CN105645501A - Method for recovering N,N-dimethyl acetamide from pharmaceutical wastewater - Google Patents
Method for recovering N,N-dimethyl acetamide from pharmaceutical wastewater Download PDFInfo
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- CN105645501A CN105645501A CN201510922637.0A CN201510922637A CN105645501A CN 105645501 A CN105645501 A CN 105645501A CN 201510922637 A CN201510922637 A CN 201510922637A CN 105645501 A CN105645501 A CN 105645501A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention relates to a method for recovering N,N-dimethyl acetamide (DMAC) from pharmaceutical wastewater, and belongs to the technical fields of environmental chemical engineering, especially extraction separation. In the wastewater generated by medical intermediate production, DMAC in industrial wastewater has a high value, and the mass content of DMAC is 5 to 20%. In the conventional method, DMAC is recovered through rectification, which has the disadvantages that the energy consumption is high, the cost is high, the directly-discharged wastewater is pollutant to the environment, the resource is wasted, and at the same time, the wastewater contains little dichloromethane and a plurality of acidic components. According to the provided method, dichloromethane with a low boiling point is taken as the extracting agent, a multi-stage extraction technology is adopted to recover DMAC from pharmaceutical wastewater in an extraction tower, and at the same time, a novel counter-current contact type extraction tower provided with multi-stage stirring pads and separation sections is designed. Before extraction, the waste liquid is subjected to pretreatments such as acid-alkali neutralization, settlement, and filtering, then the waste liquid is continuously fed into the extraction tower, and the content of DMAC in wastewater is less than 1% after extraction.
Description
Technical field
The present invention relates to a kind of method reclaiming DMAC N,N' dimethyl acetamide from medicine Wastewater by Solvent Extraction, belong to environmental chemical engineering technology, particularly extraction and separation technology field.
Background technology
DMAC N,N' dimethyl acetamide, also known as N,N-DIMETHYLACETAMIDE, is called for short DMAC, chemical formula CH3C(O)N(CH3)2It it is a kind of strong polar aprotic solvent, there is the features such as thermostability height, corrodibility is low, toxicity is little, urethane resin, polyimide resin there is good solubility energy, widespread use in the industry such as medicine, heat-resisting synthon, plastics film, vinyl cyanide spinning, refining of petroleum and pigment dyestuff. Especially in the production process of medicine intermediate, N, N-N,N-DIMETHYLACETAMIDE is as the high-value product in trade effluent, its mass content at 5-20%, if directly discharging, not only contaminate environment, also cause a large amount of N, the N-N,N-DIMETHYLACETAMIDE wasting of resources, and existing rectificating method relative energy consumption is big, cost height, does not calculate economically. Therefore, utilize low boiling point solvent extract to reclaim DMAC N,N' dimethyl acetamide and can save a large amount of energy, effectively reduce cost recovery. Due to normal with a small amount of methylene dichloride (0.5-2%) in medicine waste liquid, in order to not cause secondary pollution, have selected methylene dichloride and make the DMAC N,N' dimethyl acetamide in extraction agent recovery pharmaceutical wastewater.
In process waste water in the research of DMAC, it is that extraction agent reclaims the relevant extraction conditions containing DMAC waste water taking chloroform that Tsing-Hua University's forests and streams etc. have studied, Liu Li etc. have studied the optimum process condition that internal electrolysis removes DMAC in trade effluent, N,N-DIMETHYLACETAMIDE-water rectifying thermodynamics has been studied by Xing Haiyan etc., methylene dichloride-water-DMAC ternary system has been measured with containing salt quaternary system Liquid-liquid equilibrium data and has associated by Wang Chengxue etc., and is probed into by the recovery method of DMAC in waste water. On the basis of the present invention DMAC in the extraction and recovery waste water of laboratory, have studied take methylene dichloride as extraction agent, adopts counter-current extraction flow process, stirs the DMAC in tower extraction and recovery pharmaceutical wastewater. Both decrease waste water to the pollution of environment, reduce energy consumption, again for enterprise brings economic benefit.
