CN107473478B - Recycling treatment process for process wastewater generated in wet-process preparation of brominated butyl rubber - Google Patents
Recycling treatment process for process wastewater generated in wet-process preparation of brominated butyl rubber Download PDFInfo
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- C02F9/00—Multistage treatment of water, waste water or sewage
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- 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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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/24—Treatment of water, waste water, or sewage by flotation
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- 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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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- 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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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
Abstract
The invention relates to a process for recycling process wastewater of a process for preparing brominated butyl rubber by a wet method, which treats the process wastewater of the process for preparing the brominated butyl rubber by the wet method by combining pretreatment, a membrane integration technology and evaporative crystallization, and effectively realizes the purposes of zero emission and recycling after the wastewater is treated.
Description
Technical Field
The invention belongs to the field of wastewater treatment, and particularly relates to a process for recycling wastewater from a wet-process preparation process of brominated butyl rubber.
Background
Brominated butyl rubber (BIIR for short) is prepared by reacting bromine with hexane solution of butyl rubber, has excellent characteristics of heat resistance, corrosion resistance, ozone resistance, low air permeability, flex resistance, easy combination with other rubbers to form a co-crosslinking structure and the like, is widely applied to various rubber products, and is an irreplaceable raw material for manufacturing a radial tire inner tube and a tubeless tire. In recent years, due to the vigorous development of downstream tires and automobile industries, especially radial tires, the demand of domestic brominated butyl rubber is increasing day by day, so that the investment of enterprises on brominated butyl rubber production devices is increased. However, in the wet process of preparing brominated butyl rubber, deionized water is used for washing the product to meet the product quality requirement, so that a certain amount of rubber wastewater is generated. On one hand, the direct discharge of rubber wastewater does not accord with the sustainable development policy of the environment, and on the other hand, the rubber wastewater belongs to the waste of water resources in water-deficient areas in China. Therefore, the brominated butyl rubber production device is matched with rubber wastewater zero emission and wastewater recycling projects, economic benefits and social benefits are realized, the environment and resources are perfectly combined, and the brominated butyl rubber production device is the key for sustainable development of the brominated butyl rubber production industry in China.
The waste water discharged by the process for preparing the brominated butyl rubber by the wet method is mainly characterized in that:
(1) the waste water contains a certain amount of suspended substances such as rubber powder, stearate and the like;
(2) the waste water contains organic substances such as hexane, alkylphenol, epoxidized soybean oil and other hydrocarbons;
(3) the wastewater has high salt content and concentration and contains strong corrosive bromine ions.
At present, the processes for treating the bromine-containing rubber wastewater mainly comprise the following steps:
(1) oxidizing bromine ions in the wastewater into bromine by using chlorine and hydrogen peroxide, and then separating the bromine from the wastewater. Although the method can recover bromine in the wastewater, the method also has the disadvantages of long process flow, high equipment requirement (strong bromine corrosivity) and the like.
(2) Concentrating the bromine-containing wastewater, mixing with a chlorine-containing bactericide, and adding into industrial circulating cooling water for sterilization treatment. Although the method can achieve the effect of recycling the wastewater, substances such as suspended matters, hardness and the like in the wastewater easily pollute equipment, and part of finally discharged circulating wastewater is difficult to treat.
Aiming at the characteristics of the waste water, the invention couples the pretreatment technology, the membrane concentration technology and the evaporation technology in the current waste water treatment process to form a set of integrated treatment process with reasonable economic technology, and finally realizes zero emission and resource recycling of the waste water produced in the production of the brominated butyl rubber.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a process for recycling process wastewater generated in a process of preparing brominated butyl rubber by a wet method, and the process realizes zero emission and resource utilization of the production wastewater generated in the process of preparing the brominated butyl rubber by the wet method.
