CN202081039U - Dimethyl sulfoxide (DMSO) recovery and refining device - Google Patents
Dimethyl sulfoxide (DMSO) recovery and refining device Download PDFInfo
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- CN202081039U CN202081039U CN2011201229414U CN201120122941U CN202081039U CN 202081039 U CN202081039 U CN 202081039U CN 2011201229414 U CN2011201229414 U CN 2011201229414U CN 201120122941 U CN201120122941 U CN 201120122941U CN 202081039 U CN202081039 U CN 202081039U
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Abstract
The utility model discloses a dimethyl sulfoxide (DMSO) recovery and refining device, which comprises a primary dehydration tower, a film evaporator, an intermediate primary distillation tank, a secondary dehydration tower and a DMSO refining tower. The primary dehydration tower is connected with the intermediate primary distillation tank, and the film evaporator is connected with the intermediate primary distillation tank and is then sequentially connected with the secondary dehydration tower and the DMSO refining tower. Raw materials with DMSO are divided into two parts, the raw materials with low-concentration DMSO contain no polymer, the DMSO content is 2.0-15.0 percent, and the raw materials with low-concentration DMSO are directly fed into the primary dehydration tower to dehydrate most of water in the raw materials; and the raw materials with high-concentration DMSO contain polymer, the DMSO content is 22.0-50.0 percent, the polymer is removed through the film evaporator, and the raw materials are then fed into the secondary dehydration tower along with the dehydrated raw materials with low-concentration DMSO after polymer removal, the problems of tower blockage, removal of impurities and energy conservation can be solved effectively, and the whole process is reasonable and has a high degree of automation.
Description
Technical field
The utility model relates to a kind of recovery, refining of solvent, especially a kind of recovery, refining plant that is used for dimethyl sulfoxide (DMSO).
Background technology
Dimethyl sulfoxide (DMSO) DMSO is described as " menstruum universale ", is in the organic solvent of using always, the strongest a kind of of dissolving power.DMSO is widely used as solvent and reaction reagent, particularly makes process solvent and the solvent that reels off raw silk from cocoons in the acrylonitrile polymerization reaction, makes the synthetic and solvent that reels off raw silk from cocoons of urethane, makes the synthetic of polymeric amide, polyimide and polysulfone resin etc.Can produce the solution that contains a large amount of DMSO and superpolymer in the above-mentioned technological process, therefore reclaim the pressure that DMSO can reduce environmental protection on the one hand, recyclable on the other hand DMSO is retrieval system again, produces huge economic benefit.
Summary of the invention
Technical problem to be solved in the utility model is to provide a kind of all DMSO that contain in the high polymeric solution all can obtain efficient recovery, quality product height, good stability and level of automation high recovery, refining plant.
In order to solve the problems of the technologies described above, the technical solution adopted in the utility model is: a kind of recovery, refining plant that is used for dimethyl sulfoxide (DMSO), comprise one-level dehydration tower, luwa evaporator, just distill tundish, secondary dehydration tower and dimethyl sulfoxide (DMSO) DMSO treating tower, the one-level dehydration tower connects distillation tundish just, luwa evaporator connects distillation tundish just, and just the distillation tundish connect secondary dehydration tower, DMSO treating tower successively then.
The middle part of described one-level dehydration tower is provided with the lower concentration raw material inlet, and the discharging pipeline at the bottom of the one-level dehydration Tata is connected with the feeding line that just distills the tundish top, and the one-level dehydration column overhead connects the discharging pipeline of waste water; Luwa evaporator top is provided with the high density raw material inlet, the luwa evaporator bottom row of being provided with superpolymer mouth, the luwa evaporator top is provided with the gas phase discharge port, and the gas phase discharge port that the luwa evaporator top is provided with connects the feeding line at distillation tundish top just through condenser; The discharging pipeline that first distillation tundish are provided with is connected with the middle part opening for feed of secondary dehydration tower; The secondary dehydration column overhead connects the discharging pipeline of waste water, and the discharging pipeline at the bottom of the secondary dehydration Tata is connected with the feeding line at DMSO treating tower middle part; The discharging pipeline connects the superpolymer storage tank at the bottom of the tower of DMSO treating tower, and DMSO treating tower top connects the discharging pipeline of the DMSO product after making with extra care.
Described lower concentration DMSO raw material is not contain superpolymer, and DMSO content is 2.0%-15.0% (wt); Described high density DMSO raw material contains superpolymer, and DMSO content is 22.0-50.0% (wt).
