CN114477641A - Treatment method of comprehensive sewage of fine chemical industry park - Google Patents
Treatment method of comprehensive sewage of fine chemical industry park Download PDFInfo
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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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- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
- C02F3/12—Activated sludge processes
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- C02F3/1268—Membrane bioreactor systems
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Abstract
The invention discloses a treatment method of comprehensive sewage of a fine chemical industry park, belonging to the technical field of sewage treatment and environmental protection. The treatment method is a combined process of a plurality of units, and mainly comprises the following steps: the device comprises a front-section iron-carbon micro-electrolysis unit, a composite hydrolysis acidification unit, a composite biochemical treatment unit, a rear-section iron-carbon micro-electrolysis unit and a deep treatment unit. The invention has reasonable process combination, high impact load resistance, strong treatment capacity and stable and standard effluent quality, and is suitable for the treatment of comprehensive sewage in fine chemical industry parks, such as pesticide chemical wastewater, dye and pigment chemical wastewater, essence and spice chemical wastewater, cosmetic and health care product wastewater, food and feed additive wastewater, daily chemical wastewater, and production and domestic sewage mixed with the wastewater.
Description
Technical Field
The invention relates to a treatment method of industrial sewage, in particular to a treatment method of comprehensive sewage of a fine chemical industry park, belonging to the technical field of environmental protection.
Background
Fine chemistry is one of the most active emerging fields in the chemical industry today and is an important component of new materials. The fine chemical industry has wide range and various varieties, comprises about 40 industries such as dye, pesticide, pharmacy, spice, coating, photosensitive material, daily chemical industry and the like, has various product varieties, high added value, wide application and high industrial relevance, and directly serves various industries of national economy and various fields of high and new technology industries. The rapid development of fine chemical engineering has become the strategic focus of adjusting the chemical industry structure, improving the energy level of the chemical industry and expanding the economic benefit in all countries in the world. There are various methods for classifying fine chemical wastewater. Pharmaceutical wastewater, pesticide wastewater, dye wastewater, daily chemical wastewater and the like are classified according to the industry; if the pollutant types contained in the wastewater are classified, hydrocarbon wastewater, halocarbon wastewater, alcohol-containing wastewater, aldehyde-containing wastewater, ketone-containing wastewater, hydroxy acid wastewater, phenol-containing wastewater, amide wastewater, nitrile-containing wastewater, nitro wastewater, amine wastewater, organic sulfur wastewater, organic phosphorus wastewater, heterocyclic compound wastewater, polyvinyl alcohol wastewater, ammonia nitrogen wastewater, salt-containing wastewater and the like are contained; if the wastewater is classified according to water quality or biodegradability, the wastewater can be classified into solvent type wastewater, high-concentration biodegradable wastewater, low-concentration biodegradable wastewater, high-concentration nonbiodegradable wastewater, low-concentration nonbiodegradable wastewater, wastewater containing toxic and harmful substances and the like. The fine chemical wastewater has the following water quality characteristics: high pollutant content, high COD value, more substances difficult to be biodegraded, high chroma of colored wastewater and high ammonia nitrogen concentration. Most pollutants in the fine chemical wastewater are organic substances with complex structures, toxicity, harm and difficult biodegradation, the treatment difficulty is high, the cost is high, the wastewater is typical toxic and difficult-to-degrade industrial organic wastewater, the wastewater has the characteristics of high COD, high ammonia nitrogen, high chromaticity and the like, the main components harmful to microorganisms comprise COD, ammonia nitrogen, partial heavy metal ions, dyes, decomposers thereof and the like, the biological system has a serious inhibition effect, and the wastewater is a main reason for causing the effluent to not reach the standard. The treatment principle of the fine chemical wastewater is to adopt a production process without public hazard or with less public hazard as far as possible. Most of organic chemical wastewater is treated by adopting a biochemical technology, the wastewater needs to be pretreated before the treatment, the adverse factors to the biochemical treatment are eliminated, the biochemical treatment capacity is improved, appropriate process parameters are selected, a facultative stage is added before the aerobic treatment, or a filler is added at the rear section of a regulating tank, so that the biochemical performance of the wastewater is improved.
The industrial park is a modern industrial division cooperative production area which is suitable for market competition and industrial upgrading and is formed by dividing a region by a national or regional government through an administrative means according to the internal requirements of economic development per se, gathering various production elements, scientifically integrating the production elements in a certain space range, improving the intensive strength of industrialization, highlighting industrial characteristics and optimizing functional layout. As one type of industrial parks, the fine chemical industry park has complex industrial structure, large change of the quality and the quantity of wastewater, high concentration of pollutants, multiple types of pollutants and toxic and difficult degradation characteristics, and in order to prevent the fine chemical industry park from becoming a serious pollution area, the water pollution technology innovation must be enhanced, and the transformation from the traditional industrial park to the ecological industrial park is actively promoted.