Summary of the invention
It is an object of the invention to provide the method for DMAC N,N' dimethyl acetamide in a kind of recovery pharmaceutical wastewater extracted based on the tower with Multi-stage stirring.
The concrete technical scheme of the present invention is as follows:
(1) with the acid in alkali neutralized wastewater, and regulate the pH to 7-9 in waste water, alkali lye comprise sodium hydroxide, potassium hydroxide one or both, after standing sedimentation and Temperature fall, filter out the salt and other insoluble substance that are settled out;
(2) with the DMAC N,N' dimethyl acetamide in the stirring tower multi-stage countercurrent solvent extraction pharmaceutical wastewater of transport disengaging height;
(3) pre-treatment and extraction process are all normal temperature and pressure state, and extraction agent is methylene dichloride, and counter-current extraction progression is 5-8 level, and equipment is agitating extraction column, and stirring rake arranges number to be not less than extracting stage number, and the volume ratio of methylene dichloride and waste liquid is 1:1-2:1.
The basic structure schematic diagram of agitating extraction column of the present invention is as shown in Figure 1, the extraction height of tower and diameter proportion are between 4:1 to 6:1, the top of tower is provided with the entrance of heavy constituent extraction agent methylene dichloride and the spout of light constituent waste water extracting phase, this spout is in the upper end of extraction agent entrance, and the spacing of two mouthfuls is 2-4 tower footpath doubly. The lower end of tower is provided with the entrance of light constituent waste water and the outlet of heavy constituent extraction phase, and heavy constituent spout is located at the lower end of waterwater entrance, and the spacing of two mouthfuls is still 2-4 tower footpath doubly. Distance stirring rake is at a distance of the tower footpath of 0.5-1 times respectively for upper and lower admission port, and the distance between stirring rake is 1-2 beta footpath.
The height of standing sedimentation groove of the present invention should be 1.5-2.0 times of diameter, and strainer should be multilayer cavernous body, and lower end monolithic porous supports, aperture 2-4 millimeter, and percentage of open area is 0.25.
Useful effect: treatment process of the present invention is simple, extraction efficiency height, energy consumption are low, cost is low, have both reduced waste water to the pollution of environment, again for enterprise brings economic benefit, have good market application foreground.
Accompanying drawing illustrates:
Fig. 1 is agitating extraction column sketch in specification sheets of the present invention, wherein: 1-organic phase pump, 2-agitating extraction column, 3-is separated hypomere two-phase interface, and 4-heavy phase leaves standstill district, 5-waste drains pump, 6-multiple impellers, 7-two-phase mixtures district, section two-phase interface in 8-separation, 9-motor, A-extraction agent entrance, B-extraction phase (methylene dichloride heavy phase) exports, C-waste liquid entrance, and D-extracting phase (aqueous phase) exports.
Specific embodiment
Provide embodiment below the present invention to be specifically described; but it is worth being pointed out that following examples are only used to further illustrate the present invention; can not being interpreted as limiting the scope of the invention, improvement and the adjustment of some non-intrinsically safes that the present invention is made by the person skilled in the art in this field according to above-mentioned content of the present invention still belong to protection scope of the present invention.