The invention adopts the following scheme: a process for recycling process wastewater generated in a process of preparing brominated butyl rubber by a wet method comprises the following processing steps:
(1) discharging the wastewater into a regulating water tank and staying for more than 8 hours for regulating the water quality and the water quantity;
(2) adjusting the water outlet of the water tank to enter a nano dissolved air flotation unit, and adding 7-10ppm of PAC and 0.1-0.5ppm of PAM for removing most of hexane, alkylphenol, rubber powder and stearate in the wastewater;
(3) the effluent of the nanometer dissolved air flotation unit enters a multi-medium filtering unit and an ultrafiltration unit and is used for removing most suspended matters, colloids, bacteria and part of macromolecular organic matters in the water;
(4) the water produced by the ultrafiltration unit enters an ion exchange unit which is used for reducing Ca in the water2+Concentration, preventing calcium sulfate scaling of a subsequent reverse osmosis and reverse electrodialysis device;
(5) the effluent of the ion exchange unit enters a reverse osmosis unit, is separated into produced water and concentrated water under the action of a reverse osmosis membrane, the produced water reaches the quality of water for wet process production of the brominated butyl rubber and is reused for process production, and the concentrated water enters a reverse electrode electrodialysis unit after being collected;
(6) the wastewater enters a reverse osmosis electrodialysis unit, the salt concentration in the reverse osmosis unit is further improved through the action of an anion exchange membrane and a cation exchange membrane in electrodialysis to form high-concentration salt water, the high-concentration salt water enters an evaporation unit, meanwhile, the reverse osmosis electrodialysis unit can also form desalted light salt water, and the desalted light salt water enters the reverse osmosis unit to be combined;
(7) and (3) enabling concentrated water concentrated by the reverse electrodialysis unit to enter an evaporation crystallization unit to finally form solid salt, and combining condensate in the evaporation crystallization process and reverse osmosis produced water for producing brominated butyl rubber.
Preferably, the amount of PAM in step (2) is 0.2 ppm.
Preferably, the residence time of the nano dissolved air floatation in the step (2) is 1-2 h.
Preferably, the recovery rate of the ultrafiltration system in the step (3) is set to be 90-95%, and PVDF is preferably used as the membrane material.
Preferably, in the step (5), the reverse osmosis unit adopts a three-stage operation mode, the recovery rate is 80-85%, and the operating pH value is 7.5-8.
Preferably, the reversed electrodialysis in the step (6) is used for increasing the mass concentration of the bromine salt in the wastewater to more than 15%.
Compared with the prior art, the treatment process has the following beneficial effects:
(1) the brominated butyl rubber production wastewater is treated by combining pretreatment, membrane integration technology and evaporative crystallization, and bromine salt raw materials extracted by bromine and rubber production process water are finally formed by combined action while respective process steps play a role, so that the zero emission of the wastewater is realized, and the targets of reclaimed water recycling and salt resource recycling are realized;
(2) the reversed electrodialysis process is adopted as the wastewater re-concentration process, so that the defect that the bromine-containing wastewater is easy to corrode metal pipeline equipment under the high-pressure condition is overcome, and the treatment process is more reliable;
(3) the reverse osmosis process adopts a three-stage operation mode and operates under the condition of high pH value, so that the pollution of a reverse osmosis membrane can be reduced;
(4) the nano dissolved air flotation process is adopted as the pretreatment process of the whole integrated process, so that pollutants such as hexane, alkylphenol, rubber powder, stearate and the like can be effectively removed, the process is mature and simple, and the removal effect is good.
Drawings
The following further description is made with reference to the accompanying drawings:
FIG. 1 is a flow chart of the resource treatment process of waste water from production of brominated butyl rubber.
Detailed Description
The invention will be further illustrated with reference to the following examples:
example 1
The waste water from the wet preparation of brominated butyl rubber from a certain company is used as raw water in the present example, and the specific inlet water quality data are shown in tables 1 and 2.
