CN103588658A - DMF recovery technology - Google Patents
DMF recovery technology Download PDFInfo
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- CN103588658A CN103588658A CN201310612731.7A CN201310612731A CN103588658A CN 103588658 A CN103588658 A CN 103588658A CN 201310612731 A CN201310612731 A CN 201310612731A CN 103588658 A CN103588658 A CN 103588658A
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Abstract
The invention provides a DMF recovery technology. The technology comprises the following steps: adding toluene to a medicine intermediate dimethyl formamide (DMF) mother liquor from a pharmaceutical production workshop, carrying out stirring heating to 80-130DEG C, carrying out infinite reflux timing water separation for 4-5.5h, maintaining the water layer level in a water separator at a position accounting for 1/2 of the volume of the water separator, separating out water when water exceeds the liquid level, cooling after finishing the water separation, and respectively completely taking out the upper-layer toluene and the lower-layer water in the water separator; and cooling the reaction liquid to below 30DEG C, carrying out reduced pressure distillation under the degree of vacuum below -0.095Mpa to obtain a toluene fraction, heating to 60-65DEG C to obtain a DMF fraction, and stopping heating for distillation ending when the liquid temperature rises to 105DEG C. No new organic solvents are introduced in the solvent recovery process of the technology, so the cost consumed by the introduction of the new components in the recovery process is avoided; and the technology adopts the reduced pressure distillation, so the energy and the cost are saved, and the DMF content and the water content of the recovered DMF accord with reuse requirements.
Description
Technical field
The invention belongs to medicine intermediate solvent recovery process field, especially relate to a kind of DMF recovery process.
Background technology
Dimethyl formamide (DMF) is widely used in bulk drug and pharmaceutical intermediate as solvent, obtains the solution that dimethyl formamide, water, a small amount of toluene and trace drug composition form in production.This solution is Dimethylformamide Residue, if do not reclaimed, causes on the one hand environmental pollution, increases environmental protection pressure, and production cost improves on the other hand.For dimethyl formamide is recycled, water, toluene and trace drug impurity must be removed.Traditional technology normally adopts rectifying or extraction to remove water wherein, reclaim solvent, but rectification process dewaters, the time is long and need rectifying tower, equipment investment is larger, and energy-output ratio is large, adopts extracting process to need to find suitable extraction agent, the technique that reclaims solvent is more complicated, introduced another kind of organic solvent, separated solvent and extraction agent cost are higher, and the solvent rate of recovery is low.
Summary of the invention
The object of this invention is to provide a kind of clean, efficient, energy-conservation DMF recovery process, reduce raw materials cost, guarantee the solvent quality reclaiming.
For realizing above-mentioned goal of the invention, technical scheme of the present invention is as follows:
A recovery process, comprises the steps:
1, in the pharmaceutical intermediate dimethyl formamide mother liquor from pharmaceutical manufacturing workshop, add toluene, stirring is warming up to 80-130 ℃, the total reflux minute water 4-5.5 hour that clocks, water layer liquid level in maintenance water trap is at water trap 1/2 volume place, after exceeding liquid level, divide water outlet, minute water is complete, and cooling is all shifted out toluene at the middle and upper levels of water trap and the water of lower floor respectively;
2, when above-mentioned reacting liquid temperature is down to below 30 ℃, carry out underpressure distillation, vacuum degree control-more than 0.095Mpa, the cut that starts to produce is toluene fraction, and when temperature rises to 60-65 ℃, the cut of generation is DMF cut, when liquid temperature rises to 105 ℃, stop heating, distillation finishes.
Consisting of of described pharmaceutical intermediate dimethyl formamide mother liquor: the quality percentage composition of dimethyl formamide is 40-45%, the quality percentage composition of water is 40%-50%, the quality percentage composition of toluene is below 5% and the pharmaceutical cpd of minute quantity.
Described pharmaceutical intermediate dimethyl formamide mother liquor is 4:1 to 12:1 with the volume ratio of the toluene adding.
