CN205223068U - System for retrieve dimethyl sulfoxide , ethanolamine among useless organic solvent of follow - Google Patents

System for retrieve dimethyl sulfoxide , ethanolamine among useless organic solvent of follow Download PDF

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CN205223068U
CN205223068U CN201520538076.XU CN201520538076U CN205223068U CN 205223068 U CN205223068 U CN 205223068U CN 201520538076 U CN201520538076 U CN 201520538076U CN 205223068 U CN205223068 U CN 205223068U
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feed
static mixer
opening
condenser
extraction
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韦立宁
王治军
吴晓冬
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Huizhou TCL Environment Technology Co Ltd
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Huizhou TCL Environment Technology Co Ltd
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Abstract

The utility model discloses a system for retrieve dimethyl sulfoxide, ethanolamine among useless organic solvent of follow, include: contain the preprocessing device of equipment such as filter, preliminary treatment evaporimeter, first condenser, middle holding vessel, contain the anti - extraction device of extraction of equipment such as extractant storage tank, a static mixer, extraction reaction jar, the 2nd static mixer, stripping agent storage tank, anti - extraction reaction jar, contain the rectification refining plant of equipment such as first rectifying column, second condenser, a solvent reception pot, second rectifying column, third condenser, the 2nd solvent reception pot, among entire system preprocessing device, extract between anti - extraction device, rectification refining plant each equipment according to the technological requirement of handling, manage say wait carry on in proper order the equipment room connect with the circulation. The utility model discloses the unitary construction is simple, and degree of automation is high, and the flexible operation can handle coming from useless organic solvent not of the same trade, regeneration high -purity DMSO, MEA solvent.

