CN101186347A - Method for reclaiming low boiling point organic solvent from waste water - Google Patents
Method for reclaiming low boiling point organic solvent from waste water Download PDFInfo
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- CN101186347A CN101186347A CNA2007101150222A CN200710115022A CN101186347A CN 101186347 A CN101186347 A CN 101186347A CN A2007101150222 A CNA2007101150222 A CN A2007101150222A CN 200710115022 A CN200710115022 A CN 200710115022A CN 101186347 A CN101186347 A CN 101186347A
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Abstract
The invention relates to a method of recycling low boiling organic solvent from factory effluent in the wastewater treatment field. A flash evaporation method is adopted under a pressure-reducing condition for recycling low boiling organic solvent and a flash evaporation operation temperature is 0 to 100 DEG C. The method comprises steps that: the waste water which comprises the low boiling organic solvent enters a flash evaporation pot from bottom part to carry out pressure-reducing flash evaporation, the evaporated organic solvent steam is transported to a condenser from the top part, and the organic solvent is converted to liquid and sent to a receiving tank; negative pressure conditions are realized by respectively connecting a vacuum pumping system and a vacuum line to the flash evaporation pot, the condenser and the receiving tank. The invention has the advantages of less devices investment, simple and practical operation technique, high recycling efficiency, achieving the requirements of low emission and low pollution. A first time recycling rate of low boiling organic solvent is 85 to 95 percent, and the invention is especially applicable to the recycling of organic solvents of tetrahydrofuran, 2-tetrahydrofurfuryl, etc. which are mutual soluble with water, difficult to degrade, comparatively high in price and comparatively large in recycling value.
Description
Technical field:
The present invention relates to a kind of method that from factory effluent, reclaims low boiling point organic solvent in the water treatment field.
Technical background:
Have several different methods to be used for reclaiming the organic solvent of factory effluent at present, as utilizing the method for absorption, promptly use the organism in the activated carbon adsorption water, this method can only be applied under the situation of lower concentration, and adsorbed organic matter is difficult to utilize again.Be exactly atmospheric distillation in addition, promptly the waste water that contains low boiling point organic solvent heated, organism is evaporated and carries out conventional rectification, this method investment is big, energy consumption is high, is difficult to economically bear.Other also have extraction and distillation technology, similar with atmospheric distillation with salt distillation technology etc., investment is big, energy consumption is high.
In the Chemical Manufacture under above-mentioned technical qualification, often run into that low boiling point organic solvent enters in the waste water and effective (or low-cost) situation about reclaiming.For example: do with methyl alcohol or ethanol under the situation of solvent, in case methyl alcohol or ethanol enter in the waste water, the liquid because methyl alcohol or ethanol and water dissolve each other is difficult to reclaim methyl alcohol or ethanol with existing method.For another example: producing methyl cyclopentyl-dialkyl-tricarbon manganium (being called for short MMT) and producing in cyclopentadiene tricarbonyl manganese (the being called for short CMT) process, be with tetrahydrofuran (THF) (being called for short THF) as solvent.Although all will reclaim to tetrahydrofuran solvent in each production cycle, so that reuse, but always some THF will lose, major cause is tetrahydrofuran (THF) all can't be steamed (if at this moment steam too driedly in the technology that reclaims tetrahydrofuran (THF), to influence product yield), enter next process thereby some tetrahydrofuran (THF) is inevitable with product, that is: water vapor stripping operation.At the steam stripped initial stage of water vapor, this a part of tetrahydrofuran (THF) is a large amount of is taken out of by water vapor and flows into sewer line enter sewage network after condensation.Cause the waste of tetrahydrofuran (THF) like this, increase production cost, and it is bigger to contain the sewage smell of tetrahydrofuran (THF) in the water drain, influence surrounding environment, the concentration and the quantity of pollutent in the increase sewage are brought environmental protection pressure.How this part tetrahydrofuran (THF) of recovery being arranged, cut the waste, protect and improve environment, is problem anxious to be solved.
Summary of the invention:
Purpose of the present invention is exactly the problems that exist at above-mentioned prior art, proposes a kind of mode that adopts vacuum flashing, the method that reclaims low boiling point organic solvent from waste water of less investment, efficient energy-saving.
Technical scheme of the present invention is: adopt the mode of flash distillation to reclaim low boiling point organic solvent under reduced pressure, system operation pressure is not more than a standard atmospheric pressure, and the flash distillation service temperature is 0-100 ℃.