The sewage of the fine chemical industry park mainly comes from sewage and waste liquid produced in the production process of a park factory, and mainly contains industrial production materials, intermediate products, pollutants and the like produced in the production process along with water loss, and domestic sewage produced by park production operators. Because of the various types of industries in industrial parks and the composition of each industry by multi-stage processes, the produced sewage has large property difference, high pollutant concentration, multiple pollutant types and the characteristics of toxicity and difficult degradation, the simple biological treatment process is difficult to meet the effluent quality requirement, and the sewage can be effectively treated by effectively combining physical, chemical and other methods with biological methods. Therefore, the proper treatment process is selected according to the water quality characteristics of the industrial park, and the optimal operation condition is determined, so that the treatment effect of the sewage of the industrial park is improved.
Chinese patent application 201310125484.8 discloses a fine chemical wastewater treatment and recycling method, and particularly relates to a fine chemical wastewater treatment and recycling method based on a Membrane Bioreactor (MBR) -Reverse Osmosis (RO) combined technology. The MBR system plays a role in starting and stopping, and because the MBR system has strict requirements on water quality, the fine chemical wastewater treated by conventional treatment means such as oil removal, air floatation, coagulation, hydrolysis, aerobic treatment and the like is easy to exceed the standard, so that the MBR system is broken down, while a Reverse Osmosis (RO) system needs to operate normally and obtain good effect, and the MBR system needs to provide excellent effluent quality.
Chinese patent application 201410129246.9 discloses a fine chemical wastewater treatment process, which comprises the steps of pre-oxidation treatment, hydrolytic acidification, biological treatment, activated blood sludge treatment, flocculation sedimentation and the like. The main process of the method comprises multi-stage and alternative biological treatment means such as a UASB anaerobic sludge expansion tank, an aerobic biofilter, a sludge membrane MBBR (moving bed biofilm reactor), activated sludge and the like, is not beneficial to fully exerting the advantages of biological treatment, and effluent water quality is poor and cannot be directly discharged into an external environment.
Chinese patent application 201510506359.0 discloses a chemical wastewater comprehensive treatment method, which comprises a pretreatment system, a primary biochemical system, an ozone treatment system, a secondary biochemical system and a primary post-treatment system, wherein the pretreatment system and the post-blowing system both use a large amount of coagulant and precipitator, and the operation cost is high.
Chinese patent application 201910406212.2 discloses a daily chemical wastewater treatment process, and specifically relates to flocculation, micro-electrolysis, Fenton oxidation, oxidation decolorization, desalination and other steps. The whole process of the method is the combination of physical and chemical treatment means, and does not relate to a biological treatment process, so a large amount of chemical reagents are needed, the operation cost is high, and the method is not beneficial to popularization and application.
Chinese patent application 202010718063.6 discloses a fine chemical wastewater treatment process, including handling a section of thick bamboo, the bottom fixedly connected with actuating mechanism who handles a section of thick bamboo, actuating mechanism extend to handle inside a section of thick bamboo, the internal rotation of handling a section of thick bamboo is connected with rabbling mechanism, and rabbling mechanism is connected with actuating mechanism. The method treats the chemical wastewater by physical and chemical means such as filtering, adding an oxidant and a flocculating agent, disinfecting and the like, and has the defects of large medicament consumption, large filter residue production and the like.
Chinese patent application 202110408860.9 discloses a fine chemical wastewater treatment process, which comprises the steps of pretreatment, carbon micro-electrolysis, flocculation precipitation, anaerobic treatment, hydrolytic acidification, contact oxidation, precipitation and the like. The method is the superposition of conventional treatment means, and the specific treatment effect is not described, while the fine chemical wastewater is a special wastewater, and can be improved on the basis of the conventional treatment means to obtain a better treatment effect.
Disclosure of Invention
The invention aims to provide a method for treating comprehensive sewage of a fine chemical industry park, which is used for treating the comprehensive sewage generated by the fine chemical industry park, such as pesticide chemical wastewater, dye and pigment chemical wastewater, essence and spice chemical wastewater, cosmetic and health care product wastewater, food and feed additive wastewater, daily chemical wastewater and mixed production and living wastewater. The water quality of the fine chemical engineering comprehensive sewage treated by the combined process reaches the GB 18918-2002 first-grade A standard.
