CN102766006A - Method and device for recycling organic mixed waste liquor - Google Patents
Method and device for recycling organic mixed waste liquor Download PDFInfo
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- CN102766006A CN102766006A CN2012102836875A CN201210283687A CN102766006A CN 102766006 A CN102766006 A CN 102766006A CN 2012102836875 A CN2012102836875 A CN 2012102836875A CN 201210283687 A CN201210283687 A CN 201210283687A CN 102766006 A CN102766006 A CN 102766006A
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Abstract
The invention discloses a method and a device for recycling organic mixed waste liquor. The method includes: measuring composition proportion of the waste liquor to be treated, adding the waste liquor into an extraction barrel to be extracted and separated, stirring the waste liquor and extracting agents in the extraction barrel, leading liquid to be in standing until the liquid in the extraction barrel shows obvious two-phase layering, and then performing extracting again; drying phase raffinate through a drier, adopting a rotating evaporimeter to perform decompressing temperature-control distilling to obtain recovery agent A, and split charging the recovery agent A into a reagent bottle A; separating and recovering collected extraction phase liquid through a rectifying column to obtain solvent B, and split charging the solvent B into a reagent bottle B; and discharging separated waste water after adsorption in harmless mode. Organic solvent in the organic mixed waste liquor is separated and purified so as to be reused, and therefore recycling is achieved, content of organic solvent in the organic mixed waste liquor is reduced, and after-treatment difficulty of waste water is reduced.
Description
Technical field
The present invention relates to field of waste water treatment, especially a kind of organic mixed waste liquor recycle method and device.
Background technology
Natural product is meant the moity of animal, plant, insect, sea life and mikrobe or the chemical ingredients of its meta-bolites, mainly comprises the composition of biologically actives such as protein, polypeptide, amino acid, nucleic acid, volatile oil, vegeto-alkali, flavones, glucosides class, terpene, the plain class of phenylpropyl alcohol, quinones, steroidal compounds, antibiotics.The extract of natural product is used for satisfying human material requisite, and its product relates to all trades and professions, and wherein key areas is and human diseases and healthy relevant medicine, natural health-care products, cosmeceutical.
All the time, the natural product usage quantity of medicine but along with the reinforcement of Chinese national economy and health care consciousness, increases with the be healthy and strong research and development of related prods of efficiency health-care, beauty treatment in the highest flight year by year.In the research and development process of natural product resource, the extraction separation of efficient part and effective constituent uses a large amount of organic reagents, and these reagent adopt binary mixture usually, like chloroform-methanol, sherwood oil-acetone, petroleum ether-ethyl acetate, methanol-water etc.Because reclaiming the back waste liquid is organic mixed system of unknown ratio, is difficult to reuse in R&D process.For this reason, we carry out blank survey.Observation unit relates to chemical engineering institute, pharmaceutical college, the school of life and health sciences of colleges and universities, and medicinal plants institute, the research and development institution of pharmacy corporation, Health Products Enterprises, makeup enterprise.The survey showed that, after the disposable use organic reagent of most of research unit, all abandons and regularly transported by the waste liquid recycle bin.Every year, the organic reagent use cost expense of colleges and universities, experimental teaching is 4～60,000 yuan, research and development are 10～200,000 yuan; Corporate center is 20～300,000; Institute's usage quantity is the highest, like the annual organic reagent cost of use nearly 1,000,000 of Chinese Academy of Sciences's plant research.So a large amount of organic reagent running cost is expensive, and the waste liquid of generation has certain toxicity, and aftertreatment is difficult, can cause serious environmental to pollute and the wasting of resources in case deal with improperly.
In consulting domestic and foreign literature, find, for organic liquid waste, most of bibliographical informations the heavily steaming processing or the rectification process of single waste liquid; The part document has been reported submethod and the little tricks of the trade that handle in the laboratory to binary system, does not make Depth Study.The part document proposes the methodological study of discharging to organic waste water and waste gas.In addition, the part document calculates and simulates a certain concrete parameter in the technology, does not report all in the document that the circular treatment integrated device carries out effectively controlled organic mixed waste liquor.
