CN1660828A - Method for retrieving tetrahydrofuran from waste of pharmacy - Google Patents
Method for retrieving tetrahydrofuran from waste of pharmacy Download PDFInfo
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- CN1660828A CN1660828A CN 200410044138 CN200410044138A CN1660828A CN 1660828 A CN1660828 A CN 1660828A CN 200410044138 CN200410044138 CN 200410044138 CN 200410044138 A CN200410044138 A CN 200410044138A CN 1660828 A CN1660828 A CN 1660828A
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Abstract
A process for recovering tetrahydrofuran from the sewage generated in preparing medicines includes rectifying the sewage containing tetrahydrofuran, alcohol and water by rectifying tower to obtain tetrahydrofuran enriched fraction, extracting in high-polarity water to obtain the mixture of tetrahydrofuran and water, and absorbing water by solid alkali.
Description
Technical field
The invention discloses a kind of method that from pharmaceutical waste liquor, reclaims tetrahydrofuran (THF).
Background technology
Tetrahydrofuran (THF) (THF) is a kind of organic solvent of excellent property, and is of many uses, is called as menstruum universale in pharmaceutical industries, also is widely used in agricultural chemicals, the special rubber item; Also be used as the solvent of various coating, printing-ink, reaction process and manufacturing tape etc., be specially adapted to dissolve PVC, polyethylene.
Tetrahydrofuran (THF) can with most immiscible organic solvents, and can form azeotrope with water.Be the chemical industry of raw material, medical production in the industrial effluent that is discharged with the tetrahydrofuran (THF), tetrahydrofuran (THF) often coexists as liquid phase with water and other organic solvent to be difficult to separate, and both contaminate environment caused the waste of resource again.Tetrahydrofuran (THF), ethanol, water tertiary mixture belong to a kind of in this type of waste liquid.
This grade of Andrew George Haier of Britain discloses a kind of " reclaiming the method for tetrahydrofuran (THF) from the mixture that contains tetrahydrofuran (THF) and lower alkanols and water " in nineteen ninety Chinese patent 90106658.3.This method adopts two district's distillations, be condensed from the vapour shape mixture in first district, and in second district with elevated pressures again swallow heat up in a steamer, thereby obtain quite pure tetrahydrofuran (THF) in the bottom in second district.This method is owing to adopt the two-region distillation, and second district needs pressure distillation, to the requirement height of equipment, and the cost increasing, the operational stability of distillation tower is poor.
Lv Fengzhang equals to disclose a kind of " the recovery technology of tetrahydrofuran (THF) " in Chinese patent application number among the 01103145.X. February 27 calendar year 2001.Sepn process is to contain 10%～20% the tetrahydrofuran (THF) and the blending ingredients of ethyl acetate and water, adopt distillation method to obtain the mixed solvent that tetrahydrofuran (THF) accounts for main component, with sodium hydroxide ethyl ester in the mixture is hydrolyzed again, make extraction agent with toluene again, it is below 0.2% that the method that washes with water is washed till content to ethanol in the solvent, after the sodium hydroxide dehydration, do smart the steaming and obtain the tetrahydrofuran (THF) finished product.This method to ethanol and tetrahydrofuran (THF) what separate employing is solvent extration, need to add the 3rd kind of component toluene, thereby might bring burden, and may bring in the tetrahydrofuran (THF) finished product later separation, cause the pollution of product.
He Zhicheng etc. have delivered in " Shenyang chemical industry " the 4th phase of nineteen ninety-five in " from tetrahydrofuran (THF); ethanol; the research of separation of tetrahydrofuran in the water tertiary mixture system ", selected octane is as the extraction agent of tetrahydrofuran (THF), adopt the method separation of tetrahydrofuran of liquid-liquid extraction and rectifying, ethanol, water tertiary mixture system, Calcium Chloride Powder Anhydrous is a siccative, remove octane, micro ethanol in the tetrahydrofuran solution and water, utilize rectifying tower that both are separated into the tetrahydrofuran (THF) (66 ℃ of boiling points) of cat head and the octane (125.6 ℃ of boiling points) of tower still, the purity of product tetrahydrofuran (THF) reaches more than 98%, water content is below 1%, total recovery 62.2%.The shortcoming of this method is to need to use a large amount of organic extractants, and remains in easily in the product, and product purity is low.
Summary of the invention
The invention discloses a kind of method that from pharmaceutical waste liquor, reclaims tetrahydrofuran (THF), it is characterized in that it is 10%～50% (massfraction that utilization contains tetrahydrofuran (THF), as follows), ethanol is 3%～50%, water is 7%～50% pharmaceutical waste liquor, be to carry out preliminary rectifying earlier on 15 the rectifying tower in theoretical stage number, reflux ratio 1～5: 1, obtain 60～70 ℃ tetrahydrofuran (THF) enriched fraction; The tetrahydrofuran (THF) enriched fraction is carried out extracting rectifying, extraction agent is a water, can use tap water or distilled water, water preheat to 60～80 ℃, the charging mass ratio of extraction agent water and tetrahydrofuran (THF) enriched fraction is 1～5: 1,60～70 ℃ of cat head extraction temperature, reflux ratio 1～5: 1, the mixed fraction of acquisition tetrahydrofuran (THF) and water; The mixed fraction of tetrahydrofuran (THF) and water is added solid potassium hydroxide, the mass ratio of mixed fraction and solid potassium hydroxide is 10～20: 1, stirred 0.5～2 hour, and static 0.5～2 hour, be divided into two-layer up and down, separate, the upper strata is a tetrahydrofuran (THF) liquid, and this liquid is carried out rectifying, reflux ratio 1～5: 1 in rectifying tower, acquisition can be used for the pure tetrahydrofuran (THF) product that pharmaceutical manufacturing is used, and isolating lower floor liquid potassium hydroxide can be used for other purposes.
