CN112456710A - Method for recycling high-value materials from chemical wastewater - Google Patents
Method for recycling high-value materials from chemical wastewater Download PDFInfo
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- CN112456710A CN112456710A CN202011290730.1A CN202011290730A CN112456710A CN 112456710 A CN112456710 A CN 112456710A CN 202011290730 A CN202011290730 A CN 202011290730A CN 112456710 A CN112456710 A CN 112456710A
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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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
- C02F1/048—Purification of waste water by 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
The invention belongs to the technical field of environmental protection wastewater treatment, and particularly relates to a method for recycling high-value materials from chemical wastewater, which at least comprises the following steps: the method comprises the steps of adjusting the pH of original wastewater, performing primary membrane separation treatment on the wastewater after the pH adjustment, performing secondary membrane separation treatment on filtrate, combining secondary membrane concentrated solution and primary membrane concentrated solution, performing pre-precipitation, removing sludge for dehydration, performing tertiary membrane separation treatment on secondary membrane filtrate, performing evaporation and concentration on tertiary membrane concentrated solution, and drying the concentrated solution after the evaporation and concentration to obtain an organic phase product. And (3) removing the resin adsorption process from the third-stage membrane filtrate for adsorption, removing the fourth-stage membrane process from the filtrate after adsorption for concentration, removing evaporation crystals from the filtrate after the filtrate is subjected to fourth-stage membrane concentration to obtain semisolid strong brine, and removing centrifugal separation from the strong brine to obtain solid salt. The process can ensure that 100 percent of wastewater reaches the standard and is discharged, more than 95 percent of valuable materials in the wastewater can be recovered, the purity of the recovered materials can reach more than 90 percent, and the recovered inorganic salt is solid sodium chloride.
Description
Technical Field
The invention belongs to the technical field of environmental protection wastewater treatment, and particularly relates to a method for recycling high-value materials from chemical wastewater.
Background
The waste water related to the field of environmental protection waste water treatment belongs to waste water with high salt content and high COD, which generally contains pyridine and inorganic salt (such as ammonium sulfate, ammonium chloride and sodium chloride), the COD content of the waste water is 20000-60000 mg/L, the TDS content is 5-12%, the pyridine in the waste water is a dangerous product which is easy to cause cancer, but simultaneously the pyridine is a medical intermediate, is a necessary substance in a plurality of chemical synthesis products, has very high economic value, is a high-value material, can generate very high economic benefit when being reasonably recycled, and needs higher disposal cost when the waste water is treated. The disposal methods in the prior art mainly include the following methods: firstly, the evaporation technology: directly evaporating the wastewater, changing mother liquor into dangerous wastewater, and discharging the condensate after the condensate is treated by a wastewater treatment system (biochemical treatment) to reach the standard; secondly, resin adsorption technology: adsorbing organic matters in the wastewater by using resin, then evaporating and drying the filtrate after the resin is adsorbed, discharging the condensate, and delivering the mother liquor to a hazardous waste treatment company for disposal. Thirdly, an extraction technology: extracting with chloroform or cyclohexane as extractant, and distilling the extractive liquid.
However, these three methods all have their own disadvantages:
the conventional evaporation technology generates an azeotropic phenomenon in the treatment process, either pyridine is completely carried into a condensate liquid, and a mother solution is evaporated to dryness, or evaporation cannot be carried out at all, and cannot be carried out due to boiling. The condensate liquid is treated by waste water, higher treatment cost is needed, the solid waste belongs to dangerous waste, and the solid waste needs to be treated by qualified dangerous waste treatment companies, and higher treatment cost (4500 yuan/ton) is also needed; after the conventional resin adsorption treatment, the filtrate is evaporated to generate hazardous waste; the extraction process is long in time consumption, generally needs 20-40 hours, is low in efficiency, expensive in extractant price and large in extractant loss, and meanwhile, the extractant is also a toxic substance and is easy to generate hazardous waste.