The condenser medium of described one-level dehydration tower adopts water coolant; The condenser medium of described secondary dehydration tower and DMSO treating tower adopts freezing aqueous glycol solution.
The column internals of described three towers is efficient structured packing and forms; The reboiler of described three towers all selects for use forced circulating reboiler to carry out the heating of tower still.
The beneficial effects of the utility model are:
1) takes into full account the physicochemical property of DMSO raw material system, the device of whole separating technology is chosen to be stainless steel, as 304 materials.Thereby the problem of material corrosion resistance nature in the separating technology of having solved has fully guaranteed the quality and the stability of product.
2) distill before the tundish at the beginning of the utility model places luwa evaporator, superpolymer in the raw material is removed in advance, solve its temperature-sensitive effectively and easily decomposed, tied phenomenons such as carbon, and this automation technolo degree height, process energy consumption are less, for large-scale continuous production application provides certain advantage.
3) another advantage of the present utility model is exactly earlier the DMSO raw material to be divided into two strands.Lower concentration DMSO raw material is not contain superpolymer, and DMSO content is 2.0%-15.0% (wt), directly advances the one-level dehydration tower, sloughs most water in the raw material; High density DMSO raw material contains superpolymer, and DMSO content is 22.0-50.0% (wt), is taken off behind the slag by luwa evaporator and together advances the secondary dehydration tower with dehydration back main raw material again.Efficiently solve stifled tower jointly, take off impurity, problem such as energy-conservation, make that follow-up purified quality product is very high.
4) the condenser medium of one-level dehydration tower adopts water coolant, draws materials conveniently, and energy consumption is little, easily handles.
5) the condenser medium of secondary dehydration tower and DMSO treating tower adopts freezing ethylene glycol, because system is the decompression operation device;
6) reboiler of each tower all selects for use forced circulating reboiler to carry out the heating of tower still.
The utility model reclaims, makes with extra care DMSO effectively by appropriate design.Whole process flow is reasonable, level of automation is high and have that the process energy consumption is lower, quality product is high and characteristics such as good stability, is that a kind of efficient feasible DMSO reclaims, refining plant, uses this device that high-purity DMSO (〉=99.99%) can be provided product.
Description of drawings
Fig. 1 is recovery, the refining plant that is used for dimethyl sulfoxide (DMSO) of the present utility model.
Embodiment
Below in conjunction with the drawings and specific embodiments the utility model is described in further detail:
As shown in Figure 1, recovery, the refining plant that is used for dimethyl sulfoxide (DMSO) of the present utility model, comprise one-level dehydration tower 1, luwa evaporator 2, just distill tundish 3, secondary dehydration tower 4 and dimethyl sulfoxide (DMSO) DMSO treating tower 5, one-level dehydration tower 1 connects distillation tundish 3 just, luwa evaporator 2 connects distillation tundish 3 just, and just distillation tundish 3 connect secondary dehydration tower 4, DMSO treating tower 5 successively then.
Specifically, the middle part of described one-level dehydration tower 1 is provided with lower concentration DMSO raw material inlet, and the discharging pipeline at the bottom of one-level dehydration tower 1 tower is connected with the feeding line that just distills tundish 3 tops, and one-level dehydration tower 1 cat head connects the discharging pipeline of waste water; Luwa evaporator 2 tops are provided with high density DMSO raw material inlet, luwa evaporator 2 bottoms are provided with row's superpolymer mouth, luwa evaporator 2 tops are provided with the gas phase discharge port, and the gas phase discharge port that luwa evaporator 2 tops are provided with connects the feeding line at distillation tundish 3 tops just through condenser; The discharging pipeline that first distillation tundish 3 are provided with is connected with the middle part opening for feed of secondary dehydration tower 4; Secondary dehydration tower 4 cats head connect the discharging pipeline of waste water, and the discharging pipeline at the bottom of secondary dehydration tower 4 towers is connected with the feeding line at DMSO treating tower 5 middle parts; The discharging pipeline connects the superpolymer storage tank at the bottom of the tower of DMSO treating tower 5, and DMSO treating tower 5 tops connect the discharging pipeline of the DMSO product after making with extra care.
Described lower concentration DMSO raw material is not contain superpolymer, and DMSO content is 2.0%-15.0% (wt); Described high density DMSO raw material contains superpolymer, and DMSO content is 22.0-50.0% (wt).