Concrete scheme comprises: the waste water that contains low boiling point organic solvent enters flash tank by the bottom and carries out vacuum flashing, the organic vapor that flashes off enters condenser by top, organic solvent becomes liquid state and enters receiving tank after condensation, pressure is-101.3-0kPa (gauge pressure) in the total system operating process, and the generation of negative pressure state is connected respectively to condenser by pumped vacuum systems and vacuum pipeline and receiving tank is realized.
The flash distillation service temperature is 30 ℃ to 70 ℃.The flash tank inner bottom part is provided with a dividing plate at least, makes waste water keep the certain liquid level and the residence time, and is unlikely to wear intestines and mistake.Usually in flash tank, be provided with heating facility, as heating coil, chuck heating etc.Because Heating temperature is low, heating load is little, can utilize the inferior thermal source in the factory to heat, and as steam condensate etc., improves energy utilization rate.Receiving tank wherein is typically provided with the cold insulation measure.Said low boiling point organic solvent is under a normal atmosphere, its boiling point is lower than 100 ℃ organic solvent, comprising: the mixture of one or more organic solvents of methyl alcohol, ethanol, tetrahydrofuran (THF), 2-methyltetrahydrofuran, methyl ether, ether, methyl tertiary butyl ether, benzene, methyl acetate, ethyl acetate, acetone, butanone, Virahol.Wherein, typical low boiling point organic solvent is tetrahydrofuran (THF) and 2-methyltetrahydrofuran, and these two kinds of solvents and water dissolve each other, and are difficult to degraded, and price is higher, and big recovery value is arranged.
Method of the present invention has the equipment less investment, and operating procedure is simple and practical, and the organic efficiency height reaches low emission and oligosaprobic requirement.The high 85-95% of the disposable rate of recovery of low boiling point organic solvent is particularly suitable for tetrahydrofuran (THF) and this class of 2-methyltetrahydrofuran and water and dissolves each other, and is difficult to degraded, and price is higher, and the Recovery of Organic Solvent utilization of big recovery value is arranged.
Description of drawings
Accompanying drawing is the process flow diagram of a kind of specific embodiment of the present invention.
Embodiment
The present invention is further described with the example of tetrahydrofuran (THF) and 2-methyltetrahydrofuran below, but be not the restriction to range of application of the present invention.
Tetrahydrofuran (THF) is a kind of broad-spectrum organic solvent, molecular formula C
4H
8O, molecular mass 72.11, structural formula is as follows:
This material normal temperature is down colourless transparent liquid, and is inflammable, and the smell of similar ether is arranged, with water and most of immiscible organic solvent, and relative density (20 ℃/℃)=0.8892, boiling point (101.3kPa)=66 ℃, fusing point=-108.5 ℃.Tetrahydrofuran (THF) and water form azeotrope, and content of tetrahydrofuran is about 95% in the azeotrope.
2-methyltetrahydrofuran (being called for short MeTHF) molecular formula C
5H
10O, molecular mass 86.13, structural formula is as follows:
This material normal temperature is down colourless liquid, and the smell of similar ether is arranged, and is soluble in organic solvent, 20 ℃ in water solubleness be 13.1%, relative density (20 ℃/℃)=0.8540, boiling point (101.3kPa)=80.2 ℃, fusing point=-136 ℃.Tetrahydrofuran (THF) and water form azeotrope, 71 ℃ of azeotropic points, and azeotropic consists of: MeTHF 89.4%, moisture content 10.6%.
The volatility of low boiling point organic solvent often greater than the volatility of water, be easier to evaporation than water, and system pressure is low more, and the relative volatility of the two is big more, and separate easily is come out more.As tetrahydrofuran (THF)-aqueous solution, when (101.3kPa) about 65 ℃, the relative volatility of the relative water of tetrahydrofuran (THF) is about 4.5 under the normal pressure, and system pressure is when dropping to 25kPa, and its relative volatility is about 7.0.Therefore, easier under reduced pressure the organic solvent in the waste water is reclaimed.