TABLE 1 analysis table for effluent-water quality
TABLE 2 external drainage secondary water quality analysis meter
(1) Discharging the wastewater into a regulating water tank and staying for 8 hours for regulating the water quality and the water quantity;
(2) adjusting the water outlet of the water tank to enter a nano dissolved air flotation unit, keeping the water tank for 2 hours, adding 7-10ppm of PAC and 0.2ppm of PAM in the air flotation process, and removing the COD by 60-80%;
(3) the effluent of the nano dissolved air flotation unit enters a multi-medium filtering unit and an ultrafiltration unit, the water recovery rate of the ultrafiltration unit system is 90 percent, and the flux of a working membrane is less than or equal to 50/(m)2H), quality of produced water SDI<3；
(4) The ultrafiltration produced water enters an ion exchange unit which is used for reducing Ca in the water2+Concentration, preventing calcium sulfate scaling of a subsequent reverse osmosis and reverse electrodialysis device;
(5) the effluent of the ion exchange unit enters a reverse osmosis unit, the reverse osmosis adopts a 5-core three-section design, two-section pressurization and three-section internal circulation are adopted, the recovery rate is set to be 80 percent, the produced water is used for process production, the concentrated water enters a reverse electrode electrodialysis unit after being collected, and the quality of the produced water (namely the reuse water) is shown in the following table;
TABLE 3 quality of reuse water
(6) The wastewater enters a reverse electrodialysis unit, the reverse electrodialysis unit operates in a mode of connecting an out-of-phase anion exchange membrane, a cation exchange membrane and two stages in series, the salt concentration of reverse electrodialysis concentrated water can reach 15%, high-concentration salt water is formed and enters an evaporation unit, meanwhile, the reverse electrodialysis unit can also form desalted light salt water, and the desalted light salt water enters a reverse osmosis unit for combination treatment;
(7) and (3) enabling concentrated water concentrated by the reverse electrodialysis unit to enter an evaporation crystallization unit to finally form solid salt, and combining condensate in the evaporation crystallization process and reverse osmosis produced water for producing brominated butyl rubber.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (3)
1. A process for recycling process wastewater generated in a process of preparing brominated butyl rubber by a wet method is characterized by comprising the following processing steps:
(1) discharging the wastewater into a regulating water tank and staying for more than 8 hours for regulating the water quality and the water quantity;
(2) adjusting the water outlet of the water tank to enter a nano dissolved air flotation unit, and adding 7-10ppm of PAC and 0.1-0.5ppm of PAM for removing most of hexane, alkylphenol, rubber powder and stearate in the wastewater; the PAM in the step (2) is 0.2 ppm; the retention time of the nano dissolved air flotation in the step (2) is 1-2 h;
(3) the effluent of the nanometer dissolved air flotation unit enters a multi-medium filtering unit and an ultrafiltration unit and is used for removing most suspended matters, colloids, bacteria and part of macromolecular organic matters in the water;
(4) the water produced by the ultrafiltration unit enters an ion exchange unit which is used for reducing Ca in the water2+Concentration, preventing calcium sulfate scaling of a subsequent reverse osmosis and reverse electrodialysis device;
(5) the effluent of the ion exchange unit enters a reverse osmosis unit, is separated into produced water and concentrated water under the action of a reverse osmosis membrane, the produced water reaches the quality of water for wet process production of the brominated butyl rubber and is reused for process production, and the concentrated water enters a reverse electrode electrodialysis unit after being collected; in the step (5), the reverse osmosis unit adopts a three-stage operation mode, the recovery rate is 80-85%, and the operating pH value is 7.5-8;
(6) the wastewater enters a reverse osmosis electrodialysis unit, the salt concentration in the reverse osmosis unit is further improved through the action of an anion exchange membrane and a cation exchange membrane in electrodialysis to form high-concentration salt water, the high-concentration salt water enters an evaporation unit, meanwhile, the reverse osmosis electrodialysis unit can also form desalted light salt water, and the desalted light salt water enters the reverse osmosis unit to be combined;
(7) and (3) enabling concentrated water concentrated by the reverse electrodialysis unit to enter an evaporation crystallization unit to finally form solid salt, and combining condensate in the evaporation crystallization process and reverse osmosis produced water for producing brominated butyl rubber.
2. The process according to claim 1, wherein the recovery rate of the ultrafiltration system in step (3) is set to 90% to 95%, and the membrane material is preferably PVDF.
3. The process of claim 1, wherein the reverse electrodialysis in step (6) is used to increase the bromine salt mass concentration in the wastewater to above 15%.
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| CN110606607B (en) * | 2018-06-14 | 2021-11-19 | 中国石油化工股份有限公司 | Method for recovering bromine from brominated butyl rubber industrial wastewater |
| CN110606592B (en) * | 2018-06-14 | 2021-10-19 | 中国石油化工股份有限公司 | Comprehensive utilization method of brominated butyl rubber bromine-containing wastewater |
| CN114477568B (en) * | 2020-10-23 | 2023-05-12 | 中国石油化工股份有限公司 | Method for recycling bromine-containing wastewater |
| CN114477567B (en) * | 2020-10-23 | 2023-05-30 | 中国石油化工股份有限公司 | Method for treating sodium bromide wastewater |
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