Specifically, the technical scheme of the invention is realized as follows: a treatment method of comprehensive sewage of a fine chemical industry park comprises the following steps:
(1) front-end iron-carbon micro-electrolysis unit
Collecting various sewage in an industrial park, then discharging the sewage into an adjusting tank, configuring a submersible stirrer inside the adjusting tank, homogenizing the water quality and adjusting the water quantity of the sewage, then discharging the sewage into a front-section iron-carbon micro-electrolysis reaction tank, configuring an iron-carbon combined filler I inside the adjusting tank, adding concentrated sulfuric acid to control the pH value of the sewage to be 3-5, starting an aeration device to dissolve oxygen to be 2-4mg/L, after reacting for 4-6h, closing the aeration device, discharging the sewage into a neutralization flocculation tank I, adding liquid alkali to adjust the pH value of the sewage to be 8-9, adding a flocculating agent I, stirring and reacting for 1-2h, closing stirring, standing and precipitating for 1-2h, and discharging supernatant into the next unit;
(2) composite hydrolysis acidification unit
Discharging the sewage treated in the step (1) into a composite hydrolysis acidification reaction tank, configuring a submersible stirrer and biological suspension filler inside the tank, adding ferrous salt, light and bacteria into the tank, controlling the dissolved oxygen to be 0.5-1.0 mg/l, maintaining the hydraulic power for 24-36h, and discharging the supernatant into the next unit;
(3) composite biochemical treatment unit
Discharging the sewage treated in the step (2) into an enzyme-adding anaerobic tank, configuring a submersible stirrer inside the tank, adding compound biological enzyme into the anaerobic tank, controlling dissolved oxygen to be 0.1-0.3mg/L, performing anaerobic digestion on organic matters in the sewage for 15-20 hours, discharging supernatant into an enzyme-adding aerobic tank, configuring an aeration device inside the tank, adding a microbial accelerant into the aerobic tank, controlling dissolved oxygen to be 3-5mg/L, removing most of the organic matters and ammonia nitrogen in the sewage, controlling the reaction time to be 8-10 hours, discharging effluent into a settling tank for natural settling, and discharging the supernatant into the next unit;
(4) rear iron-carbon micro-electrolysis unit
Discharging the sewage treated in the step (3) into a rear-section iron-carbon micro-electrolysis unit, preparing an iron-carbon combined filler II inside the rear-section iron-carbon micro-electrolysis unit, adding concentrated sulfuric acid to control the pH value of the sewage to be 4-6, starting an aeration device to dissolve oxygen to be 2-4mg/L, after reacting for 6-8h, closing the aeration device, discharging the sewage into a neutralization flocculation tank II, adding liquid alkali to adjust the pH value of the sewage to be 8-9, adding a flocculating agent II, stirring and reacting for 1-2h, closing stirring, standing and precipitating for 1-2h, and discharging the supernatant into the next unit;
(5) deep processing unit
And (4) discharging the sewage treated in the step (4) into a membrane bioreactor, controlling the dissolved oxygen to be 3-4mg/L, and discharging the wastewater into a final sedimentation tank for natural sedimentation after aeration reaction for 4-8h so as to achieve the standard and discharge.
Further, in the step (1) of the present invention, the average particle size of the iron-carbon composite filler i is 5-8cm, the filling amount is 0.1-0.5 times of the volume of the sewage, the iron-carbon composite filler i is formed by combining the following components by mass ratio, and the iron powder: activated carbon powder: metal: dispersing agent: adhesive: catalyst ═ (30-40): (10-20): (5-10); (1-5): (1-5): (1-3), wherein the metal is one or a composition of copper powder, molybdenum powder and zinc powder, the dispersing agent is one or a composition of hydrated lime, sodium carbonate and calcium oxide, the binder is one or a composition of sodium silicate, diatomite and bentonite, and the catalyst is one or a composition of aluminum oxide, ammonium chloride and sodium borate. Furthermore, the iron-carbon combined filler I is prepared by the steps of adding water, mixing, extrusion molding, medium-temperature drying, high-temperature calcining, cooling molding and the like, wherein the medium-temperature drying is drying in an oven at the temperature of 80-120 ℃ for 12-24 hours, and the high-temperature calcining is calcining in a muffle furnace at the temperature of 800-1000 ℃ for 60-90 minutes by filling nitrogen.
Further, the flocculant I in the step (1) of the invention is prepared by combining the following components in percentage by mass: aluminum sulfate: sodium alginate: polyacrylamide ═ (15-20): (10-15); (6-10): (1-5), the adding amount of the flocculating agent I is 0.5-2.5mg/L, the concentrated sulfuric acid is added for multiple times, and the pH value is controlled to be 4-6 in the reaction process.
Further, the ferrous salt in the step (2) of the invention is one or a combination of ferrous sulfate, ferrous chloride and ferrous carbonate, the total adding amount of the ferrous salt is 0.3-0.5mg/L, and the photosynthetic bacteria are photosynthetic bacteria with the concentration of more than 109Per milliliter ofThe addition amount of the commercial photosynthetic bacteria bacterial suspension is 6-12 mg/L.
Furthermore, the anaerobic tank in the step (3) is one of an up-flow anaerobic sludge tank, a baffle plate anaerobic tank and a sequencing batch anaerobic tank, and the aerobic tank is one of a sequencing batch activated sludge tank, a biological contact oxidation tank and a circulating activated sludge tank. The compound biological enzyme is a composition of yeast, sodium acetate and urea, and the microbial accelerant is a composition of glucose, urea, zinc acetate, monopotassium phosphate and vitamin C. Furthermore, the adding amount of the compound biological enzyme is 3-5mg/L, and the mass ratio of the yeast: sodium acetate: urea (80-100): (6-10): (1-3), the adding amount of the microbial accelerant is 5-10mg/L, calculated by mass ratio, glucose: urea: zinc acetate: potassium dihydrogen phosphate: vitamin C ═ 50-100: (3-6): (5-10): (1-6): (1-3).