The condenser medium of described one-level dehydration tower 1 adopts water coolant; The condenser medium of described secondary dehydration tower and DMSO treating tower adopts freezing aqueous glycol solution.
The column internals of described three towers is efficient structured packing and forms; The reboiler of described three towers all selects for use forced circulating reboiler to carry out the heating of tower still.
Described recovery, device are chosen to be stainless steel.
The recovery of above-mentioned recovery, the dimethyl sulfoxide (DMSO) of refining plant, refining separation method comprise following step:
1) lower concentration DMSO raw material enters the one-level dehydration tower, and the top distillates the waste water that contains a small amount of DMSO, and the cut of discharging at the bottom of the tower is to just distilling tundish;
2) high density DMSO raw material enters luwa evaporator, and heavy constituent are discharged in the bottom, and the gaseous component on top enters distillation tundish just through condensation;
3) after above-mentioned two components that enter first distillation tundish are respectively mixed in first distillation tundish, enter the secondary dehydration tower, the top distillates the waste water that contains a small amount of DMSO, and the cut of discharging at the bottom of the tower is to the DMSO treating tower;
4) the DMSO product is from the extraction of DMSO treating tower cat head, and the cut that discharge the bottom is to the superpolymer storage tank.
Described lower concentration DMSO raw material is not contain superpolymer, and DMSO content is 2.0%-15.0% (wt); Described high density DMSO raw material contains superpolymer, and DMSO content is 22.0-50.0% (wt).
Described one-level dehydration tower operational condition is: the cat head working pressure is 10.0～20.OKPa, tower pressure reduction 0.8～1.0KPa, and reflux ratio is 0.5/1～2/1, and tower top temperature is 45.0～55.0 ℃, and column bottom temperature is 85.0～90.0 ℃; The luwa evaporator operational condition is: working pressure is 1～5KPa, and the upper gaseous phase temperature out is 55.0～65.0 ℃; Secondary dehydration tower operational condition is: the cat head working pressure is 1.0～5.OKPa, tower pressure reduction 0.9～1.1KPa, and reflux ratio is 0.5/1～2/1, and tower top temperature is 15.0～25.0 ℃, and column bottom temperature is 85.0～90.0 ℃; DMSO treating tower operational condition is: the cat head working pressure is 1.0～5.OKPa, tower pressure reduction 1.1～1.3KPa, and reflux ratio is 0.5/1～2/1, and tower top temperature is 75.0～85.0 ℃, and column bottom temperature is 85.0～90.0 ℃.
Recovery of the present utility model, process for purification are by the one-level dehydration tower, luwa evaporator, just distill tundish, secondary dehydration tower, DMSO treating tower and finish.
The utility model is by two dehydration towers and recovery, the process for refining that rectifying tower is formed, three towers are packing tower, to guarantee that this tower has higher separation efficiency and has lower pressure drop again, each is divided into rectifying section and stripping section, constitute by efficient structured packing, all adopt forced circulating reboiler to carry out the heating of tower still simultaneously.
Be elaborated below in conjunction with specific embodiment:
Embodiment 1
Be used to make the polyacrylonitrile polymerization of carbon fiber and the stock liquid that contains DMSO waste water that spinning process produces is divided into two strands at domestic, DMSO lower concentration raw material promptly contains 12.0% (wt) and does not contain high boiling material and DMSO high density raw material promptly contains 32.0% (wt) but contains high boiling material.At first the lower concentration raw material is entered the one-level dehydration tower, 46.5 ℃ of cat head temperature, 86.0 ℃ of still temperature, tower top pressure (cutting off) is 10.0KPa, and tower pressure reduction is 0.8KPa, and the top obtains purity the end greater than 90% light constituent DMSO, enters distillation tundish just; The high density raw material at first enters luwa evaporator simultaneously, and bottom discharging superpolymer is handled to the battery limit (BL), and material enters distillation tundish just from the top; Material enters the secondary dehydration tower from first distillation tundish, 16.2 ℃ of cat head temperature, and 86.0 ℃ of still temperature, tower top pressure (cutting off) is 1.5KPa, and tower pressure reduction is 0.9KPa, and the end, top, obtain light constituent DMSO, enters the DMSO treating tower, and overhead fraction is delivered to waste water tank processing outside the battery limit (BL); DMSO treating tower operating parameters is: 76.2 ℃ of top temperature, and 85.5 ℃ of still temperature, tower top pressure (cutting off) is 1.0KPa, and tower pressure reduction is 1.1KPa, and bottom discharging superpolymer is handled to the battery limit (BL).