Summary of the invention
The objective of the invention is: a kind of organic mixed waste liquor recycle method and device are provided; It can carry out separation and purification with the organic mixed waste liquor that extracts natural product; To need can obtain the pure organic solvent of utilization; Can effectively waste water be carried out harmless treatment again, reduce the post-processing difficulty of waste water, to overcome the deficiency of prior art.
The present invention is achieved in that organic mixed waste liquor recycle method, measures the proportion of composing of pending waste liquid earlier, after mensuration is accomplished; With waste liquid add in the extraction bucket and carry out extracting and separating, and add corresponding extraction agent, waste liquid and extraction agent are stirred in extraction barrel; Make its thorough mixing; Tangible two phase stratification appears in the liquid that leaves standstill to the extraction bucket, carries out extracting operation again, and measures the effect of extracting and separating; Extracting phase liquid after the moisture eliminator drying, is adopted the Rotary Evaporators temperature control distillation of reducing pressure, can accelerate evaporation process, improve separating effect, obtain to reclaim reagent A, detect the purity that reclaims reagent A after, will reclaim the reagent A branch and be filled among the reagent bottle A; Extraction phase liquid with collection obtains carries out Separation and Recovery through rectifying volumn, and the cut of gained behind cooling drying, is obtained solvent B, detect the purity of solvent B after, solvent B divided be filled to reagent bottle
BIn; The waste water separated in the rectifying through innoxious discharging after the adsorption treatment, and is carried out quality examination to discharge water.
Selection of Extractant is done conventional the selection according to organic composition concrete in the waste liquid.
The waste liquid that adds in the extraction bucket is extraction bucket volumetrical 1/3.After adding extraction agent, can guarantee also have enough spaces in the extraction bucket, guarantee carrying out smoothly of stirring.
Described extraction behaviour specifically is meant, lower floor's extracting phase liquid and upper strata extraction phase liquid are sent into respectively in two different storage barrels, and extracting phase liquid is sent in the extraction bucket again for the first time, carries out the extraction second time; Repeat above-mentioned steps, meet the demands until the extracting and separating effect of measuring.
In the exit of waste liquid bucket, the ingress of the ingress of the ingress of the exit of extraction bucket, reagent bottle A, reagent bottle B and activated charcoal filter is equipped with the measuring method employing index determination or the absorbance measurement of analyzing and testing point.In above measuring method: the detection of midbody can be adopted chemistry or physical detection, like spectra photometric method or refractive index method; The detection of the finished product then can adopt national standard GC/HPLC method to detect.
Organic mixed waste liquor integrative machine comprises the waste liquid bucket, and the waste liquid bucket is connected with the extraction bucket, on the extraction bucket, is connected with storage barrel I and storage barrel II, and storage barrel I is connected with Rotary Evaporators, and Rotary Evaporators is connected with reagent bottle A; Storage barrel II is connected with rectifying volumn and activated charcoal filter respectively, and the top of rectifying volumn is connected with reagent bottle B through condensing surface and solids dryer, and the bottom of rectifying volumn is connected with activated charcoal filter; Be equipped with the analyzing and testing device in the exit of waste liquid bucket, exit, the ingress of reagent bottle A, the ingress of reagent bottle B and the ingress of activated charcoal filter of extraction bucket.
Rotary Evaporators is connected with the constant temperature water cooler with the cooling segment of rectifying volumn.Through the constant temperature water cooler quench liquid of using in evaporimeter and the rectifying volumn is carried out refrigeration cycle.
Owing to adopt above-mentioned technical scheme; Compared with prior art; The present invention adopts the abstraction technique of binary or multicomponent system; Jointly organic mixed waste liquor is separated through Technologies such as extraction, rectifying, fractionation and dryings, and on each key point, be provided with the monitoring point, raw material, effect of extracting, the finished product, discharge of wastewater are detected; Can the organic solvent in organic mixed waste liquor be separated and purifies like this; For recycling; So not only realize recycling, and reduced the content of the organic solvent in organic mixed waste liquor, reduced the post-processing difficulty of waste water; The environmental protection concept that meets energy-saving and emission-reduction, recycling economy has tangible economic benefit and social effect; The inventive method is simple, and the apparatus structure that is adopted is simple, and is with low cost, and result of use is good.