Further, the average particle size of the filler of the iron-carbon combined filler II obtained in the step (4) of the invention is 2-5cm, the filling amount is 0.1-0.5 times of the volume of sewage, the iron-carbon combined filler II is formed by combining the following components in percentage by mass, and iron powder: activated carbon powder: metal: dispersing agent: adhesive: catalyst ═ (20-30): (15-20): (8-12); (2-6): (1-5): (1-3), wherein the metal is one or a composition of copper powder, aluminum powder and manganese powder, the dispersing agent is one or a composition of calcium carbonate, sodium carbonate and zinc oxide, the binder is one or a composition of phenolic resin, clay and diatomite, and the catalyst is one or a composition of zinc oxide, ammonium chloride and magnesium borate. Furthermore, the iron-carbon combined filler II is subjected to steps of water mixing, extrusion forming, medium-temperature drying, high-temperature calcination, cooling forming and the like, wherein the medium-temperature drying is drying in an oven at the temperature of 60-110 ℃ for 12-24 hours, and the high-temperature calcination is calcining in a muffle furnace at the temperature of 600-900 ℃ for 60-90 minutes by filling nitrogen.
Further, the flocculant II in the step (4) of the invention is prepared by combining the following components in percentage by mass: poly ferric chloride: sodium alginate: polyacrylamide ═ (25-30): (10-15); (8-12): (2-6), the adding amount of the flocculating agent II is 0.2-1.8mg/L, the concentrated sulfuric acid is added for multiple times, and the pH value is controlled to be 4-6 in the reaction process.
Further, the invention relates to a treatment method of comprehensive sewage of a fine chemical industry park, which comprises the following steps:
(1) front-end iron-carbon micro-electrolysis unit
The method comprises the following steps of collecting various sewage in an industrial park, then discharging the sewage into an adjusting tank, arranging a submersible stirrer inside the adjusting tank, homogenizing the water quality and adjusting the water quantity of the sewage, then discharging the sewage into a front-section iron-carbon micro-electrolysis reaction tank, arranging an iron-carbon combined filler I inside the adjusting tank, wherein the average particle size of the iron-carbon combined filler I is 5-8cm, and the filling amount of the iron-carbon combined filler I is 0.1-0.5 times of the volume of the sewage, and the iron-carbon combined filler I is formed by combining the following components in percentage by mass: activated carbon powder: copper powder, molybdenum powder, zinc powder: slaked lime: sodium carbonate: sodium silicate, diatomaceous earth: 35 parts of ammonium chloride: 15: 3: 3: 3: 2: 1: 2: 2: 3, mixing the components with water, extruding the mixture into a spherical or ellipsoidal shape, drying the mixture in an oven at the temperature of between 80 and 120 ℃ for 12 to 24 hours, calcining the dried mixture in a muffle furnace at the temperature of between 800 and 1000 ℃ for 60 to 90 minutes, and cooling and forming the mixture. In the reaction process, concentrated sulfuric acid is added for multiple times to control the pH value of sewage to be 3-5, an aeration device is started at the same time, dissolved oxygen is 2-4mg/L, after the reaction is carried out for 4-6 hours, the aeration device is closed, the sewage is discharged to a neutralization flocculation tank I, liquid caustic soda is added to adjust the pH value of the sewage to be 8-9, a flocculating agent I is added, the adding amount is 0.5-2.5mg/L, and the flocculating agent is formed by combining the following components in percentage by mass and ferrous sulfate: aluminum sulfate: sodium alginate: polyacrylamide 18: 12; 8: and 3, stirring for reaction for 1-2h, stopping stirring, standing for precipitation for 1-2h, and discharging the supernatant into the next unit.
(2) Composite hydrolysis acidification unit
And (2) discharging the sewage treated in the step (1) into a composite hydrolysis acidification reaction tank, configuring a submersible stirrer and biological suspension filler inside the tank, adding 0.2mg/L ferrous sulfate, 0.2mg/L ferrous chloride, 10mg/L light and bacteria into the tank, controlling the dissolved oxygen to be 0.5-1.0 mg/L, and allowing the water power to stay for 24-36h, and discharging the supernatant into the next unit.