Based on above-mentioned principle, the concrete grammar of embodiments of the invention 1 is (as shown in Figure 1): the waste water 1 that contains low boiling point organic solvent (tetrahydrofuran (THF) or) enters flash tank 2 by the bottom and carries out vacuum flashing, the organic vapor 3 that flashes off enters condenser 4 by top, organic solvent becomes liquid state after condensation, and gravity flow enters receiving tank 5.Pressure in the total system operating process is-101.3kPa to 0 (gauge pressure) (be that system pressure is lower than external atmospheric pressure, that is to say to have certain vacuum tightness in the system) that the generation of vacuum tightness realizes by vacuum line 6 and pumped vacuum systems 7.The service temperature of flash tank 2 is 30 ℃ to 70 ℃, is provided with a dividing plate 8 in the flash tank, has only when the liquid level of waste water in the jar surpasses the top of dividing plate, just can overflow to outlet 9, thereby makes waste water keep the certain liquid level and the residence time.Flash tank exports 9 back also should connect the low-voltage vacuum system, so that waste water flows out.The heat-eliminating medium of condenser 4 (refrigerant) should be adopted and adopt the low temperature refrigerant as far as possible, as the ethylene glycol cold water below 0 ℃, to improve cooling performance.Receiving tank 5 is typically provided with the cold insulation measure, can adopt measures such as inner spiral coil cooling tube, cooling jacket, cold insulation material, reduces the temperature of the organic solvent of collecting in the receiving tank, reduces the secondary volatilization.
The vacuum flashing method reclaims tetrahydrofuran (THF) experiment representative data
| Raw material waste water | Waste water after the flash distillation | The tetrahydrofuran (THF) that reclaims | |||
| Quantity, kg | 2000 | Quantity, kg | 1830 | Quantity, kg | 150 |
| THF content, % | 8 | THF content, % | Do not detect | THF content, % | 95 |
| Vacuum tightness: about 50kpa evaporation loss: about 15kg (heat-eliminating medium is a tap water, about 15 ℃) | |||||
The rate of recovery of tetrahydrofuran (THF) in this example (THF) is about 89%, and the THF purity of recovery is 95%, and wherein the uncolled volatilization loss of getting off of some THF is fallen, if adopt the more medium cooling of low temperature, effect can be more better.
Embodiment 2: be on the basis of reference embodiment 1, reclaim the 2-methyltetrahydrofuran from the waste water that contains low boiling point organic solvent (2-methyltetrahydrofuran).Difference is: in order to improve flash distillation speed, will contain 2-methyltetrahydrofuran waste water and enter and be heated to 60～70 ℃ (being provided with heating coil in the flash tank) after the flash tank.Other technical process and condition are substantially the same manner as Example 1.
Claims (10)
1. method that reclaims low boiling point organic solvent from waste water, it is characterized in that: adopt the mode of flash distillation to reclaim low boiling point organic solvent under reduced pressure, the flash distillation service temperature is 0-100 ℃.
2. the method that from waste water, reclaims low boiling point organic solvent as claimed in claim 1, it is characterized in that: the waste water that contains low boiling point organic solvent enters flash tank by the bottom and carries out vacuum flashing, the organic vapor that flashes off enters condenser by top, organic solvent becomes liquid state and enters receiving tank after condensation, gauge pressure pressure is-101.3-0kPa in the total system operating process, and the generation of negative pressure state is connected respectively to condenser by pumped vacuum systems and vacuum pipeline and receiving tank is realized.
3. the method that reclaims low boiling point organic solvent from waste water as claimed in claim 2 is characterized in that: be provided with at least one dividing plate in the flash tank wherein.
4. the method that reclaims low boiling point organic solvent from waste water as claimed in claim 3 is characterized in that: be provided with heating facility in the flash tank wherein.
5. the method that reclaims low boiling point organic solvent from waste water as claimed in claim 2, it is characterized in that: receiving tank wherein is provided with the cold insulation device.
6. the method that reclaims low boiling point organic solvent from waste water as claimed in claim 1 or 2, it is characterized in that: the flash distillation service temperature is 30 ℃ to 70 ℃.
7. the method that reclaims low boiling point organic solvent from waste water as claimed in claim 1 or 2, it is characterized in that: said low boiling point organic solvent is that its boiling point is lower than 100 ℃ organic solvent under a normal atmosphere.
8. the method that reclaims low boiling point organic solvent from waste water as claimed in claim 7, it is characterized in that: said low boiling point organic solvent comprises: a kind of in methyl alcohol, ethanol, tetrahydrofuran (THF), 2-methyltetrahydrofuran, methyl ether, ether, methyl tertiary butyl ether, benzene, methyl acetate, ethyl acetate, acetone, butanone, the Virahol or the mixture of several organic solvents wherein.
9. the method that reclaims low boiling point organic solvent from waste water as claimed in claim 8, it is characterized in that: low boiling point organic solvent is a tetrahydrofuran (THF).
10. the method that reclaims low boiling point organic solvent from waste water as claimed in claim 8, it is characterized in that: low boiling point organic solvent is the 2-methyltetrahydrofuran.
