CN114409167A - High COD concentration wastewater treatment and recovery process in PSPI production process - Google Patents
High COD concentration wastewater treatment and recovery process in PSPI production process Download PDFInfo
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- CN114409167A CN114409167A CN202210093825.7A CN202210093825A CN114409167A CN 114409167 A CN114409167 A CN 114409167A CN 202210093825 A CN202210093825 A CN 202210093825A CN 114409167 A CN114409167 A CN 114409167A
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/42—Liquid level
Abstract
The invention discloses a high COD concentration wastewater treatment and recovery process in the PSPI production process, which comprises the following steps of collecting wastewater, feeding the collected wastewater into a wastewater collection tank, feeding the wastewater into an acid-base neutralization treatment tank by a first wastewater pump to adjust the pH value to 7-9, feeding the wastewater into a solvent recovery tank by a second wastewater pump to be distilled to obtain a water phase and an oil phase respectively, feeding the water phase into a water phase storage tank, uniformly treating and discharging the water phase, feeding the oil phase into an oil phase storage tank, feeding the oil phase into a continuous rectifying device to be rectified and separated to obtain an NMP organic solvent, and storing the NMP organic solvent in a finished product tank. The high COD concentration wastewater treatment and recovery process in the PSPI production process with the structure can reduce the COD concentration in the wastewater, simultaneously can recycle the NMP organic solvent, has simpler treatment process after the COD in the wastewater is reduced, reduces the treatment time and the treatment cost, and greatly reduces the wastewater treatment capacity.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a high COD concentration wastewater treatment and recovery process in a PSPI production process.
Background
The sewage generally contains inorganic pollutants (acid, alkali, salt, heavy metal ions and the like), organic pollutants (organic hydrocarbons such as alkane, alkene, ketone, ether, phenol, aldehyde and the like), and biological pollutants (containing pathogenic microorganisms such as bacteria, viruses and the like). The production process of photosensitive polyimide (PSPI) generally produces a large amount of waste water containing 1 wt% of hydrochloric acid and sulfurous acid, 10 to 20 wt% of NMP solvent, 0.5 to 0.7 wt% of sodium ion salt, and a small amount of solid particles.
The general treatment mode adopts the processes of acid-base neutralization regulation, precipitation, heavy metal capture, high-pressure ozone electrolysis, precise adsorption capture, photocatalytic reaction and advanced oxidation to treat sewage.
The defects and shortcomings of the prior art are as follows:
1. the high COD wastewater containing the NMP organic solvent is treated by the prior art, the floor area of a sewage tank and the like is greatly restricted by a field, the process is complicated, the sludge and the like generated in the process need secondary treatment, and the treatment cost is high;
NMP organic solvent is a polar solvent with strong selectivity and good stability, and has the advantages of low toxicity, high boiling point, strong dissolving power, nonflammability, biodegradability, recyclability, safe use, suitability for various formula purposes and the like. Through the original process treatment, the residual NMP organic solvent in the wastewater is decomposed, the aim of recycling can not be achieved, and the phase change increases the production cost for enterprises.
Disclosure of Invention
The invention aims to provide a high COD concentration wastewater treatment and recovery process in the PSPI production process, so as to solve the problems that NMP organic solvent in the wastewater is decomposed and cannot be recycled and the wastewater treatment process is complex.
In order to achieve the purpose, the invention provides a high COD concentration wastewater treatment and recovery process in the PSPI production process, which comprises the following steps of collecting wastewater, feeding the collected wastewater into a wastewater collection tank, feeding the wastewater into an acid-base neutralization treatment tank by a first wastewater pump to adjust the pH value to 7-9, feeding the wastewater into a solvent recovery tank by a second wastewater pump to be distilled to obtain a water phase and an oil phase respectively, feeding the water phase into a water phase storage tank, uniformly treating and discharging the water phase, feeding the oil phase into an oil phase storage tank, feeding the oil phase into a continuous rectification device to be rectified and separated to obtain an NMP organic solvent, and storing the NMP organic solvent in a finished product tank;
alkaline liquid storage jar is linked together through measuring pump and acid-base neutralization treatment tank, is provided with the pH controller in the acid-base neutralization treatment tank, and the pH controller is connected with the measuring pump through controller one, is provided with the level gauge in the waste water collection tank, and the level gauge is connected with waste liquid pump one through controller two.
Preferably, the continuous rectifying device is formed by connecting a plurality of rectifying and separating mechanisms with the same structure in series through a cache tank, each rectifying and separating mechanism comprises a rectifying tower, a condenser and a reflux tank, light components flowing out of the top end of the rectifying tower sequentially pass through the condensers and the reflux tanks and then return to the middle of the rectifying tower, and heavy components flowing out of the bottom end of the rectifying tower flow into a waste liquid collecting tank.