(3) Composite biochemical treatment unit
Discharging the sewage treated in the step (2) into an enzyme-added upflow anaerobic sludge tank, configuring a submersible stirrer inside the tank, controlling the dissolved oxygen to be 0.1-0.3mg/L, and adding 3-5mg/L of composite biological enzyme into the anaerobic tank, wherein the composite biological enzyme is formed by combining the following components in percentage by mass: yeast: sodium acetate: urea 90: 10: 2, after carrying out anaerobic digestion on organic matters in the sewage for 15-20 hours, discharging supernatant into an enzyme-added circulating activated sludge tank, configuring an aeration device inside, controlling dissolved oxygen to be 3-5mg/L, and adding 5-10mg/L of a microbial accelerant into an aerobic tank, wherein the microbial accelerant is formed by combining the following components in percentage by mass: glucose: urea: zinc acetate: potassium dihydrogen phosphate: 80 parts of vitamins: 4: 7: 3: 1, reacting for 8-10 hours, removing most organic matters and ammonia nitrogen in the sewage, discharging the effluent into a sedimentation tank for natural sedimentation, and discharging the supernatant into the next unit.
(4) Rear iron-carbon micro-electrolysis unit
Discharging the sewage treated in the step (3) into a rear-section iron-carbon micro-electrolysis unit, wherein an iron-carbon combined filler II is arranged in the rear-section iron-carbon micro-electrolysis unit, the average particle size is 2-5cm, and the filling amount is 0.1-0.5 time of the volume of the sewage, and the iron-carbon combined filler I is formed by combining the following components in percentage by mass: activated carbon powder: copper powder, aluminum powder, manganese powder: calcium carbonate: zinc chloride: phenolic resin, diatomaceous earth: zinc oxide: 25 parts of magnesium borate: 18: 4: 3: 3: 2: 2: 2: 1: 1: 1, the components are mixed by adding water and then extruded into a spherical or ellipsoidal shape, dried in an oven at the temperature of 60-110 ℃ for 12-24 hours, calcined in a muffle furnace at the temperature of 600-900 ℃ for 60-90 minutes and then cooled and molded. In the reaction process, concentrated sulfuric acid is added for multiple times to control the pH value of the sewage to be 4-6, an aeration device is started at the same time, dissolved oxygen is 2-4mg/L, after the reaction is carried out for 6-8 hours, the aeration device is closed, the sewage is discharged to a neutralization flocculation tank I, liquid caustic soda is added to adjust the pH value of the sewage to be 8-9, a flocculating agent I is added, the adding amount is 0.2-1.8mg/L, and the flocculating agent is formed by combining the following components in mass ratio and polymerized aluminum chloride: poly ferric chloride: sodium alginate: polyacrylamide 26: 14; 10: and 4, stirring for reaction for 1-2h, stopping stirring, standing for precipitation for 1-2h, and discharging the supernatant into the next unit.
(5) Deep processing unit
And (4) discharging the sewage treated in the step (4) into a membrane bioreactor, controlling the dissolved oxygen to be 3-4mg/L, and discharging the wastewater into a final sedimentation tank for natural sedimentation after aeration reaction for 4-8h so as to achieve the standard and discharge.
Compared with the prior art, the technical scheme of the invention has unexpected technical effects, such as:
1. the iron-carbon combined filler is compounded by iron-carbon-metal-dispersant-binder-catalyst. Wherein, the iron, the carbon, the metal, the catalyst and the oxygen form a multi-element catalytic micro-electrolysis system, the contact resistance between the iron and the carbon is reduced, and the potential difference of the formed micro-battery is large. The addition of the dispersing agent and the binder can enable more microporous structures to be formed inside the filler, the contact area between the filler and wastewater is increased, the formed filler has high binding power and strong mechanical strength. The iron-carbon combined filler solves the problems of easy hardening, easy passivation, easy crushing, easy pipeline blockage, serious loss and difficult replacement of the filler in the traditional micro-electrolysis treatment process, and concentrated sulfuric acid is added for multiple times, so that the pH value can be controlled within a certain range in the whole reaction process, thereby being beneficial to slowly generating nascent ferrous ions, quickly catalyzing and oxidizing pollutants which are difficult to degrade in sewage, improving the biodegradability of the sewage, reducing chromophoric groups and reducing the chromaticity of the sewage.
2. Ferrous salt, light and bacteria are added to form a composite hydrolysis acidification system on the basis of a traditional hydrolysis acidification pool. The ferrous ions in the ferrous salt not only play a role in catalyzing and promoting biochemical reaction, but also can perform complex reaction and reduction reaction with chromophoric groups in sewage, and the chemical flocculation effect and the biological flocculation effect of the hydrolysate of the iron are organically combined together, so that the removal rate of organic matters and chromaticity is increased. The photosynthetic bacteria are added, indigenous flora such as hydrolytic acidification bacteria and sulfate reducing bacteria form a co-metabolic system, so that the biodegradability of the sewage is improved, and favorable conditions are created for subsequent anaerobic and aerobic biological treatment.