The present invention reclaims the method for tetrahydrofuran (THF) from pharmaceutical waste liquor, adopt big, cheap, the nonpoisonous and tasteless water of polarity as extraction agent, effective separation of tetrahydrofuran-ethyl alcohol blending ingredients, 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: tetrahydrofuran (THF) is 25.6%, and ethanol is 5.3%, and water is 69.1%, get this pharmaceutical waste liquor 200ml, joining in the 250ml there-necked flask, is to carry out rectifying on 15 the rectifying tower in theoretical stage number, and reflux ratio is 3: 1, cut extraction temperature is 63～65 ℃, obtain 52ml liquid, the gas chromatographic analysis result is 84.1% for tetrahydrofuran (THF), and ethanol is 3.4%, water is 12.5%, and the yield of tetrahydrofuran (THF) is 85.4%.
Embodiment 2:
Pharmaceutical waste liquor is formed: tetrahydrofuran (THF) is 36.4%, and ethanol is 5.1%, and water is 58.5%, get this pharmaceutical waste liquor 200ml, joining in the 250ml there-necked flask, is to carry out rectifying on 15 the rectifying tower in theoretical stage number, and reflux ratio is 3: 1, cut extraction temperature is 63～68 ℃, obtain 76ml liquid, the gas chromatographic analysis result is 82.6% for tetrahydrofuran (THF), and ethanol is 3.9%, water is 13.5%, and the yield of tetrahydrofuran (THF) is 86.2%.
Embodiment 3:
Get and consist of tetrahydrofuran (THF) 83.4%, ethanol 3.5%, the tetrahydrofuran (THF) enriched fraction mixed solution 200ml that the preliminary rectifying of water 13.1% obtains, place the 500ml there-necked flask, be to carry out extracting rectifying on 15 the extractive distillation column in theoretical stage number, extraction agent is a tap water, and the charging mass ratio of water and tetrahydrofuran (THF) enriched fraction is 2: 1, and is preheating to 75 ℃.Reflux ratio is 3: 1, and cut extraction temperature is 63～65 ℃, obtains 152ml liquid, and the gas chromatographic analysis result is 93.2% for tetrahydrofuran (THF), and ethanol is 0.02%, and water is 6.78%, and the tetrahydrofuran (THF) yield is 84.9%.
Embodiment 4:
Get and consist of tetrahydrofuran (THF) 83.4%, ethanol 3.5%, the tetrahydrofuran (THF) enriched fraction mixed solution 200ml that the preliminary rectifying of water 13.1% obtains, place the 500ml there-necked flask, be to carry out extracting rectifying on 15 the extractive distillation column in theoretical stage number, extraction agent is a distilled water, the charging mass ratio of water and tetrahydrofuran (THF) enriched fraction is 2: 1, and is preheating to 78 ℃, and reflux ratio is 3: 1, cut extraction temperature is 63～66 ℃, obtain 158ml liquid, the gas chromatographic analysis result is 92.6% for tetrahydrofuran (THF), and ethanol is 0.03%, water is 7.37%, and the tetrahydrofuran (THF) yield is 87.7%.
Embodiment 5:
Get the tetrahydrofuran (THF) cut 50ml of embodiment 3,4, add the 2.5g solid potassium hydroxide, stirred 40 minutes, static 1 hour, two-layer about being divided into, to separate, the upper strata is a tetrahydrofuran (THF) liquid, this liquid is carried out rectifying in rectifying tower, reflux ratio 2: 1, the massfraction that obtains the tetrahydrofuran (THF) product is 99.67, the massfraction of water is 0.33%, ethanol does not detect, and isolating lower floor liquid potassium hydroxide can be used for other purposes.
The present invention reclaims the method for tetrahydrofuran (THF) from pharmaceutical waste liquor, adopt big, cheap, the nonpoisonous and tasteless water of polarity as extraction agent, effective separation of tetrahydrofuran-ethyl alcohol blending ingredients, technical process is simple, the separation efficiency height, simple to operate, can reduce environmental pollution, valuable resource is reused.