Preferably, the continuous rectification device comprises a primary rectification separation mechanism and a secondary rectification separation mechanism which are sequentially connected, the primary rectification separation mechanism comprises a first rectification tower, a first condenser and a first reflux tank, light components flowing out of the top end of the first rectification tower sequentially pass through the first condenser and the first reflux tank and then return to the middle part of the first rectification tower, the secondary rectification separation mechanism comprises a second rectification tower, a second condenser and a second reflux tank, the light components flowing out of the top end of the second rectification tower sequentially pass through the second condenser and the second reflux tank and then return to the middle part of the second rectification tower, and heavy components flowing out of the bottom end of the first rectification tower and the bottom end of the second rectification tower flow into a waste liquid collection tank;
the feed inlet of the first rectifying tower is communicated with the oil phase storage tank through a first cache tank, the feed inlet of the second rectifying tower is communicated with the first reflux tank through a second cache tank, and the finished product tank is communicated with the second reflux tank through a third cache tank.
Preferably, the oil phase storage tank, the first buffer tank, the second buffer tank and the third buffer tank are all provided with a transport pump.
Preferably, the second condenser is communicated with the catcher.
Preferably, the first rectifying tower is subjected to normal-pressure rectification treatment at the temperature of 80-90 ℃, and the reflux ratio is 1.
Preferably, the second rectifying tower is used for reduced pressure distillation, the temperature is 60-75 ℃, the vacuum degree is 1mmHg, the reflux ratio is controlled to be 1.0-1.5 in a light fraction section, and the section control of a transition fraction is 2-3.
Preferably, the content of the NMP organic solvent in the oil phase storage tank is 80-90%.
Preferably, the content of NMP organic solvent in the finished tank is 99% or more.
Therefore, the technology for treating and recycling high-COD wastewater in the PSPI production process with the structure can reduce the COD concentration in the wastewater, simultaneously recycle the NMP organic solvent, simplify the treatment process after the COD in the wastewater is reduced, reduce the treatment time and the treatment cost and greatly reduce the wastewater treatment capacity.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a process flow diagram of an embodiment of a high COD concentration wastewater treatment and recovery process in the PSPI production process of the present invention;
FIG. 2 is a flow chart of a continuous rectification device of an embodiment of a high COD concentration wastewater treatment and recovery process in the PSPI production process.
Detailed Description
The technical solution of the present invention is further illustrated by the accompanying drawings and examples.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The use of "first," "second," and similar terms in the present application do not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
Embodiments of the present invention will be further described with reference to the accompanying drawings. As shown in fig. 1-2, a high COD concentration wastewater treatment and recovery process in PSPI production process includes the following steps, collecting wastewater, entering a wastewater collection tank, sending the wastewater to an acid-base neutralization treatment tank by a first wastewater pump to adjust pH to 7-9, performing acid-base neutralization to mainly remove hydrogen ions in the wastewater, neutralizing the wastewater to neutrality, reducing corrosivity of the wastewater, sending the wastewater to a solvent recovery tank by a second wastewater pump to perform distillation to obtain a water phase and an oil phase, respectively, sending the water phase to a water phase storage tank, performing uniform treatment and discharging, sending the oil phase to an oil phase storage tank, introducing the oil phase to a continuous distillation device to perform distillation separation to obtain an NMP organic solvent, storing the NMP organic solvent in a finished product tank, wherein the main components of the wastewater in the solvent recovery tank are sodium ion salts and NMP organic solvent crude products, distilling the wastewater in the solvent recovery tank, most of water is distilled out of a solution recovery tank and is stored in a water phase storage tank, the water phase storage tank can be connected to a sewage station for treatment, and is discharged after reaching the discharge standard, an NMP organic solvent crude product formed by an NMP organic solvent and other organic impurities is mainly contained in an oil phase storage tank, and the content of the NMP organic solvent in the oil phase storage tank is 80-90%; the continuous rectifying device is formed by connecting a plurality of rectifying and separating mechanisms with the same structure in series through a cache tank, each rectifying and separating mechanism comprises a rectifying tower, a condenser and a reflux tank, light components flowing out of the top end of the rectifying tower sequentially pass through the condenser and the reflux tank and then return to the middle of the rectifying tower, and heavy components flowing out of the bottom end of the rectifying tower flow into a waste liquid collecting tank. And (3) rectifying the crude NMP organic solvent in the oil phase storage tank for multiple times by using a continuous rectifying device to obtain the NMP organic solvent, wherein the content of the NMP organic solvent in the finished product tank is more than 99%.