3. On the basis of traditional anaerobic biological treatment and aerobic biological treatment, composite biological enzyme and microbial agent are added respectively to form an enhanced biological treatment process, so that the microbial co-metabolism can be started quickly, a co-metabolism system is constructed, and the removal capability of organic matters is greatly enhanced. The yeast has the characteristics of bacteria, fast growth and propagation, and capability of forming better floccules, and also has the characteristics of filamentous fungi, and has the advantages of larger cells, vigorous metabolism, higher removal rate of COD and the like; glucose, urea and potassium dihydrogen phosphate are the most widely used carbon source, nitrogen source and trace elements of the microorganism, the bioavailability is high, and the cost is low; the sodium acetate and the zinc acetate can enhance the induction of key enzyme and the supply of energy, and provide energy for the co-metabolism of microorganisms; vitamin C provides reducing power, various prosthetic groups and coenzymes for its metabolic pathways.
4. The membrane bioreactor process system ensures that organic pollutants in the sewage have enough retention time in the bioreactor with limited volume, thereby greatly improving the degradation efficiency. Due to the high-efficiency separation effect of the membrane, the effluent quality is excellent and stable.
In conclusion, the iron-carbon combined filler, the flocculating agent, the compound biological enzyme and the microbial agent are all selected by the inventor through creative experiments. The invention creatively connects the front-section iron-carbon micro-electrolysis unit, the composite hydrolysis acidification unit, the composite biochemical treatment unit, the rear-section iron-carbon micro-electrolysis unit and the advanced treatment unit skillfully to form a continuous step reaction unit, has high impact load resistance, strong treatment capability and stable operation effect, and is particularly suitable for the treatment of comprehensive sewage in fine chemical engineering parks.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following is further illustrated by the specific examples, and it should be understood by those skilled in the art that the present invention is not limited to these examples. The invention has enough flexibility and adaptability to broad spectrum for treating the comprehensive sewage of fine chemical industry park, such as pesticide chemical wastewater, dye and pigment chemical wastewater, essence and spice chemical wastewater, cosmetic health product wastewater, food and feed additive wastewater, daily chemical wastewater and mixed production and domestic sewage, and the external drainage is stable and reaches the standard for discharge.
In order to further verify the iron-carbon combined filler, the compound biological enzyme and the microbial agent used in the invention, a small-scale experiment with multiple conditions and single factor is carried out, which specifically comprises the following steps:
(1) verification of use of iron-carbon combined filler I in the front-stage iron-carbon micro-electrolysis unit: under the condition that other test conditions and steps are the same, the single iron-carbon micro-electrolysis treatment is carried out on the sewage of pesticide chemical industry, dye and pigment chemical industry and daily chemical products, the iron-carbon combined filler I and a certain commercially available iron-carbon filler are adopted to carry out multiple same-level test verification and comparison, the test results are averaged, and the test results are shown in table 1.
Table 1 verification of iron-carbon composite Filler I
The test result shows that: compared with the commercially available iron-carbon filler, the iron-carbon composite filler I provided by the invention is used for treating COD and NH in pesticide chemical industry, dye and pigment and daily chemical wastewater3both-N and chromaticity showed higher removal rates.
(2) And (3) verifying the use of the iron-carbon combined filler II in the rear-section iron-carbon micro-electrolysis unit: under the condition that other test conditions and steps are the same, the single iron-carbon micro-electrolysis treatment is carried out on sewage of essence, spice, chemical industry, cosmetics, health products, food and feed additives after being subjected to biological treatment, the iron-carbon combined filler II and a certain commercially available iron-carbon filler are adopted to carry out multiple same-level test verification and comparison, the test results are averaged, and the test results are shown in the table 2.
TABLE 2 verification of iron-carbon combination Filler II
The test result shows that: compared with the commercially available iron-carbon filler, the iron-carbon combined filler II has higher removal rate on COD and chroma of sewage of essence, spice, chemical industry, cosmetics, health products, food and feed additives, and can obviously improve the biodegradability of the sewage.
(3) And (3) verifying the use of the compound biological enzyme and the microbial agent in the compound biochemical treatment unit: treating the pesticide after conventional pretreatment by using a single composite biochemical unitThe mixed sewage of chemical wastewater and dye pigment chemical wastewater, the wastewater index is: COD is 6450 mg/L; the BOD is 2570 mg/L; NH (NH)3the-N is 440mg/L, the chroma is 750 times, the treatment capacity is 1000L respectively, and under the condition that other test conditions and steps are the same, the composite biochemical treatment process and the conventional biochemical treatment process are adopted for verification and comparison, the removal rate is percent, and the test results are shown in Table 3.
TABLE 3 verification of composite Biochemical treatment of wastewater
The test result shows that: on the basis of traditional anaerobic biological treatment and aerobic biological treatment, composite biological enzyme and microbial agent are added, so that excellent treatment effects of degrading organic pollutants and decomposing colored groups can be shown.