In view of the above, the invention provides a method for recycling high-value materials from chemical wastewater, which realizes a treatment method for wastewater treatment to reach discharge standards or recycle by recycling material components with high economic values in wastewater, and realizes pollution control by waste nutrient and green.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the method for recycling the high-value materials from the chemical wastewater is provided, and the treatment method for the standard discharge or recycling of the wastewater is realized by recycling the material components with high economic values in the wastewater, so that the pollution control by the waste nutrient and the green pollution control are realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for recycling high-value materials from chemical wastewater at least comprises the following steps:
firstly, adjusting the pH of original wastewater, performing primary membrane separation treatment on the wastewater after the pH adjustment, and sending filtrate subjected to the primary membrane separation treatment into secondary membrane separation treatment;
step two, the concentrated solution obtained by the secondary membrane separation treatment is merged with the concentrated solution obtained by the primary membrane separation treatment and then sent to sludge dehydration treatment, and the filtrate obtained by the secondary membrane separation treatment is sent to the tertiary membrane separation treatment;
and thirdly, carrying out evaporation concentration process treatment on the concentrated solution generated by the three-stage membrane separation by adopting a negative-pressure single-effect forced circulation evaporation process, and sending the obtained concentrated solution into a drying process for treatment to obtain an organic phase product to be recovered.
As an improvement of the method for recycling high-value materials from chemical wastewater, the method also comprises the fourth step of: and (3) the penetrating fluid generated by the three-stage membrane separation is sent to a resin adsorption process for adsorption treatment, the filtrate generated by the resin adsorption process is sent to a four-stage membrane concentration process for treatment, the analytic solution generated by the resin adsorption process is collected and sent to a raw water tank for secondary repeated treatment, and the rinsing water generated by the resin adsorption process is collected as the maintainable water of the system.
As an improvement of the method for recycling high-value materials from chemical wastewater, the method also comprises the fifth step of: and (3) carrying out evaporative crystallization salt separation treatment on the concentrated solution generated by the four-stage membrane concentration process by adopting a negative pressure triple effect evaporation process, sending the obtained salt water mixed solution into centrifugal separation, obtaining inorganic phase solid salt after the centrifugal separation, directly discharging or recycling penetrating fluid generated by the four-stage membrane treatment, and removing ammonia nitrogen from condensed water generated by the evaporation process by adopting an ion exchange process.
As an improvement of the method for recycling high-value materials from chemical wastewater, the pH value of the original wastewater is adjusted by hydrochloric acid in the first step, and the adjusted pH value is 7-8.
As an improvement of the method for recycling high-value materials from chemical wastewater, the concentrated solution after the second step of confluence is pretreated by a tubular ultrafiltration membrane device (an organic tubular membrane and an inorganic tubular membrane), and the separated concentrated solution is subjected to sludge dehydration treatment; the second step of the second-stage membrane separation treatment process adopts a nanofiltration membrane to intercept macromolecular organic matters and chromaticity in the first-stage membrane treatment filtrate and allow the micromolecular organic matters and inorganic salts to permeate.
As an improvement of the method for recycling high-value materials from chemical wastewater, a nanofiltration membrane capable of intercepting small molecules is adopted in the third-level membrane separation treatment process, and the drying process is a spiral drying process.
As an improvement of the method for recycling high-value materials from chemical wastewater, the fourth-stage membrane concentration process adopts a seawater desalination membrane to concentrate filtrate generated by the resin adsorption process, so that the concentration of inorganic salts in the wastewater is increased.
In the third step, the concentrated solution generated by the three-stage membrane treatment is washed by pure water for 2-3 times in equal proportion, and then is subjected to evaporation concentration process treatment to reduce the inorganic phase content of the recovered target substance (organic substance).
As an improvement of the method for recycling high-value materials from chemical wastewater, the original wastewater is further treated as follows before the pH is adjusted: and (2) feeding the raw wastewater into a wastewater collecting pool provided with a submersible stirrer, feeding the raw wastewater into a raw water tank through a wastewater lifting pump after stirring, feeding the raw wastewater into an ultrafiltration device, and feeding the filtrate obtained by ultrafiltration into a pH adjusting tank for pH adjustment.