The alkaline liquid storage tank is communicated with the acid-base neutralization treatment tank through a metering pump, sodium hydroxide solution is mainly stored in the alkaline liquid storage tank, a pH controller is arranged in the acid-base neutralization treatment tank and is connected with the metering pump through a first controller, the pH controller comprises a pH monitor and a pH probe, the pH probe extends into wastewater in the acid-base neutralization treatment tank and transmits pH value signals of the wastewater to the pH monitor, the pH monitor transmits signals to a first controller through comparing a set pH value with the pH value of the wastewater, if the wastewater is acidic, the first controller controls to open the metering pump and dropwise add the sodium hydroxide into the acid-base neutralization treatment tank until the pH value reaches 7-9, the first controller controls to close the metering pump, a liquid level meter is arranged in the wastewater collection tank and is connected with a first wastewater pump through a second controller, when the wastewater level in the wastewater collection tank is high, and the second controller controls the first waste liquid pump to be opened so that the waste liquid enters the acid-base neutralization treatment tank, and when the liquid level of the waste water in the waste water collection tank is lower, the first controller controls the first waste liquid pump to be closed.
The continuous rectification device comprises a first-stage rectification separation mechanism and a second-stage rectification separation mechanism which are sequentially connected, wherein the first-stage rectification separation mechanism comprises a first rectification tower, a first condenser and a first reflux tank, light components flowing out of the top end of the first rectification tower sequentially pass through the first condenser and the first reflux tank and then return to the middle of the first rectification tower, the second-stage rectification separation mechanism comprises a second rectification tower, a second condenser and a second reflux tank, light components flowing out of the top end of the second rectification tower sequentially pass through the second condenser and the second reflux tank and then return to the middle of the second rectification tower, heavy components flowing out of the bottom end of the first rectification tower and the second rectification tower uniformly flow into a waste liquid collecting tank, the first rectification tower is subjected to normal-pressure rectification treatment, the temperature is 80-90 ℃, and the reflux ratio is 1. And the second rectifying tower is used for reduced pressure distillation, the temperature is 60-75 ℃, the vacuum degree is 1mmHg, the reflux ratio is controlled to be 1.0-1.5 in a light fraction section, and the transition fraction section is controlled to be 2-3. The feed inlet of the first rectifying tower is communicated with the oil phase storage tank through a first cache tank, the feed inlet of the second rectifying tower is communicated with the first reflux tank through a second cache tank, and the finished product tank is communicated with the second reflux tank through a third cache tank. And the discharge ports of the oil phase storage tank, the first cache tank, the second cache tank and the third cache tank are all provided with transport pumps. The second condenser is communicated with the catcher.
Therefore, the technology for treating and recycling high-COD wastewater in the PSPI production process with the structure can reduce the COD concentration in the wastewater, simultaneously recycle the NMP organic solvent, simplify the treatment process after the COD in the wastewater is reduced, reduce the treatment time and the treatment cost and greatly reduce the wastewater treatment capacity.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (9)
1. A high COD concentration wastewater treatment and recovery process in the PSPI production process is characterized in that: the method comprises the following steps that the wastewater is collected and then enters a wastewater collection tank, the wastewater is sent into an acid-base neutralization treatment tank through a first wastewater pump to adjust the pH value to 7-9, then the wastewater is sent into a solvent recovery tank through a second wastewater pump to be distilled to respectively obtain a water phase and an oil phase, the water phase enters a water phase storage tank and then is treated uniformly and discharged, the oil phase enters an oil phase storage tank, and then the oil phase is introduced into a continuous rectifying device to be rectified and separated to obtain an NMP organic solvent which is stored in a finished product tank;
alkaline liquid storage jar is linked together through measuring pump and acid-base neutralization treatment tank, is provided with the pH controller in the acid-base neutralization treatment tank, and the pH controller is connected with the measuring pump through controller one, is provided with the level gauge in the waste water collection tank, and the level gauge is connected with waste liquid pump one through controller two.
2. The high COD concentration wastewater treatment and recovery process in the PSPI production process according to claim 1, which is characterized in that: the continuous rectifying device is formed by connecting a plurality of rectifying and separating mechanisms with the same structure in series through a cache tank, each rectifying and separating mechanism comprises a rectifying tower, a condenser and a reflux tank, light components flowing out of the top end of the rectifying tower sequentially pass through the condenser and the reflux tank and then return to the middle of the rectifying tower, and heavy components flowing out of the bottom end of the rectifying tower flow into a waste liquid collecting tank.