The advantage that the present invention has with positively effect is: compare with present technology, do not introduce new organic solvent component in dimethyl formamide solvent removal process, avoided introducing because of removal process the expense that new component consumes.This technique is taked underpressure distillation, save energy expense, and dimethyl formamide moisture and the content of recovery, reached recycling requirement.In this recovery process, the dimethyl formamide rate of recovery reaches more than 50%, and cost approximately 4% economizes in raw materials.In this invention dimethyl formamide solvent removal process, have the waste after a small amount of waste water and a small amount of distillation, original nut liquid does not reclaim, therefore in contrast, resource utilization is high, discharging of waste liquid amount reduces, and technological operation is simple, is a kind of solvent recovery method of clean, energy-saving and environmental protection.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.
Embodiment 1
In four parts of pharmaceutical intermediate dimethyl formamide mother liquors, add a toluene, add the volume of toluene to be more than or equal to the volume of water trap, stir, heat up, 93 ℃ of liquid temperatures have cut to produce, 99 ℃ of liquid temperatures, and 80 ℃ of temperature produce total refluxs, separate at any time moisture.Backflow timing finishes for 4 hours, 130 ℃ of liquid temperatures, and 115 ℃ of temperature, are cooled to 50 ℃, and water in water trap and toluene are separated, and prepare underpressure distillation.Mother liquor vacuum tightness is-0.097MPa, heating, and the ethanol that condenser is logical-10 ℃, under agitation condition, carries out underpressure distillation, 39 ℃ of liquid temperatures, 32 ℃ of temperature, have cut to produce, and are toluene fraction, and this toluene fraction can be recycled.67 ℃ of liquid temperatures, 60 ℃ of temperature, receive positive cut DMF, 105 ℃ of liquid temperatures, 75 ℃ of temperature, underpressure distillation finishes.In the DMF reclaiming, the quality percentage amounts of water is 0.46%, DMF gas phase content is DMF content 96.25%, toluene level 3.75%, the DMF biodiversity percentage amounts <0.5% of this recovery, positive cut DMF gas phase content >=95%, meets the requirement recycling.
Embodiment 2
In four parts of pharmaceutical intermediate dimethyl formamide mother liquors, add a toluene, add the volume of toluene to be more than or equal to the volume of water trap, stir, heat up, 93 ℃ of liquid temperatures have cut to produce, 99 ℃ of liquid temperatures, and 80 ℃ of temperature produce total refluxs, separate at any time moisture.Backflow timing finishes for 5.5 hours, 130 ℃ of liquid temperatures, and 115 ℃ of temperature, are cooled to 50 ℃, and water in water trap and toluene are separated, and prepare underpressure distillation.Mother liquor vacuum tightness is-0.097MPa, heating, and the ethanol that condenser is logical-10 ℃, under agitation condition, carries out underpressure distillation, 39 ℃ of liquid temperatures, 32 ℃ of temperature, have cut to produce, and are toluene fraction, and this toluene fraction can be recycled.69 ℃ of liquid temperatures, 63 ℃ of temperature, receive positive cut DMF, 105 ℃ of liquid temperatures, 75 ℃ of temperature, underpressure distillation finishes.In the DMF reclaiming, the quality percentage amounts of water is 0.25%, DMF gas phase content is DMF content 98.54%, toluene level 1.46%, the DMF biodiversity percentage amounts <0.5% of this recovery, positive cut DMF gas phase content >=95%, meets the requirement recycling.
Above embodiments of the invention are had been described in detail, but described content is only preferred embodiment of the present invention, can not be considered to for limiting practical range of the present invention.All equalization variations of doing according to the present patent application scope and improvement etc., within all should still belonging to patent covering scope of the present invention.
Claims (3)
1. a DMF recovery process, comprises the steps:
1) in the pharmaceutical intermediate dimethyl formamide mother liquor from pharmaceutical manufacturing workshop, add toluene, stirring is warming up to 80-130 ℃, the total reflux minute water 4-5.5 hour that clocks, water layer liquid level in maintenance water trap is at water trap 1/2 volume place, after exceeding liquid level, divide water outlet, minute water is complete, and cooling is all shifted out toluene at the middle and upper levels of water trap and the water of lower floor respectively;
2) when above-mentioned reacting liquid temperature is down to below 30 ℃, carry out underpressure distillation, vacuum degree control-more than 0.095Mpa, the cut that starts to produce is toluene fraction, and when temperature rises to 60-65 ℃, the cut of generation is DMF cut, when liquid temperature rises to 105 ℃, stop heating, distillation finishes.