Example 1: a certain fine chemical industry park in Guangdong province is an industrial park which mainly comprises essence, spice, cosmetics, health care products and daily chemicals, and the comprehensive sewage indexes are as follows: COD concentration 9580-, 3NH- n concentration 1100-1300mg/L, color 1250 times. The treatment method of the comprehensive sewage of the fine chemical industry park, which is related by the invention, is adopted for treatment, and the specific treatment process is as follows:
front-stage iron-carbon microelectrolysis unit: the method comprises the following steps of collecting various sewage in an industrial park, then discharging the sewage into an adjusting tank, internally configuring a submersible stirrer, carrying out water quality homogenization and water quantity adjustment on the sewage, then discharging the sewage into a front-section iron-carbon micro-electrolysis reaction tank, internally configuring an iron-carbon combined filler I, wherein the average particle size is 5-8cm, and the filling amount is 0.3 time of the volume of the sewage, wherein the iron-carbon combined filler I is formed by combining the following components in percentage by mass: activated carbon powder: copper powder, molybdenum powder: slaked lime: calcium oxide: sodium silicate, diatomaceous earth: alumina: 30 parts of ammonium chloride: 10: 3: 4: 1: 1: 2: 2: 1: 1, the components are mixed by adding water and then extruded into a spherical or ellipsoidal shape, dried in an oven at the temperature of 80-120 ℃ for 12-24 hours, calcined in a muffle furnace at the temperature of 800-1000 ℃ for 60-90 minutes and then cooled and molded. In the reaction process, concentrated sulfuric acid is added for multiple times to control the pH value of sewage to be 3-5, an aeration device is started at the same time, dissolved oxygen is 2-4mg/L, after the reaction is carried out for 4-6 hours, the aeration device is closed, the sewage is discharged to a neutralization flocculation tank I, liquid alkali is added to adjust the pH value of the sewage to be 8-9, a flocculating agent I is added, the adding amount is 1.0mg/L, and the flocculating agent is formed by combining the following components in percentage by mass and ferrous sulfate: aluminum sulfate: sodium alginate: polyacrylamide 15: 10; 6: 1, stirring for reaction for 1-2h, closing stirring, standing for precipitation for 1-2h, and discharging the supernatant into the next unit.
A composite hydrolysis acidification unit: and discharging the sewage into a composite hydrolysis acidification reaction tank, arranging a submersible stirrer and biological suspension filler inside the tank, adding 0.2mg/L ferrous sulfate, 0.1mg/L ferrous carbonate, light and bacteria 6mg/L into the tank, controlling the dissolved oxygen to be 0.5-1.0 mg/L, and controlling the hydraulic retention time to be 24-36h, and discharging the supernatant into the next unit.
A composite biochemical treatment unit: discharging the sewage into an enzyme-added baffle plate anaerobic tank, arranging a submersible stirrer inside the anaerobic tank, controlling dissolved oxygen to be 0.1-0.3mg/L, and adding composite biological enzyme into the anaerobic tank to be 3mg/L, wherein the composite biological enzyme is formed by combining the following components in percentage by mass: yeast: sodium acetate: urea 80: 6: 1, after carrying out anaerobic digestion on organic matters in sewage for 15-20 hours, discharging supernate into an enzyme-added circulating activated sludge tank, configuring an aeration device inside, controlling dissolved oxygen to be 3-5mg/L, and adding 5mg/L of a microbial accelerant into an aerobic tank, wherein the microbial accelerant is formed by combining the following components in percentage by mass: glucose: urea: zinc acetate: potassium dihydrogen phosphate: vitamin 70: 3: 5: 2: 1, reacting for 8-10 hours, removing most organic matters and ammonia nitrogen in the sewage, discharging the effluent into a sedimentation tank for natural sedimentation, and discharging the supernatant into the next unit.
Rear section iron carbon micro-electrolysis unit: discharging the sewage into a rear-section iron-carbon micro-electrolysis unit, wherein an iron-carbon combined filler II is arranged in the rear-section iron-carbon micro-electrolysis unit, the average particle size is 2-5cm, and the filling amount is 0.1 time of the volume of the sewage, and the iron-carbon combined filler I is formed by combining the following components in percentage by mass: activated carbon powder: copper powder, aluminum powder: calcium carbonate: sodium carbonate: clay, diatomaceous earth: zinc oxide 20: 15: 5: 3: 2: 1: 1: 1: 1, the components are mixed by adding water and then extruded into a spherical or ellipsoidal shape, dried in an oven at the temperature of 60-110 ℃ for 12-24 hours, calcined in a muffle furnace at the temperature of 600-900 ℃ for 60-90 minutes and then cooled and molded. In the reaction process, concentrated sulfuric acid is added for multiple times to control the pH value of the sewage to be 4-6, an aeration device is started at the same time, dissolved oxygen is 2-4mg/L, after the reaction is carried out for 6-8 hours, the aeration device is closed, the sewage is discharged to a neutralization flocculation tank I, liquid caustic soda is added to adjust the pH value of the sewage to be 8-9, a flocculating agent II is added, the adding amount is 0.3mg/L, and the flocculating agent is formed by combining the following components in percentage by mass and is polymerized aluminum chloride: poly ferric chloride: sodium alginate: polyacrylamide 25: 15; 8: and 2, stirring for reaction for 1-2h, stopping stirring, standing for precipitation for 1-2h, and discharging the supernatant into the next unit.