Embodiment 1
Stirring the method for DMAC N,N' dimethyl acetamide in the waste water of tower Pyatyi counter-current extraction production cefuroxime acid, its operation steps is as follows:
(1) getting the waste water that 1000L produces cefuroxime acid, the massfraction of DMAC N,N' dimethyl acetamide is 20%, methylene dichloride mass content 1.5%, phosphoric acid quality content 7.5%, and hydrochloric acid mass content 8.2% puts into the beaker of 2000L. Then, progressively add sodium hydrate solid stirring and dissolving on a small quantity, the acid in neutralized wastewater, stir the pH value measuring in waste water, until regulating the pH to 7 of waste water. Leave standstill neutralizer 30 minutes, to normal temperature, filter out the insoluble substance of precipitation with sponge;
(2) waste water after process in step (1) is sent into the agitating extraction column with five stirring rakes (actual extraction progression is 5 grades) from the bottom of tower by waste water pump, speed is 2.4m3oh-1, meanwhile, dichloromethane extraction liquid is pumped into admission port on stirring tower with identical speed by extraction agent, two-phase fully contacts in stirring tower inside and carries out Pyatyi cross solvent extraction, and operational condition is normal temperature and pressure. Now, the volume ratio of methylene dichloride and waste liquid is 1:1, and tower footpath is 0.07m, and extraction section tower height is 0.30m, upper section and lower segment length be all 0.20m, the distance of two entrances and stirring rake is all 0.04m. Then, two-phase is respectively in tower top end and tower bottom layering, and the upper strata of tower top is gently the waste liquid phase after process mutually, and the organic phase of tower underlying layers is the methylene dichloride heavy phase that extraction absorbs DMAC N,N' dimethyl acetamide;
(3), after extraction terminates, two-phase extraction result adopts gas chromatographic analysis, and in its upper end extracting phase relief liquor, the massfraction of DMAC N,N' dimethyl acetamide is 0.894%, and recovery of extraction is 95.53%.
Embodiment 2
The Pyatyi adverse current agitating extraction column adopting embodiment 1 same, N in the waste water of remanufacture cefuroxime acid, N-N,N-DIMETHYLACETAMIDE, wherein N, the massfraction of N-N,N-DIMETHYLACETAMIDE is 12.5%, methylene dichloride mass content 1.1%, phosphoric acid quality content 1.9%, hydrochloric acid mass content 6.3%, its operation steps is as follows:
(1) get the waste water that 1000L produces cefuroxime acid, put into the beaker of 2000L. Progressively add sodium hydrate solid, stirring and dissolving on a small quantity, stir the pH value measuring waste water, regulate the pH to 9 of waste water. Leave standstill this neutralizer 30 minutes, to normal temperature, filter out the solid being settled out with sponge;
(2) waste water after process in step (1) is stirred tower from sending into by waste water pump at the bottom of tower, speed is 2.4m3oh-1, and meanwhile, dichloromethane extraction liquid is pumped into admission port on stirring tower with the speed of 4.83oh-1 by extraction agent, now, the volume ratio of methylene dichloride and waste liquid is 2:1;
(3), after extraction terminates, the gas chromatographic analysis result of two-phase extraction is: in the extracting phase relief liquor of tower upper end, the massfraction of DMAC N,N' dimethyl acetamide is 0.525%, and recovery of extraction is 95.8%.
Embodiment 3
Stirring the method for DMAC N,N' dimethyl acetamide in the tower six stage countercurrent extracting head sad factory effluent of big gun furan, its operation steps is as follows:
(1) getting the waste water that 500L produces cefuroxime acid, the massfraction of DMAC N,N' dimethyl acetamide is 16.2%, methylene dichloride mass content 1.8%, phosphoric acid quality content 8.9%, and hydrochloric acid mass content 6.6% puts into the beaker of 1000L. Then, progressively add potassium hydroxide solid stirring and dissolving on a small quantity, survey the pH value in waste water while stirring, until pH to 8. Leave standstill this neutralizer 30 minutes, after being chilled to normal temperature, filter out the insoluble substance of precipitation with sponge;
(2) waste water after process in step (1) is sent into (actual extraction progression is 6 grades) the stirring tower of 6 stirring rakes from the bottom of tower by waste water pump, speed is 2.0m3oh-1, meanwhile, dichloromethane extraction liquid is pumped into admission port on stirring tower with the speed of 2.2m3oh-1 by extraction agent, operates at normal temperatures and pressures. Now, the volume ratio of methylene dichloride and waste liquid is 1.1:1;
(3) the tower footpath stirring tower is 0.05m, and tower height is 0.40m, upper section and the transport disengaging height of hypomere be all 0.01m, the distance of two entrances and stirring rake is all 0.03m;
(4) extraction results is: in the extracting phase relief liquor of upper end, the massfraction of DMAC N,N' dimethyl acetamide is 0.561%, and recovery of extraction is 96.49%.
