en) * | 2016-11-24 | 2017-04-26 | 北京航天试验技术研究所 | Vapor phase cleaning system and method of propellant tank |
| CN106582060B (en) * | 2016-11-24 | 2019-11-22 | 北京航天试验技术研究所 | A kind of vapour phase cleaning system and method for propellant tank |
| CN109608476A (en) * | 2018-12-28 | 2019-04-12 | 广州白云山医药集团股份有限公司白云山化学制药厂 | A kind of the production method for treating waste liquid and production method of cephalosporin analog antibiotic |
| CN112441929A (en) * | 2020-11-23 | 2021-03-05 | 浙江大学衢州研究院 | Method for separating mixture of diisopropylamine and ethanol by azeotropic distillation |
| CN117224988A (en) * | 2023-11-16 | 2023-12-15 | 内蒙古华欣药业有限公司 | Solvent recovery method and system |
| CN117224988B (en) * | 2023-11-16 | 2024-01-30 | 内蒙古华欣药业有限公司 | Solvent recovery method and system |
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| Publication number | Publication date |
|---|---|
| CN100391862C (en) | 2008-06-04 |
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