Description

A kind of system reclaiming dimethyl sulfoxide (DMSO), thanomin from spent organic solvent
Technical field
The utility model relates to spent organic solvent recovery and reusing and recycling technical field, is specifically related to a kind of system of reclaiming high purity dimethyl sulfoxide (DMSO), thanomin (MEA) from spent organic solvent.
Background technology
Dimethyl sulfoxide (DMSO) (DMSO) is as the Typical Representative of non-proton multipolarity class organic solvent, it is the extremely strong menstruum universale of inertia, normal and alkanol amine organic solvent thanomin (MEA) carries out formulated in combination by a certain percentage, forms the mixed solvent that stripping liquid etc. possesses special purpose.DMSO-MEA type stripping liquid is applied to the stripping technology process of liquid crystal panel assembly in electronic industry, integrated circuit usually, by stripping liquid, the photoresist material being covered in design configuration surface on substrate after etching technics process is carried out stripping and removes.In technological process, DMSO-MEA type stripping liquid can be mixed into non-volatility, lower boiling and the high-boiling-point impurity compositions such as moisture, heavy metal, photoresist material, particulate, along with time lapse, the increase of foreign matter content, peeling effect declines, form inferior product probability to rise, need stripping liquid replacing be carried out, form useless stripping liquid thus.Meanwhile, DMSO, MEA are in industry also widespread uses such as medicine synthesis, fibrous woven, and technological process, owing to being mixed into impurity, also can form the main solvent slop containing DMSO or MEA or DMSO-MEA.
In recent years, electronic manufacture, medicine synthesis, fibrous woven high speed development, all kinds of organic solvent demand such as DMSO, MEA relating to use increases day by day, especially at electronics manufacturing, the sharp increase of liquid crystal display output, DMSO-MEA type stripper usage quantity also significantly increases, and useless stripping liquid generation also increases severely thereupon.DMSO, MEA specification of domestic electron trade production and application is substantially all electronic-grade, and very major part depends on external import.And Present Domestic can carry out producer that the solvent slop containing DMSO or MEA or DMSO-MEA circulates online still in minority, high-quality, the caning be counted on one's fingers especially of high-recovery online recycling can be reached.Form the solvent slop containing DMSO or MEA or DMSO-MEA in every profession and trade, part is still directly to process in burning mode, causes the pollution of environment and the waste of resource to a great extent.
The processing mode of the current spent organic solvent containing DMSO, MEA composition mainly contains: directly burning method, membrane sepn absorption method, rectifying condensation method of reproduction etc.Adopt the process of direct burning mode, do not meet the theory of resource circulation utilization, and easily cause secondary pollution, be progressively eliminated; Patent CN1421398A adopts membrane sepn absorption method, utilize isolated molecule amount be 100 ~ 1500 membranous system, the resist stripper that electron trade given up is separated into containing permeate and concentrated solution, though it is high to reclaim stripping liquid quality, but still novel solvent allotment stripping liquid concentration need be filled into according to stripping technology, the overall rate of recovery is on the low side, and separatory membrane is difficult to tackle impurity composition complicated and changeable, easy blocking damages, and cost of investment is higher; Patent CN102219272B and CN101424889B adopts rectifying-condensation method of reproduction, utilize rectification under vacuum, Cryogenic condensation system, removing electron trade to be given up in stripping liquid stripping liquid for regenerating after light constituent and heavy constituent, but because DMSO and MEA boiling point is substantially identical, regenerated liquid is mixed solution, be difficult to ensure quality, again the allotment of new liquid need be filled into, and this technique can only be back to, and DMSO or MEA cannot be made to be applied to separately other industry or the technique such as electronic manufacture, petrochemical complex, medicine synthesis, fibrous woven, synthetic resins.In addition, what above-mentioned publication (CN1421398A, CN102219272B, CN101424889B) provided has some limitations containing DMSO-MEA solvent slop reclaiming device, be used only in the useless stripping liquid that electronic manufacturing industry produces, all do not relate to the reclaiming containing DMSO, MEA solvent slop that other industry is originated.
Utility model content
For foregoing, the utility model provides the system of a kind of reclaiming high purity DMSO, MEA from spent organic solvent, realizes the high purity containing DMSO, MEA spent organic solvent in conglomerate source, high-recovery regeneration.
The technical solution of the utility model is as follows: one reclaiming high purity DMSO from spent organic solvent, the system of MEA, comprise: containing strainer, pretreatment steaming hair device, first condenser, the pretreatment unit of the equipment such as relay storage tank, containing extraction agent storage tank, first static mixer, extractive reaction tank, second static mixer, strippant storage tank, the Extraction and back extraction device of the equipment such as reextraction retort, containing the first rectifying tower, second condenser, first solvent receiving tank, Second distillation column, 3rd condenser, the rectified purified device of the equipment such as the second solvent receiving tank.In whole system, between pretreatment unit, Extraction and back extraction device, rectified purified device, each equipment, according to the processing requirement of process, carries out equipment room successively through pipeline etc. and connects and circulation.
Described pretreatment steaming hair device is preferably luwa evaporator, and top liquid phase feeding mouth is connected with strainer, and bottom is provided with the heavy constituent discharge outlets such as photoresist material, and top gas phase outlet is connected to the import of relay storage tank through the first condenser; The waste liquid import of described first static mixer, extraction agent import export with relay storage tank discharge port and extraction agent hold-up vessel respectively and are connected, and discharge port is then connected to extractive reaction tank opening for feed; Another opening for feed of described extractive reaction tank exports with extraction agent hold-up vessel and is connected, and discharge port is connected with the first rectifying tower opening for feed and the second static mixer waste liquid import respectively; The reverse-extraction agent import of described second static mixer is connected with strippant outlet, and discharge port is then connected with reextraction retort opening for feed; Another opening for feed of described reextraction retort exports with reverse-extraction agent hold-up vessel and is connected, and discharge port is connected with Second distillation column opening for feed and the first static mixer extraction agent import respectively; Described first rectifying tower opening for feed also exports with relay storage tank and is connected, and top gaseous phase outlet is connected to the first solvent receiving tank opening for feed through the second condenser, and bottom liquid phases discharge port is then connected with pretreatment steaming hair device opening for feed and Second distillation column opening for feed respectively; Described Second distillation column top gas phase discharge port is connected to the reverse-extraction agent import of the second solvent receiving tank opening for feed and the second static mixer respectively through condenser, bottom liquid phases discharge port is connected with pretreatment steaming hair device opening for feed and circulates;