Embodiment 2
The stock liquid that contains DMSO waste water at certain Fibre Plant is divided into two strands, and DMSO lower concentration raw material promptly contains 10.0% (wt) and do not contain high boiling material and DMSO high density raw material promptly contains 40.0% (wt) but contains high boiling material.At first the lower concentration raw material is entered the one-level dehydration tower, 49.5 ℃ of cat head temperature, 87.0 ℃ of still temperature, tower top pressure (cutting off) is 15.5KPa, and tower pressure reduction is 0.88KPa, and the top obtains purity the end greater than 90% light constituent DMSO, enters distillation tundish just; The high density raw material at first enters luwa evaporator simultaneously, and bottom discharging superpolymer is handled to the battery limit (BL), and material enters distillation tundish just from the top; Material enters the secondary dehydration tower from first distillation tundish, 20.0 ℃ of cat head temperature, and 88.1 ℃ of still temperature, tower top pressure (cutting off) is 2.4KPa, and tower pressure reduction is 0.95KPa, and the end, top, obtain light constituent DMSO, enters the DMSO treating tower, and overhead fraction is delivered to waste water tank processing outside the battery limit (BL); DMSO treating tower operating parameters is: 79.0 ℃ of top temperature, and 88.5 ℃ of still temperature, tower top pressure (absolute pressure) is 2.1KPa, and tower pressure reduction is 1.2KPa, and bottom discharging superpolymer is handled to the battery limit (BL).
Embodiment 3
The stock liquid that contains DMSO waste water at certain Fibre Plant is divided into two strands, and DMSO lower concentration raw material promptly contains 14.0% (wt) and do not contain high boiling material and DMSO high density raw material promptly contains 30.0% (wt) but contains high boiling material.At first the lower concentration raw material is entered the one-level dehydration tower, 54.2 ℃ of cat head temperature, 89.0 ℃ of still temperature, tower top pressure (cutting off) is 19.5KPa, and tower pressure reduction is 1.0KPa, and the top obtains purity the end greater than 90% light constituent DMSO, enters distillation tundish just; The high density raw material at first enters luwa evaporator simultaneously, and bottom discharging superpolymer is handled to the battery limit (BL), and material enters distillation tundish just from the top; Material enters the secondary dehydration tower from first distillation tundish, 24.0 ℃ of cat head temperature, and 89.8 ℃ of still temperature, tower top pressure (cutting off) is 4.5KPa, and tower pressure reduction is 1.1KPa, and the end, top, obtain light constituent DMSO, enters the DMSO treating tower, and overhead fraction is delivered to waste water tank processing outside the battery limit (BL); DMSO treating tower operating parameters is: 84.5 ℃ of top temperature, and 89.0 ℃ of still temperature, tower top pressure (cutting off) is 4.8KPa, and tower pressure reduction is 1.3KPa, and bottom discharging superpolymer is handled to the battery limit (BL).
In sum, content of the present utility model is not limited in the above-described embodiment, knowledgeable people in the same area can propose other embodiment easily within technical director's thought of the present utility model, but this embodiment is included within the scope of the present utility model.
Claims (5)
1. recovery, refining plant that is used for dimethyl sulfoxide (DMSO), it is characterized in that, comprise one-level dehydration tower (1), luwa evaporator (2), just distill tundish (3), secondary dehydration tower (4) and dimethyl sulfoxide (DMSO) DMSO treating tower (5), one-level dehydration tower (1) connects distillation tundish (3) just, luwa evaporator (2) connects distillation tundish (3) just, and just distillation tundish (3) connect secondary dehydration tower (4), DMSO treating tower (5) successively then.