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| CNA2007101150222A CN101186347A (en) | 2007-11-22 | 2007-11-22 | Method for reclaiming low boiling point organic solvent from waste water |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456640B (en) * | 2008-12-30 | 2010-12-01 | 洛阳尚德太阳能电力有限公司 | Processing method of crystalline silicon texture etch wastewater and system for the same |
| CN102374698A (en) * | 2011-11-29 | 2012-03-14 | 林绍风 | Refrigerating system being opening-type refrigerating and heating device |
| CN102925983A (en) * | 2012-11-02 | 2013-02-13 | 洛阳尚德太阳能电力有限公司 | Recovering device and method for monocrystalline silicon piece frocking liquid |
| CN103553260A (en) * | 2013-11-22 | 2014-02-05 | 焦伟祥 | Synergic extraction and negative-pressure flash evaporation dephenolizing method of high-concentration semi-coke phenolic wastewater |
| CN104600302A (en) * | 2015-01-27 | 2015-05-06 | 江苏华东锂电技术研究院有限公司 | Hot preparation technology of lithium iron phosphate solvent |
| CN105130779A (en) * | 2015-08-06 | 2015-12-09 | 曹宇锋 | Apparatus and method for separating butanone, ethyl acetate and isopropyl alcohol aqueous solution |
| CN105293801A (en) * | 2015-10-28 | 2016-02-03 | 宁波大学 | Method for removing acetaldehyde in starch sugar evaporated condensate water |
| CN107617227A (en) * | 2017-10-30 | 2018-01-23 | 广西万山香料有限责任公司 | The process units of trans-anethole rectifying section |
| CN109399742A (en) * | 2018-12-14 | 2019-03-01 | 重庆工商大学 | A method of antibiotic waste water toxicity is reduced by flash distillation |
| CN112012903A (en) * | 2020-07-15 | 2020-12-01 | 国环危险废物处置工程技术(天津)有限公司 | Pumping transfer method of low-boiling-point solvent |
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2007
- 2007-11-22 CN CNA2007101150222A patent/CN101186347A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456640B (en) * | 2008-12-30 | 2010-12-01 | 洛阳尚德太阳能电力有限公司 | Processing method of crystalline silicon texture etch wastewater and system for the same |
| CN102374698A (en) * | 2011-11-29 | 2012-03-14 | 林绍风 | Refrigerating system being opening-type refrigerating and heating device |
| CN102374698B (en) * | 2011-11-29 | 2013-07-10 | 林绍风 | Refrigerating and heating device with refrigerating system being opening-type |
| CN102925983A (en) * | 2012-11-02 | 2013-02-13 | 洛阳尚德太阳能电力有限公司 | Recovering device and method for monocrystalline silicon piece frocking liquid |
| CN103553260A (en) * | 2013-11-22 | 2014-02-05 | 焦伟祥 | Synergic extraction and negative-pressure flash evaporation dephenolizing method of high-concentration semi-coke phenolic wastewater |
| CN104600302A (en) * | 2015-01-27 | 2015-05-06 | 江苏华东锂电技术研究院有限公司 | Hot preparation technology of lithium iron phosphate solvent |
| CN105130779A (en) * | 2015-08-06 | 2015-12-09 | 曹宇锋 | Apparatus and method for separating butanone, ethyl acetate and isopropyl alcohol aqueous solution |
| CN105130779B (en) * | 2015-08-06 | 2017-12-05 | 南通大学 | A kind of device and method for separating butanone, ethyl acetate and isopropanol water solution |
| CN105293801A (en) * | 2015-10-28 | 2016-02-03 | 宁波大学 | Method for removing acetaldehyde in starch sugar evaporated condensate water |
| CN107617227A (en) * | 2017-10-30 | 2018-01-23 | 广西万山香料有限责任公司 | The process units of trans-anethole rectifying section |
| CN107617227B (en) * | 2017-10-30 | 2023-12-15 | 广西玉蓝生物科技有限公司 | Production device of anethole rectifying section |
| CN109399742A (en) * | 2018-12-14 | 2019-03-01 | 重庆工商大学 | A method of antibiotic waste water toxicity is reduced by flash distillation |
| CN109399742B (en) * | 2018-12-14 | 2021-07-23 | 重庆工商大学 | Method for reducing toxicity of antibiotic wastewater through flash evaporation |
| CN112012903A (en) * | 2020-07-15 | 2020-12-01 | 国环危险废物处置工程技术(天津)有限公司 | Pumping transfer method of low-boiling-point solvent |
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Open date: 20080528 |