Described spent organic solvent can be the useless stripping liquid of the industries such as the electronic manufacture simultaneously containing DMSO, MEA, or the main useless sanitising agent containing the industries such as the fibrous woven of MEA, or the solvent slop etc. of the main materials synthesis industry containing DMSO;
Described extractive reaction tank, reextraction retort all assemble remote controlled differential pressure transmitter formula automatic liquid separation device;
Described first condenser condenses medium adopts freezing aqueous glycol solution, and the second condenser and the 3rd condenser condenses medium adopt refrigerated water;
Described first rectifying tower and Second distillation column inside adopt Stainless Steel Wire corrugated wire gauze packing 700Y;
System of the present utility model has following advantage:
1. one-piece construction is simple, structure rationally, level of automation is high, can process derive from multiple industry containing DMSO, MEA spent organic solvent, and according to waste liquid composition and actual product conditions of demand, flexible transformation extraction, reextraction and distillation operation, reclaiming high purity DMSO, MEA component, cycle applications is in industries such as electronic manufacture, medicine synthesis, fibrous woven;
2. carry out solid particle polluter and heavy constituent process early stage, can effectively avoid specific examples of such components to decompose in deuterogenesis's temperature-sensitive, tie carbon, damage the situations such as filler;
3. extraction agent and strippant can be recycled, and running cost is lower.
Accompanying drawing explanation
Below in conjunction with accompanying drawing and preferred embodiment, realization, feature etc. to the utility model object further illustrate.
Fig. 1 is the schematic diagram of spent organic solvent reclaiming system of the present utility model.
Embodiment
As shown in the figure, one reclaiming high purity DMSO from spent organic solvent, the system of MEA or DMSO-MEA mixed solution, comprise: containing strainer 1, pretreatment steaming hair device 2, first condenser 3, the pretreatment unit of equipment such as relay storage tank 4 grade, containing extraction agent storage tank 5, first static mixer 6, extractive reaction tank 7, second static mixer 10, strippant storage tank 12, the Extraction and back extraction device of equipment such as reextraction retort 13 grade, containing the first rectifying tower 8, second condenser 9, first solvent receiving tank 10, Second distillation column 14, 3rd condenser 15, the rectified purified device of the second equipment such as solvent receiving tank 16 grade.
Described pretreatment steaming hair device 2 is preferably luwa evaporator, and top liquid phase feeding mouth is connected with strainer 1, and bottom is provided with the heavy constituent discharge outlets such as photoresist material, and top gas phase outlet is connected to relay storage tank 4 import through the first condenser 3; The waste liquid import of described first static mixer 6, extraction agent import export with relay storage tank 4 and extraction agent hold-up vessel 5 respectively and are connected, and discharge port is then connected to extractive reaction tank 7 opening for feed; Another opening for feed of described extractive reaction tank 7 exports with extraction agent hold-up vessel 5 and is connected, and discharge port is connected with the first rectifying tower 8 opening for feed and the second static mixer 11 waste liquid import respectively; The reverse-extraction agent import of described second static mixer 11 exports with strippant storage tank 12 and is connected, and discharge port is then connected with reextraction retort 13 opening for feed; Another opening for feed of described reextraction retort 13 exports with reverse-extraction agent hold-up vessel 12 and is connected, and discharge port is connected with Second distillation column 14 opening for feed and the first static mixer 6 extraction agent import respectively; Described first rectifying tower 8 opening for feed also exports with relay storage tank 4 and is connected, top gaseous phase outlet is connected to the first solvent receiving tank 10 opening for feed through the second condenser 9, and bottom liquid phases discharge port is then connected with pretreatment steaming hair device 2 opening for feed and Second distillation column 14 opening for feed respectively; Described Second distillation column 14 top gaseous phase discharge port distills out strippant returns the second static mixer 11 reverse-extraction agent import through condensation cycle, distill out target components and be connected to the second solvent receiving tank 16 through the 3rd condenser 15, bottom liquid phases discharge port is connected with pretreatment steaming hair device opening for feed and circulates.
In preferred embodiment, spent organic solvent is main containing DMSO, MEA composition, reclaiming high purity DMSO and MEA.
Reclaiming high purity DMSO, MEA one-component step: spent organic solvent is filtered after the obvious granule foreign of removal through filter 1 and delivers to pretreatment steaming hair device 2 underpressure distillation, leave away except the heavy constituent such as photoresist material, superpolymer from bottom part, from top, the mixed solvent distilled out containing light constituent and DMSO and MEA is collected into relay storage tank 4 after the first condenser 3 cryogenic condensation; Relay storage tank 4 solvent is beaten to the first static mixer 6 and is mixed by a certain percentage with the extraction agent (benzene) from extraction agent storage tank 5, initial extraction, and then enter extractive reaction tank 7 and again mix by a certain percentage with the extraction agent (benzene) from extraction agent storage tank 5, reextraction, automatic liquid separation after stratification; Extracting phase is mainly containing MEA, beat to the first rectifying tower 8 rectification under vacuum, after the light constituents such as tower top distillation water outlet, continue to distill out high purity MEA is collected into the first solvent receiving tank 10 after the second condenser 9 condensation, and residual components at the bottom of tower loops back pretreatment steaming hair device 2 and processes; Extraction phase is mainly containing DMSO and extraction agent (benzene), beat to the second static mixer 11 and mix by a certain percentage with the strippant (water) from strippant storage tank 12, initial extraction, and then enter reextraction retort 13 and again mix by a certain percentage with the extraction agent (water) from strippant storage tank 12, secondary counter extracts, automatic liquid separation after stratification; Extracting phase mainly containing benzene, loops back the first static mixer 6; Extraction phase is mainly containing DMSO and water, beat to Second distillation column 14 rectification under vacuum, tower top distills out reverse-extraction agent (water) and returns the second static mixer 11 through condensation cycle, tower top distills out high purity DMSO and is collected into the second solvent receiving tank 16 through the 3rd condenser 15 condensation, and residual components at the bottom of tower loops back pretreatment steaming hair device 2.
Above preferred embodiment is only in order to illustrate the technical solution of the utility model; not thereby the scope of the claims of the present utility model is limited; every the utility model that utilizes carries out equivalent structure transformation; or directly or indirectly change in form and details, all do not depart from scope of patent protection of the present utility model.