As an improvement of the method for recycling high-value materials from chemical wastewater, if the wastewater contains phosphorus, the wastewater is firstly sent into a reaction tank added with calcium oxide from a raw water tank before being sent into an ultrafiltration device, and then is sent into the ultrafiltration device after reaction; and (4) feeding the concentrated solution obtained by ultrafiltration into a sludge concentration tank, and carrying out dehydration by a screw stacking machine to transport the sludge outside.
Compared with the prior art, the process can ensure that the wastewater reaches 100 percent and is discharged after reaching the standard, more than 95 percent of valuable materials in the wastewater can be recovered, the purity of the recovered materials can reach more than 90 percent, and the recovered inorganic salt is solid sodium chloride (the water content is less than or equal to 3 percent). The whole process has the advantages of high treatment efficiency, stable operation, low treatment cost, maximum recovery of valuable materials in the wastewater, realization of maximum benefit of projects and reduction of discharge. The invention realizes the treatment method of up-to-standard discharge or reuse of the wastewater by recovering the material components with high economic value in the wastewater, and realizes the treatment of the wastewater by waste nutrient and green.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a process flow diagram of a pretreatment process in the present invention.
Detailed Description
As shown in figure 1, the invention provides a method for recycling high-value materials from chemical wastewater, which at least comprises the following steps:
a method for recycling high-value materials from chemical wastewater at least comprises the following steps:
firstly, adjusting the pH of original wastewater, performing primary membrane separation treatment on the wastewater after the pH adjustment, and sending filtrate subjected to the primary membrane separation treatment into secondary membrane separation treatment;
step two, the concentrated solution obtained by the secondary membrane separation treatment is merged with the concentrated solution obtained by the primary membrane separation treatment and then sent to sludge dehydration treatment, and the filtrate obtained by the secondary membrane separation treatment is sent to the tertiary membrane separation treatment;
and thirdly, carrying out evaporation concentration process treatment on the concentrated solution generated by the three-stage membrane separation by adopting a negative-pressure single-effect forced circulation evaporation process, and sending the obtained concentrated solution into a drying process for treatment to obtain an organic phase product to be recovered.
The method further comprises a fourth step of: and (3) the penetrating fluid generated by the three-stage membrane separation is sent to a resin adsorption process for adsorption treatment, the filtrate generated by the resin adsorption process is sent to a four-stage membrane concentration process for treatment, the analytic solution generated by the resin adsorption process is collected and sent to a raw water tank for secondary repeated treatment, and the rinsing water generated by the resin adsorption process is collected as the maintainable water of the system.
The method further comprises a fifth step of: and (3) carrying out evaporative crystallization salt separation treatment on the concentrated solution generated by the four-stage membrane concentration process by adopting a negative pressure triple effect evaporation process, sending the obtained salt water mixed solution into centrifugal separation, obtaining inorganic phase solid salt after the centrifugal separation, directly discharging or recycling penetrating fluid generated by the four-stage membrane treatment, and removing ammonia nitrogen from condensed water generated by the evaporation process by adopting an ion exchange process.
In the first step, hydrochloric acid is adopted to adjust the pH value of the original wastewater, and the adjusted pH value is 7-8.
Pretreating the concentrated solution after the second step by adopting a tubular ultrafiltration membrane device (an organic tubular membrane and an inorganic tubular membrane), and dehydrating the separated concentrated solution; the second step of the second-stage membrane separation treatment process adopts a nanofiltration membrane to intercept macromolecular organic matters and chromaticity in the first-stage membrane treatment filtrate and allow the micromolecular organic matters and inorganic salts to permeate.
In the third step, a nanofiltration membrane capable of intercepting small molecules is adopted in the three-stage membrane separation treatment process, and the drying process in the third step is a spiral drying process.