Embodiment 4
Stirring the method for DMAC N,N' dimethyl acetamide in tower eight stage countercurrent extraction cephalofruxin acid producing waste water, its operation steps is as follows:
(1) getting the waste water that 500L produces cefuroxime acid, the massfraction of DMAC N,N' dimethyl acetamide is 5.5%, methylene dichloride mass content 1.0%, phosphoric acid quality content 5.8%, and hydrochloric acid mass content 4.9% puts into the beaker of 1000L. Then, progressively add potassium hydroxide solid stirring and dissolving on a small quantity, survey the pH value in waste water while stirring, until pH to 7. Leave standstill this neutralizer 30 minutes, after being chilled to normal temperature, filter out the insoluble substance of precipitation with sponge;
(2) waste water after process in step (1) is sent into (actual extraction progression is 8 grades) the stirring tower of 8 stirring rakes from the bottom of tower by waste water pump, speed is 1.4m3oh-1, meanwhile, dichloromethane extraction liquid is pumped into admission port on stirring tower with the speed of 2.1m3oh-1 by extraction agent, operates at normal temperatures and pressures. Now, the volume ratio of methylene dichloride and waste liquid is 1.5:1;
(3) the tower footpath stirring tower is 0.05m, and tower height is 0.40m, upper section and the transport disengaging height of hypomere be all 0.10m, the distance of two entrances and stirring rake is all 0.03m;
(4) extraction results is: in the extracting phase relief liquor of upper end, the massfraction of DMAC N,N' dimethyl acetamide is 0.127%, and recovery of extraction is 97.70%.
Finally it should be noted that, above embodiment is only in order to illustrate the technical scheme of the present invention and unrestricted, although with reference to better embodiment to invention has been detailed description, it should be appreciated by those skilled in the art that, a point technical scheme for invention can be modified or replaced on an equal basis, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the right of the present invention.
Claims (5)
1. the method from medicine Wastewater by Solvent Extraction DMAC N,N' dimethyl acetamide, it is characterised in that: comprise the steps:
(1) acid in alkali Pre process pharmaceutical wastewater, regulates pH to 7-9, and waste liquid, after standing sedimentation and Temperature fall, enters strainer, filters the insoluble solid in waste liquid;
(2) pharmaceutical wastewater processed in step (1) is led to carry out multi-stage countercurrent solvent extraction DMAC N,N' dimethyl acetamide wherein into stirring tower.
2. according to the method described in claim 1, it is characterised in that: in described step (1), regulate pH time, alkali used be sodium hydroxide, potassium hydroxide one or both.
3. according to the method described in claim 1, it is characterised in that: in described step (1), the height of standing sedimentation groove should be 1.5-2.0 times of diameter, and strainer is multilayer cavernous body, and lower end monolithic porous supports, aperture 2-4 millimeter, and percentage of open area is 0.25.
4. according to the method described in claim 1, it is characterized in that: pre-treatment and the extracting and separating of waste liquid complete all at normal temperatures and pressures, extraction agent is methylene dichloride, counter-current extraction progression is 5-8 level, stirring rake arranges number to be not less than theoretical stage, and the volume ratio of methylene dichloride and waste liquid is 1:1-2:1.