Claims (5)

1. one kind is reclaimed dimethyl sulfoxide (DMSO) from spent organic solvent, the system of thanomin, it is characterized in that: comprising: containing strainer (1), pretreatment steaming hair device (2), the pretreatment unit of the first condenser (3) and relay storage tank (4), containing extraction agent storage tank (5), first static mixer (6), extractive reaction tank (7), second static mixer (11), the Extraction and back extraction device of strippant storage tank (12) and reextraction retort (13), containing the first rectifying tower (8), second condenser (9), first solvent receiving tank (10), Second distillation column (14), the rectified purified device of the 3rd condenser (15) and the second solvent receiving tank (16), pretreatment unit, Extraction and back extraction device carry out equipment room with rectified purified device successively through pipeline and are connected and circulation.
2. the system reclaiming dimethyl sulfoxide (DMSO), thanomin from spent organic solvent according to claim 1, it is characterized in that: its top feed mouth of described pretreatment steaming hair device (2) is connected with strainer (1), bottom is provided with heavy constituent discharge outlet, and the top first condenser (3) of described pretreatment steaming hair device (2) is connected to the import of relay storage tank (4); Waste liquid import, the extraction agent import of described first static mixer (6) are connected with the outlet of relay storage tank (4) and extraction agent hold-up vessel (5) respectively, and the discharge port of described first static mixer (6) is connected to an opening for feed of extractive reaction tank (7); Another opening for feed of described extractive reaction tank (7) is connected with extraction agent hold-up vessel (5), and the discharge port of described extractive reaction tank (7) is connected with the opening for feed of the first rectifying tower (8) and the waste liquid import of the second static mixer (11) respectively; The reverse-extraction agent import of described second static mixer (11) is connected with the outlet of strippant storage tank (12), and the discharge port of described second static mixer (11) is then connected with an opening for feed of reextraction retort (13); Another opening for feed of described reextraction retort (13) is connected with the outlet of reverse-extraction agent hold-up vessel (12), and the discharge port of described reextraction retort (13) is connected with the opening for feed of Second distillation column (14) and the extraction agent import of the first static mixer (6) respectively; The opening for feed of described first rectifying tower (8) is also connected with the outlet of relay storage tank (4), the top gaseous phase outlet of described first rectifying tower (8) is connected to the opening for feed of the first solvent receiving tank (10) through the second condenser (9), the bottom liquid phases discharge port of described first rectifying tower (8) is then connected with the opening for feed of pretreatment steaming hair device (2) and the opening for feed of Second distillation column (14) respectively; The top gas phase discharge port of described Second distillation column (14) is connected to the second solvent receiving tank (16) through the 3rd condenser (15), the top gas phase discharge port of described Second distillation column (14) is also connected with the import of the second static mixer (11), and the bottom liquid phases discharge port of described Second distillation column (14) is connected with the opening for feed of pretreatment steaming hair device (2).
3. the system reclaiming dimethyl sulfoxide (DMSO), thanomin from spent organic solvent according to claim 1, is characterized in that: described pretreatment steaming hair device (2) is luwa evaporator.
4. the system reclaiming dimethyl sulfoxide (DMSO), thanomin from spent organic solvent according to claim 1, is characterized in that: described extractive reaction tank (7), reextraction retort (13) all assemble remote controlled differential pressure transmitter formula automatic liquid separation device.
5. the system reclaiming dimethyl sulfoxide (DMSO), thanomin from spent organic solvent according to claim 1, is characterized in that: described first rectifying tower (8) and Second distillation column (14) inside employing model are the Stainless Steel Wire corrugated wire gauze packing of 700Y.
CN201520538076.XU 2015-07-23 2015-07-23 System for retrieve dimethyl sulfoxide , ethanolamine among useless organic solvent of follow Active CN205223068U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108840495A (en) * 2018-05-13 2018-11-20 四川久远化工技术有限公司 A kind of stripping waste liquor method of purification
CN112110587A (en) * 2020-09-03 2020-12-22 南京沿江资源生态科学研究院有限公司 Equipment for extracting mixed alcohol from light components at top of high-concentration wastewater pretreatment rectifying tower

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108840495A (en) * 2018-05-13 2018-11-20 四川久远化工技术有限公司 A kind of stripping waste liquor method of purification
CN108840495B (en) * 2018-05-13 2020-12-22 四川久远化工技术有限公司 Method for purifying stripping waste liquid
CN112110587A (en) * 2020-09-03 2020-12-22 南京沿江资源生态科学研究院有限公司 Equipment for extracting mixed alcohol from light components at top of high-concentration wastewater pretreatment rectifying tower

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