And in the fourth step, the four-stage membrane concentration process adopts a seawater desalination membrane to concentrate the filtrate generated by the resin adsorption process, so that the concentration of inorganic salts in the wastewater is improved.
In the third step, the concentrated solution generated by the three-stage membrane treatment is washed by pure water for 2-3 times in equal proportion, and then is treated by an evaporation concentration process to reduce the inorganic phase content of the recovered target substance (organic substance).
As shown in fig. 2, the raw wastewater was treated as follows before pH adjustment (pretreatment step): and (2) feeding the raw wastewater into a wastewater collecting pool provided with a submersible stirrer, feeding the raw wastewater into a raw water tank through a wastewater lifting pump after stirring, feeding the raw wastewater into an ultrafiltration device, and feeding the filtrate obtained by ultrafiltration into a pH adjusting tank for pH adjustment. If the waste water contains phosphorus, the waste water is firstly sent into a reaction tank added with calcium oxide from a raw water tank before being sent into the ultrafiltration device, and then is sent into the ultrafiltration device after reaction. And (4) feeding the concentrated solution obtained by ultrafiltration into a sludge concentration tank, and transporting the sludge outside through a screw stacking machine.
The process can ensure that 100 percent of wastewater reaches the standard and is discharged, more than 95 percent of valuable materials in the wastewater can be recovered, the purity of the recovered materials can reach more than 90 percent, and the recovered inorganic salt is solid sodium chloride (the water content is less than or equal to 3 percent). The process is characterized in that: the treatment is efficient, the operation is stable, the treatment cost is low, valuable materials in the wastewater are recycled to the maximum extent, the project maximum benefit is realized, and the emission is reduced.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. A method for recycling high-value materials from chemical wastewater is characterized by at least comprising the following steps:
firstly, adjusting the pH of original wastewater, performing primary membrane separation treatment on the wastewater after the pH adjustment, and sending filtrate subjected to the primary membrane separation treatment into secondary membrane separation treatment;
step two, the concentrated solution obtained by the secondary membrane separation treatment is merged with the concentrated solution obtained by the primary membrane separation treatment and then sent to sludge dehydration treatment, and the filtrate obtained by the secondary membrane separation treatment is sent to the tertiary membrane separation treatment;
and thirdly, carrying out evaporation concentration process treatment on the concentrated solution generated by the three-stage membrane separation by adopting a negative-pressure single-effect forced circulation evaporation process, and sending the obtained concentrated solution into a drying process for treatment to obtain an organic phase product to be recovered.
2. The method for recycling high-value materials from chemical wastewater as claimed in claim 1, wherein the method further comprises a fourth step of: and (3) the penetrating fluid generated by the three-stage membrane separation is sent to a resin adsorption process for adsorption treatment, the filtrate generated by the resin adsorption process is sent to a four-stage membrane concentration process for treatment, the analytic solution generated by the resin adsorption process is collected and sent to a raw water tank for secondary repeated treatment, and the rinsing water generated by the resin adsorption process is collected as the maintainable water of the system.
3. The method for recycling high-value materials from chemical wastewater as claimed in claim 2, wherein the method further comprises a fifth step of: and (3) carrying out evaporative crystallization salt separation treatment on the concentrated solution generated by the four-stage membrane concentration process by adopting a negative pressure triple effect evaporation process, sending the obtained salt water mixed solution into centrifugal separation, obtaining inorganic phase solid salt after the centrifugal separation, directly discharging or recycling penetrating fluid generated by the four-stage membrane treatment, and removing ammonia nitrogen from condensed water generated by the evaporation process by adopting an ion exchange process.
4. The method for recycling high-value materials from chemical wastewater as claimed in claim 1, wherein in the first step, the pH value of the original wastewater is adjusted by hydrochloric acid, and the adjusted pH value is 7-8.