2. recovery, the refining plant that is used for dimethyl sulfoxide (DMSO) according to claim 1, it is characterized in that, the middle part of described one-level dehydration tower (1) is provided with the lower concentration raw material inlet, discharging pipeline at the bottom of one-level dehydration tower (1) tower is connected with the feeding line that just distills tundish (3) top, and one-level dehydration tower (1) cat head connects the discharging pipeline of waste water; Luwa evaporator (2) top is provided with the high density raw material inlet, luwa evaporator (2) the bottom row of being provided with superpolymer mouth, luwa evaporator (2) top is provided with the gas phase discharge port, and the gas phase discharge port that luwa evaporator (2) top is provided with connects the feeding line at distillation tundish (3) top just through condenser; The discharging pipeline that first distillation tundish (3) are provided with is connected with the middle part opening for feed of secondary dehydration tower (4); Secondary dehydration tower (4) cat head connects the discharging pipeline of waste water, and the discharging pipeline at the bottom of secondary dehydration tower (4) tower is connected with the feeding line at DMSO treating tower (5) middle part; The discharging pipeline connects the superpolymer storage tank at the bottom of the tower of DMSO treating tower (5), and DMSO treating tower (5) top connects the discharging pipeline of the DMSO product after making with extra care.
3. recovery, the refining plant that is used for dimethyl sulfoxide (DMSO) according to claim 1 and 2 is characterized in that, the condenser medium of described one-level dehydration tower (1) adopts water coolant; The condenser medium of described secondary dehydration tower (4) and DMSO treating tower (5) adopts freezing aqueous glycol solution.
4. recovery, the refining plant that is used for dimethyl sulfoxide (DMSO) according to claim 1 and 2 is characterized in that, the column internals of described three towers is efficient structured packing and forms; The reboiler of described three towers all selects for use forced circulating reboiler to carry out the heating of tower still.
5. recovery, the refining plant that is used for dimethyl sulfoxide (DMSO) according to claim 1 and 2 is characterized in that described recovery, device are chosen to be stainless steel.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011201229414U CN202081039U (en) | 2011-04-22 | 2011-04-22 | Dimethyl sulfoxide (DMSO) recovery and refining device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011201229414U CN202081039U (en) | 2011-04-22 | 2011-04-22 | Dimethyl sulfoxide (DMSO) recovery and refining device |
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| CN202081039U true CN202081039U (en) | 2011-12-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107362568A (en) * | 2017-09-04 | 2017-11-21 | 中安信科技有限公司 | The apparatus and method of high efficiente callback solvent in a kind of high-performance carbon fibre production |
| CN110902742A (en) * | 2019-12-09 | 2020-03-24 | 成都民航六维航化有限责任公司 | Method for recovering organic matters in high-concentration organic wastewater |
| CN113559542A (en) * | 2021-07-19 | 2021-10-29 | 常州乐研分离技术有限公司 | Device and method for DMSO (dimethyl sulfoxide) concentration process |
| CN114436458A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Solvent recovery system and method for flushing waste liquid in carbon fiber precursor production and application of solvent recovery system and method |
| CN116199608A (en) * | 2023-01-19 | 2023-06-02 | 常州乐研分离技术有限公司 | Process and device for recovering solvent from wastewater in carbon fiber production |
-
2011
- 2011-04-22 CN CN2011201229414U patent/CN202081039U/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107362568A (en) * | 2017-09-04 | 2017-11-21 | 中安信科技有限公司 | The apparatus and method of high efficiente callback solvent in a kind of high-performance carbon fibre production |
| CN107362568B (en) * | 2017-09-04 | 2018-12-04 | 中安信科技有限公司 | The method of high efficiente callback solvent in a kind of production of high-performance carbon fibre |
| CN110902742A (en) * | 2019-12-09 | 2020-03-24 | 成都民航六维航化有限责任公司 | Method for recovering organic matters in high-concentration organic wastewater |
| CN114436458A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Solvent recovery system and method for flushing waste liquid in carbon fiber precursor production and application of solvent recovery system and method |
| CN114436458B (en) * | 2020-10-20 | 2023-07-04 | 中国石油化工股份有限公司 | Solvent recovery system and recovery method for flushing waste liquid in carbon fiber precursor production and application of solvent recovery system and recovery method |
| CN113559542A (en) * | 2021-07-19 | 2021-10-29 | 常州乐研分离技术有限公司 | Device and method for DMSO (dimethyl sulfoxide) concentration process |
| CN116199608A (en) * | 2023-01-19 | 2023-06-02 | 常州乐研分离技术有限公司 | Process and device for recovering solvent from wastewater in carbon fiber production |
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| C14 | Grant of patent or utility model | ||
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| AV01 | Patent right actively abandoned |
Granted publication date: 20111221 Effective date of abandoning: 20131127 |
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| RGAV | Abandon patent right to avoid regrant |