Claims (3)
1. method that from pharmaceutical waste liquor, reclaims tetrahydrofuran (THF), it is characterized in that utilizing contain that tetrahydrofuran (THF) is 10%～50%, ethanol is 3%～50%, water is 7%～50% pharmaceutical waste liquor, be to carry out preliminary rectifying earlier on 15 the rectifying tower in theoretical stage number, reflux ratio 1～5: 1, obtain 60～70 ℃ tetrahydrofuran (THF) enriched fraction; The tetrahydrofuran (THF) enriched fraction is carried out extracting rectifying, and extraction agent is a water, and reflux ratio is 1～5: 1,60～70 ℃ of cat head extraction temperature, the mixed fraction of acquisition tetrahydrofuran (THF) and water; In the mixed fraction of tetrahydrofuran (THF) and water, add solid potassium hydroxide, stirred 0.5～2 hour, static 0.5～2 hour, two-layer about being divided into, to separate, the upper strata is a tetrahydrofuran (THF) liquid, this liquid is carried out rectifying in rectifying tower, reflux ratio is 1～5: 1, obtains to can be used for the pure tetrahydrofuran (THF) product that pharmaceutical manufacturing is used, and isolating lower floor liquid potassium hydroxide can be used for other purposes.
2. according to the described method that from pharmaceutical waste liquor, reclaims tetrahydrofuran (THF) of claim 1, it is characterized in that described extraction agent is a water, can be tap water, also can be distilled water, the charging mass ratio of water and tetrahydrofuran (THF) enriched fraction is 1～5: 1, and is preheating to 60～80 ℃.
3. according to the described method that from pharmaceutical waste liquor, reclaims tetrahydrofuran (THF) of claim 1, it is characterized in that the mixed fraction of described tetrahydrofuran (THF) and water and the mass ratio of solid potassium hydroxide are 10～20: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410044138 CN1660828A (en) | 2004-12-21 | 2004-12-21 | Method for retrieving tetrahydrofuran from waste of pharmacy |
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| CN 200410044138 CN1660828A (en) | 2004-12-21 | 2004-12-21 | Method for retrieving tetrahydrofuran from waste of pharmacy |
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| CN1660828A true CN1660828A (en) | 2005-08-31 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447636A (en) * | 2014-11-07 | 2015-03-25 | 济南大学 | Method and device for separating ethanol-tetrahydrofuran by extractive distillation by using dividing tower |
| CN105968073A (en) * | 2016-07-10 | 2016-09-28 | 青岛科技大学 | Method for recycling tetrahydrofuran in tetrahydrofuran-methanol-water by single-tower extractive distillation |
| CN107954950A (en) * | 2017-12-06 | 2018-04-24 | 成都化润药业有限公司 | The recovery method of high efficiente callback tetrahydrofuran |
| CN109180614A (en) * | 2018-11-20 | 2019-01-11 | 江苏九天高科技股份有限公司 | The purifying technique of tetrahydrofuran in a kind of hexane, tetrahydrofuran and aqueous mixtures |
| CN110964048A (en) * | 2019-12-18 | 2020-04-07 | 江苏创拓新材料有限公司 | Method for recycling organic boric acid waste liquid |
| CN111888792A (en) * | 2020-08-24 | 2020-11-06 | 大连理工大学 | Device and method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation |
| CN114437001A (en) * | 2022-01-19 | 2022-05-06 | 上海天汉环境资源有限公司 | Method for recovering tetrahydrofuran in wastewater |
-
2004
- 2004-12-21 CN CN 200410044138 patent/CN1660828A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447636A (en) * | 2014-11-07 | 2015-03-25 | 济南大学 | Method and device for separating ethanol-tetrahydrofuran by extractive distillation by using dividing tower |
| CN105968073A (en) * | 2016-07-10 | 2016-09-28 | 青岛科技大学 | Method for recycling tetrahydrofuran in tetrahydrofuran-methanol-water by single-tower extractive distillation |
| CN105968073B (en) * | 2016-07-10 | 2018-05-29 | 青岛科技大学 | The method of tetrahydrofuran in single column extracting rectifying recycling tetrahydrofuran-methanol-water |
| CN107954950A (en) * | 2017-12-06 | 2018-04-24 | 成都化润药业有限公司 | The recovery method of high efficiente callback tetrahydrofuran |
| CN109180614A (en) * | 2018-11-20 | 2019-01-11 | 江苏九天高科技股份有限公司 | The purifying technique of tetrahydrofuran in a kind of hexane, tetrahydrofuran and aqueous mixtures |
| CN109180614B (en) * | 2018-11-20 | 2023-08-29 | 江苏九天高科技股份有限公司 | Purification process of tetrahydrofuran in mixture of hexane, tetrahydrofuran and water |
| CN110964048A (en) * | 2019-12-18 | 2020-04-07 | 江苏创拓新材料有限公司 | Method for recycling organic boric acid waste liquid |
| CN110964048B (en) * | 2019-12-18 | 2022-05-03 | 江苏创拓新材料有限公司 | Method for recycling organic boric acid waste liquid |
| CN111888792A (en) * | 2020-08-24 | 2020-11-06 | 大连理工大学 | Device and method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation |
| CN114437001A (en) * | 2022-01-19 | 2022-05-06 | 上海天汉环境资源有限公司 | Method for recovering tetrahydrofuran in wastewater |
| CN114437001B (en) * | 2022-01-19 | 2023-12-26 | 上海天汉环境资源有限公司 | Recovery method of tetrahydrofuran in wastewater |
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