5. The method for recycling high-value materials from chemical wastewater as resources according to claim 1, wherein the concentrated solution merged in the second step is pretreated by using a tubular ultrafiltration membrane device, and the separated concentrated solution is subjected to sludge dehydration treatment; the second step of the second-stage membrane separation treatment process adopts a nanofiltration membrane to intercept macromolecular organic matters and chromaticity in the first-stage membrane treatment filtrate and allow the micromolecular organic matters and inorganic salts to permeate.
6. The method for recycling high-value materials from chemical wastewater as claimed in claim 1, wherein a nanofiltration membrane capable of intercepting small molecules is adopted in the third step of the three-stage membrane separation treatment process, and the third step of the drying process is a spiral drying process.
7. The method for recycling high-value materials from chemical wastewater as claimed in claim 2, wherein the fourth step of the four-stage membrane concentration process is to concentrate the filtrate generated by the resin adsorption process by using a seawater desalination membrane, so as to increase the concentration of inorganic salts in the wastewater.
8. The method for recycling high-value materials from chemical wastewater as claimed in claim 1, wherein in the third step, the concentrated solution generated by the three-stage membrane treatment is washed with pure water for 2-3 times in equal proportion, and then treated by an evaporation concentration process to reduce the inorganic phase content of the recycled target substances.
9. The method for recycling high-value materials from chemical wastewater as claimed in claim 1, wherein the raw wastewater is further treated as follows before the pH is adjusted: and (2) feeding the raw wastewater into a wastewater collecting pool provided with a submersible stirrer, feeding the raw wastewater into a raw water tank through a wastewater lifting pump after stirring, feeding the raw wastewater into an ultrafiltration device, and feeding the filtrate obtained by ultrafiltration into a pH adjusting tank for pH adjustment.
10. The method for recycling high-value materials from chemical wastewater as claimed in claim 9, wherein if the wastewater contains phosphorus, the wastewater is fed from a raw water tank to a reaction tank containing calcium oxide before being fed to the ultrafiltration device, and then fed to the ultrafiltration device after reaction; and (4) feeding the concentrated solution obtained by ultrafiltration into a sludge concentration tank, and carrying out dehydration by a screw stacking machine to transport the sludge outside.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113666559A (en) * | 2021-08-10 | 2021-11-19 | 广西贵港市蓝月亮水处理环保科技有限公司 | Method for recovering high-value organic materials from high-salt high-COD wastewater |
| CN113860669A (en) * | 2021-11-10 | 2021-12-31 | 广州兰德环保资源科技有限公司 | Method for recycling cellulose ether production wastewater |
| CN115520934A (en) * | 2021-06-25 | 2022-12-27 | 中国石油化工股份有限公司 | Membrane separation recovery system and method |
| CN115608135A (en) * | 2022-10-08 | 2023-01-17 | 湖北泰盛化工有限公司 | Self-consistent type resource treatment method for salt-containing wastewater and hydrochloric acid-containing waste gas |
-
2020
- 2020-11-18 CN CN202011290730.1A patent/CN112456710A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115520934A (en) * | 2021-06-25 | 2022-12-27 | 中国石油化工股份有限公司 | Membrane separation recovery system and method |
| CN115520934B (en) * | 2021-06-25 | 2024-05-03 | 中国石油化工股份有限公司 | Membrane separation recovery system and method |
| CN113666559A (en) * | 2021-08-10 | 2021-11-19 | 广西贵港市蓝月亮水处理环保科技有限公司 | Method for recovering high-value organic materials from high-salt high-COD wastewater |
| CN113860669A (en) * | 2021-11-10 | 2021-12-31 | 广州兰德环保资源科技有限公司 | Method for recycling cellulose ether production wastewater |
| CN115608135A (en) * | 2022-10-08 | 2023-01-17 | 湖北泰盛化工有限公司 | Self-consistent type resource treatment method for salt-containing wastewater and hydrochloric acid-containing waste gas |
| CN115608135B (en) * | 2022-10-08 | 2023-05-12 | 湖北泰盛化工有限公司 | Self-consistent recycling treatment method for salt-containing wastewater and hydrochloric acid-containing waste gas |
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