Description of drawings
Accompanying drawing 1 is a structural representation of the present invention.
Embodiment
Embodiments of the invention: organic mixed waste liquor recycle method, the proportion of composing of the pending waste liquid of mensuration is measured and is learnt that pending waste liquid is the chloroform-methanol binary mixed solvent earlier; With waste liquid add in the extraction bucket, add-on is an extraction bucket volumetrical 1/3, and adds the equal-volume deionized water as extraction agent; Perform fighting and extract the stirring switch of bucket; Waste liquid and extraction agent are stirred in extraction is disclosed, make its thorough mixing, tangible two phase stratification appears in the liquid that leaves standstill in back to the extraction bucket; Lower floor's extracting phase liquid is sent among the storage barrel I; Upper strata aqueous phase extracted liquid is sent among the storage barrel II, and extracting phase liquid is sent in the extraction bucket again for the first time again, adds isopyknic deionized water again and carries out the extraction second time; Measure separating effect; The result proves that after twice washing, methyl alcohol is removed basically in the chloroform; With extracting phase liquid after the moisture eliminator drying; Adopt the Rotary Evaporators temperature control distillation (adopted Rotary Evaporators quickening evaporation process, improve separating effect) of reducing pressure, obtain pure chloroform reagent; After detecting the purity of pure chloroform reagent, pure chloroform reagent branch is filled among the reagent bottle A; The aqueous phase extracted liquid that collection obtains is the methanol-water binary system; With the methanol-water binary system, carry out Separation and Recovery through rectifying volumn, because methanol-water is difficult for forming azeotrope; Through rectifying volumn with the cut of gained behind cooling drying; Can get anhydrous pure methanol solvate, detect the purity of anhydrous pure methanol solvate after, anhydrous pure methanol solvate branch is filled to reagent bottle
BIn; The waste water of separating in the rectifying is carried out innoxious discharging after the adsorption treatment with active carbon adsorber, and discharge water is carried out quality examination.
The structure of organic mixed waste liquor integrative machine is as shown in Figure 1; Comprise waste liquid bucket 1, waste liquid bucket 1 is connected with extraction bucket 2, on extraction bucket 2, is connected with storage barrel I3-1 and storage barrel II3-2; Storage barrel I3-1 is connected with Rotary Evaporators 4, and Rotary Evaporators 4 is connected with reagent bottle A10-1; Storage barrel II3-2 is connected with rectifying volumn 5 and activated charcoal filter 9 respectively, and the top of rectifying volumn 5 is connected with reagent bottle B10-2 through condensing surface 6 and solids dryer 8, and the bottom of rectifying volumn 5 is connected with activated charcoal filter 9; Rotary Evaporators 4 is connected with constant temperature water cooler 7 with the cooling segment of rectifying volumn 5; Be equipped with analyzing and testing device 11 in the exit of waste liquid bucket 1, exit, the ingress of reagent bottle A10-1, the ingress of reagent bottle B10-2 and the ingress of activated charcoal filter 9 of extraction bucket 2.
Claims (6)
1. an organic mixed waste liquor recycle method is characterized in that: measure the proportion of composing of pending waste liquid earlier, after mensuration is accomplished; Waste liquid added in the extraction bucket carry out extracting and separating, and add corresponding extraction agent, waste liquid and extraction agent are stirred in extraction barrel; Make its thorough mixing; Tangible two phase stratification appears in the liquid that leaves standstill to the extraction bucket, carries out extracting operation again, and measures the effect of extracting and separating; Extracting phase liquid after the moisture eliminator drying, is adopted the Rotary Evaporators temperature control distillation of reducing pressure, obtains to reclaim reagent A, detect the purity that reclaims reagent A after, will reclaim the reagent A branch and be filled among the reagent bottle A; Extraction phase liquid with collection obtains carries out Separation and Recovery through rectifying volumn, and the cut of gained behind cooling drying, is obtained solvent B, detect the purity of solvent B after, solvent B divided be filled to reagent bottle
BIn; The waste water separated in the rectifying through innoxious discharging after the adsorption treatment, and is carried out quality examination to discharge water.