5. according to the method described in claim 1, it is characterized in that: the basic structure of the agitating extraction column with transport disengaging height in described step (2) is: the extraction height of tower and diameter proportion are between 4:1 to 6:1, the top of tower is provided with the entrance of heavy constituent extraction agent methylene dichloride and the spout of light constituent raffinate, spout is in the upper end of extraction agent entrance, and the spacing of two mouthfuls is 2-4 tower footpath doubly;The lower end of tower is provided with the entrance of waste water and the outlet of heavy constituent extraction phase, heavy constituent spout is located at the lower end of waste liquid, the spacing of two mouthfuls is still 2-4 tower footpath doubly, upper and lower admission port is 0.5-1 tower footpath doubly apart from the distance of the top with stirring rake bottom, and the distance between stirring rake is 1-2 beta footpath.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510922637.0A CN105645501A (en) | 2015-12-14 | 2015-12-14 | Method for recovering N,N-dimethyl acetamide from pharmaceutical wastewater |
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| CN201510922637.0A CN105645501A (en) | 2015-12-14 | 2015-12-14 | Method for recovering N,N-dimethyl acetamide from pharmaceutical wastewater |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110078285A (en) * | 2019-05-08 | 2019-08-02 | 徐州工程学院 | A kind of Urethane Elastic Fibre Industrial Wastewater efficient treatment process |
| CN110776041A (en) * | 2019-11-22 | 2020-02-11 | 武汉格林环源净化工程有限公司 | Pretreatment method of high-concentration medical intermediate wastewater |
| CN112513007A (en) * | 2020-10-23 | 2021-03-16 | 安徽金禾实业股份有限公司 | DMF (dimethyl formamide) recovery method |
| CN112574060A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide |
| CN114436359A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Method for extracting and recovering N, N-dimethylacetamide in wastewater |
| CN114436883A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide from multi-component solution system |
| CN114604928A (en) * | 2022-03-22 | 2022-06-10 | 北京安胜瑞力科技有限公司 | Recycling treatment process of industrial wastewater containing DMAC (dimethylacetamide) |
| CN115093041A (en) * | 2022-02-22 | 2022-09-23 | 邓国文 | Recycling treatment method for industrial wastewater generated by producing 5-amino-2-nitrobenzotrifluoride |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110078285A (en) * | 2019-05-08 | 2019-08-02 | 徐州工程学院 | A kind of Urethane Elastic Fibre Industrial Wastewater efficient treatment process |
| CN112574060A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide |
| CN112574060B (en) * | 2019-09-29 | 2022-10-11 | 中国石油化工股份有限公司 | Recovery method of N, N-dimethylacetamide |
| CN110776041A (en) * | 2019-11-22 | 2020-02-11 | 武汉格林环源净化工程有限公司 | Pretreatment method of high-concentration medical intermediate wastewater |
| CN114436359A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Method for extracting and recovering N, N-dimethylacetamide in wastewater |
| CN114436883A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide from multi-component solution system |
| CN114436359B (en) * | 2020-10-19 | 2023-05-02 | 中国石油化工股份有限公司 | Method for extracting and recovering N, N-dimethylacetamide in wastewater |
| CN112513007A (en) * | 2020-10-23 | 2021-03-16 | 安徽金禾实业股份有限公司 | DMF (dimethyl formamide) recovery method |
| CN112513007B (en) * | 2020-10-23 | 2022-01-21 | 安徽金禾实业股份有限公司 | DMF (dimethyl formamide) recovery method |
| CN115093041A (en) * | 2022-02-22 | 2022-09-23 | 邓国文 | Recycling treatment method for industrial wastewater generated by producing 5-amino-2-nitrobenzotrifluoride |
| CN115093041B (en) * | 2022-02-22 | 2024-02-13 | 杨自林 | Recycling treatment method of industrial wastewater generated in production of 5-amino-2-nitrobenzotrifluoride |
| CN114604928A (en) * | 2022-03-22 | 2022-06-10 | 北京安胜瑞力科技有限公司 | Recycling treatment process of industrial wastewater containing DMAC (dimethylacetamide) |
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Application publication date: 20160608 |