3. The high COD concentration wastewater treatment and recovery process in the PSPI production process according to claim 2, which is characterized in that: the continuous rectification device comprises a primary rectification separation mechanism and a secondary rectification separation mechanism which are sequentially connected, wherein the primary rectification separation mechanism comprises a first rectification tower, a first condenser and a first reflux tank, light components flowing out of the top end of the first rectification tower sequentially pass through the first condenser and the first reflux tank and then return to the middle of the first rectification tower, the secondary rectification separation mechanism comprises a second rectification tower, a second condenser and a second reflux tank, light components flowing out of the top end of the second rectification tower sequentially pass through the second condenser and the second reflux tank and then return to the middle of the second rectification tower, and heavy components flowing out of the bottom end of the first rectification tower and the bottom end of the second rectification tower flow into a waste liquid collecting tank;
the feed inlet of the first rectifying tower is communicated with the oil phase storage tank through a first cache tank, the feed inlet of the second rectifying tower is communicated with the first reflux tank through a second cache tank, and the finished product tank is communicated with the second reflux tank through a third cache tank.
4. The high COD concentration wastewater treatment and recovery process in the PSPI production process according to claim 3, which is characterized in that: and the discharge ports of the oil phase storage tank, the first cache tank, the second cache tank and the third cache tank are all provided with transport pumps.
5. The high COD concentration wastewater treatment and recovery process in the PSPI production process according to claim 4, which is characterized in that: the second condenser is communicated with the catcher.
6. The high COD concentration wastewater treatment and recovery process in the PSPI production process according to claim 4, which is characterized in that: and the first rectifying tower is used for normal pressure rectification treatment, the temperature is 80-90 ℃, and the reflux ratio is 1.
7. The high COD concentration wastewater treatment and recovery process in the PSPI production process according to claim 4, which is characterized in that: and the second rectifying tower is used for reduced pressure distillation, the temperature is 60-75 ℃, the vacuum degree is 1mmHg, the reflux ratio is controlled to be 1.0-1.5 in a light fraction section, and the transition fraction section is controlled to be 2-3.
8. The high COD concentration wastewater treatment and recovery process in the PSPI production process according to claim 1, which is characterized in that: the content of NMP organic solvent in the oil phase storage tank is 80-90%.
9. The high COD concentration wastewater treatment and recovery process in the PSPI production process according to claim 1, which is characterized in that: the content of NMP organic solvent in the finished product tank is more than 99%.
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| CN202210093825.7A CN114409167A (en) | 2022-01-26 | 2022-01-26 | High COD concentration wastewater treatment and recovery process in PSPI production process |
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| CN202210093825.7A CN114409167A (en) | 2022-01-26 | 2022-01-26 | High COD concentration wastewater treatment and recovery process in PSPI production process |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4057491A (en) * | 1976-03-26 | 1977-11-08 | Exxon Research & Engineering Co. | Solvent recovery process for N-methyl-2-pyrrolidone in hydrocarbon extraction |
| CN211005207U (en) * | 2019-11-28 | 2020-07-14 | 黄山金石木塑料科技有限公司 | Polyimide solvent recovery and separation device |
| CN211645081U (en) * | 2019-11-18 | 2020-10-09 | 扬州瑞邦化工技术有限公司 | Novel EG is retrieved in succession device |
| US20210039963A1 (en) * | 2018-12-18 | 2021-02-11 | Lg Chem, Ltd. | Process for recovering amide compounds |
| CN112807732A (en) * | 2021-02-02 | 2021-05-18 | 常州冀德环保科技有限公司 | Three-tower two-effect rectification system and recovery method for NMP waste liquid |
-
2022
- 2022-01-26 CN CN202210093825.7A patent/CN114409167A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4057491A (en) * | 1976-03-26 | 1977-11-08 | Exxon Research & Engineering Co. | Solvent recovery process for N-methyl-2-pyrrolidone in hydrocarbon extraction |
| US20210039963A1 (en) * | 2018-12-18 | 2021-02-11 | Lg Chem, Ltd. | Process for recovering amide compounds |
| CN211645081U (en) * | 2019-11-18 | 2020-10-09 | 扬州瑞邦化工技术有限公司 | Novel EG is retrieved in succession device |
| CN211005207U (en) * | 2019-11-28 | 2020-07-14 | 黄山金石木塑料科技有限公司 | Polyimide solvent recovery and separation device |
| CN112807732A (en) * | 2021-02-02 | 2021-05-18 | 常州冀德环保科技有限公司 | Three-tower two-effect rectification system and recovery method for NMP waste liquid |
Non-Patent Citations (1)
| Title |
|---|
| 马建标等: "《功能高分子材料》", 化学工业出版社 * |
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