2. organic mixed waste liquor recycle method according to claim 1 is characterized in that: the waste liquid that adds in the extraction bucket is extraction bucket volumetrical 1/3.
3. organic mixed waste liquor recycle method according to claim 1; It is characterized in that: described extraction behaviour specifically is meant; Lower floor's extracting phase liquid and upper strata extraction phase liquid are sent into respectively in two different storage barrels; Extracting phase liquid is sent in the extraction bucket again for the first time, carries out the extraction second time; Repeat above-mentioned steps, meet the demands until the extracting and separating effect of measuring.
4. organic mixed waste liquor recycle method according to claim 1, it is characterized in that: above-mentioned measuring method is index determination or absorbance measurement.
5. organic mixed waste liquor integrative machine; Comprise waste liquid bucket (1); It is characterized in that: waste liquid bucket (1) is connected with extraction bucket (2); On extraction bucket (2), be connected with storage barrel I (3-1) and storage barrel II (3-2), storage barrel I (3-1) is connected with Rotary Evaporators (4), and Rotary Evaporators (4) is connected with reagent bottle A (10-1); Storage barrel II (3-2) is connected with rectifying volumn (5) and activated charcoal filter (9) respectively; The top of rectifying volumn (5) is connected with reagent bottle B (10-2) through condensing surface (6) and solids dryer (8), and the bottom of rectifying volumn (5) is connected with activated charcoal filter (9); Be equipped with analyzing and testing device (11) in the exit of waste liquid bucket (1), exit, the ingress of reagent bottle A (10-1), the ingress of reagent bottle B (10-2) and the ingress of activated charcoal filter (9) of extraction bucket (2).
6. organic mixed waste liquor integrative machine according to claim 5 is characterized in that: Rotary Evaporators (4) is connected with constant temperature water cooler (7) with the cooling segment of rectifying volumn (5).
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| CN2012102836875A CN102766006A (en) | 2012-08-10 | 2012-08-10 | Method and device for recycling organic mixed waste liquor |
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| CN2012102836875A CN102766006A (en) | 2012-08-10 | 2012-08-10 | Method and device for recycling organic mixed waste liquor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109133023A (en) * | 2017-06-27 | 2019-01-04 | 天津金牛电源材料有限责任公司 | The circulation utilization method of nonaqueous solvents in a kind of difluorophosphate preparation process |
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| CN1462729A (en) * | 2003-06-19 | 2003-12-24 | 上海交通大学 | Treatment process for two stage recycling alkali waste liquid drained off by process system of synthesizing octanol |
| JP2008266181A (en) * | 2007-04-19 | 2008-11-06 | Toray Ind Inc | Method for recovering hydrophobic organic solvent and method for producing polyarylene sulfide |
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2012
- 2012-08-10 CN CN2012102836875A patent/CN102766006A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462729A (en) * | 2003-06-19 | 2003-12-24 | 上海交通大学 | Treatment process for two stage recycling alkali waste liquid drained off by process system of synthesizing octanol |
| JP2008266181A (en) * | 2007-04-19 | 2008-11-06 | Toray Ind Inc | Method for recovering hydrophobic organic solvent and method for producing polyarylene sulfide |
Non-Patent Citations (3)
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| 杨会玲: "实验室乙醇-环己烷废液的回收与利用", 《化学工程师》 * |
| 杨成德等: "《化工单元操作与控制》", 30 September 2010, 化学工业出版社 * |
| 陈丽萍等: "实验室异丙醇-环己烷废液回收的研究", 《实验室研究与探索》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109133023A (en) * | 2017-06-27 | 2019-01-04 | 天津金牛电源材料有限责任公司 | The circulation utilization method of nonaqueous solvents in a kind of difluorophosphate preparation process |
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Application publication date: 20121107 |