2. DMF recovery process according to claim 1, it is characterized in that: the consisting of of described step 1 Chinese traditional medicine intermediate dimethyl formamide mother liquor: the quality percentage composition of dimethyl formamide is 40-45%, the quality percentage composition of water is 40%-50%, and the quality percentage composition of toluene is below 5% and the pharmaceutical cpd of minute quantity.
3. DMF recovery process according to claim 1, is characterized in that: described step 1 Chinese traditional medicine intermediate dimethyl formamide mother liquor is 4:1 to 12:1 with the volume ratio of the toluene adding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310612731.7A CN103588658B (en) | 2013-11-26 | 2013-11-26 | A kind of DMF recovery technology |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310612731.7A CN103588658B (en) | 2013-11-26 | 2013-11-26 | A kind of DMF recovery technology |
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| CN103588658A true CN103588658A (en) | 2014-02-19 |
| CN103588658B CN103588658B (en) | 2015-11-18 |
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| CN201310612731.7A Active CN103588658B (en) | 2013-11-26 | 2013-11-26 | A kind of DMF recovery technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10370398B2 (en) | 2016-06-23 | 2019-08-06 | Tate & Lyle Technology Limited | Liquid-liquid extraction of DMF |
| CN111187180A (en) * | 2018-11-15 | 2020-05-22 | 江苏优士化学有限公司 | Method for recycling tetrafluoroterephthalonitrile synthetic wastewater |
| CN114539089A (en) * | 2022-01-21 | 2022-05-27 | 浙江大学衢州研究院 | Method for extracting and separating dimethyl formamide in wastewater by using eutectic solvent |
| CN115724708A (en) * | 2022-12-29 | 2023-03-03 | 南京长江江宇环保科技股份有限公司 | Method for separating toluene and N, N-dimethylformamide mixture |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587239A (en) * | 2004-07-22 | 2005-03-02 | 浙江大学 | Method for recovering toluene, butanone and dimethyl formamide from waste gas in wet synthetic leather production |
| CN102503759A (en) * | 2011-10-27 | 2012-06-20 | 天津大学 | Method and device for simultaneously recycling methylbenzene and dimethyl formamide in industrial waste gas by using solvent |
-
2013
- 2013-11-26 CN CN201310612731.7A patent/CN103588658B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587239A (en) * | 2004-07-22 | 2005-03-02 | 浙江大学 | Method for recovering toluene, butanone and dimethyl formamide from waste gas in wet synthetic leather production |
| CN102503759A (en) * | 2011-10-27 | 2012-06-20 | 天津大学 | Method and device for simultaneously recycling methylbenzene and dimethyl formamide in industrial waste gas by using solvent |
Non-Patent Citations (2)
| Title |
|---|
| 曲晶心，陈均志: "回收及处理合成革厂废水中DMF方法的研究进展", 《西部皮革》, vol. 31, no. 21, 30 November 2009 (2009-11-30), pages 34 - 38 * |
| 王景莲，等: "啶虫脒生产总含有DMF废水的回收利用", 《黑龙江科技信息》, no. 3, 31 December 2012 (2012-12-31), pages 43 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10370398B2 (en) | 2016-06-23 | 2019-08-06 | Tate & Lyle Technology Limited | Liquid-liquid extraction of DMF |
| US10899783B2 (en) | 2016-06-23 | 2021-01-26 | Tate & Lyle Technology Limited | Liquid-liquid extraction of DMF |
| CN111187180A (en) * | 2018-11-15 | 2020-05-22 | 江苏优士化学有限公司 | Method for recycling tetrafluoroterephthalonitrile synthetic wastewater |
| CN114539089A (en) * | 2022-01-21 | 2022-05-27 | 浙江大学衢州研究院 | Method for extracting and separating dimethyl formamide in wastewater by using eutectic solvent |
| CN114539089B (en) * | 2022-01-21 | 2024-01-30 | 浙江大学衢州研究院 | Method for extracting and separating dimethylformamide in wastewater by adopting eutectic solvent |
| CN115724708A (en) * | 2022-12-29 | 2023-03-03 | 南京长江江宇环保科技股份有限公司 | Method for separating toluene and N, N-dimethylformamide mixture |
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| CN103588658B (en) | 2015-11-18 |
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