A depth processing unit: discharging the sewage into a membrane bioreactor, controlling the dissolved oxygen to be 3-4mg/L, carrying out aeration reaction for 4-8h, discharging the wastewater into a final sedimentation tank, naturally settling, and discharging the wastewater up to the standard. The indexes of the treated sewage are as follows: COD concentration is 35-40mg/L, BOD concentration is 3-6mg/L, 3NH-N concentration is 0.4-2mg/L, and the chroma is less than or equal to 30 times.
Example 2: one industrial park in Shandong province mainly uses pesticide chemical industry and dye and pigment chemical industry, and the comprehensive sewage indexes are as follows: the COD concentration is 11360-, 3NH-N concentration 1300-mg/L, chroma 1500 times. The treatment method of the comprehensive sewage of the fine chemical industry park, which is related by the invention, is adopted for treatment, and the specific treatment process is as follows:
front-stage iron-carbon microelectrolysis unit: the method comprises the following steps of collecting various sewage in an industrial park, then discharging the sewage into an adjusting tank, internally configuring a submersible stirrer, carrying out water quality homogenization and water quantity adjustment on the sewage, then discharging the sewage into a front-section iron-carbon micro-electrolysis reaction tank, internally configuring an iron-carbon combined filler I, wherein the average particle size is 5-8cm, and the filling amount is 0.5 times of the volume of the sewage, wherein the iron-carbon combined filler I is formed by combining the following components in percentage by mass: activated carbon powder: molybdenum powder and zinc powder: sodium carbonate: calcium oxide: sodium silicate, diatomaceous earth, bentonite: alumina: sodium borate 40: 20: 5: 5: 3: 2: 2: 2: 1: 2: 1, the components are mixed by adding water and then extruded into a spherical or ellipsoidal shape, dried in an oven at the temperature of 80-120 ℃ for 12-24 hours, calcined in a muffle furnace at the temperature of 800-1000 ℃ for 60-90 minutes and then cooled and molded. In the reaction process, concentrated sulfuric acid is added for multiple times to control the pH value of sewage to be 3-5, an aeration device is started at the same time, dissolved oxygen is 2-4mg/L, after the reaction is carried out for 4-6 hours, the aeration device is closed, the sewage is discharged to a neutralization flocculation tank I, liquid alkali is added to adjust the pH value of the sewage to be 8-9, a flocculating agent I is added, the adding amount is 2.5mg/L, and the flocculating agent is formed by combining the following components in percentage by mass and ferrous sulfate: aluminum sulfate: sodium alginate: polyacrylamide 20: 15; 9: and 4, stirring for reaction for 1-2h, stopping stirring, standing for precipitation for 1-2h, and discharging the supernatant into the next unit.
A composite hydrolysis acidification unit: and discharging the sewage into a composite hydrolysis acidification reaction tank, arranging a submersible stirrer and biological suspension filler inside the tank, adding ferrous iron chloride 0.4mg/L, ferrous carbonate 0.1mg/L, light and bacteria 12mg/L into the tank, controlling dissolved oxygen 0.5-1.0 mg/L, and allowing the water power to stay for 24-36h, and discharging the supernatant into the next unit.
A composite biochemical treatment unit: discharging the sewage into an enzyme-added sequencing batch anaerobic tank, arranging a submersible stirrer inside the anaerobic tank, controlling dissolved oxygen to be 0.1-0.3mg/L, and adding composite biological enzyme into the anaerobic tank to be 5mg/L, wherein the composite biological enzyme is formed by combining the following components in percentage by mass: yeast: sodium acetate: urea 100: 10: 3, after carrying out anaerobic digestion on organic matters in the sewage for 15-20 hours, discharging the supernatant into an enzyme-added biological contact oxidation tank, configuring an aeration device inside, controlling dissolved oxygen to be 3-5mg/L, and adding 10mg/L of a microbial accelerant into an aerobic tank, wherein the microbial accelerant is formed by combining the following components in percentage by mass: glucose: urea: zinc acetate: potassium dihydrogen phosphate: vitamin 100: 6: 8: 6: 2, reacting for 8-10 hours, removing most organic matters and ammonia nitrogen in the sewage, discharging the effluent into a sedimentation tank for natural sedimentation, and discharging the supernatant into the next unit.
Rear section iron carbon micro-electrolysis unit: discharging the sewage into a rear-section iron-carbon micro-electrolysis unit, wherein an iron-carbon combined filler II is arranged in the rear-section iron-carbon micro-electrolysis unit, the average particle size is 2-5cm, and the filling amount is 0.4 times of the volume of the sewage, and the iron-carbon combined filler I is formed by combining the following components in percentage by mass: activated carbon powder: copper powder and manganese powder: calcium carbonate: sodium carbonate: zinc oxide: diatomite: ammonium chloride: magnesium borate is 30: 20: 7: 5: 3: 3: 3: 4: 2: 1, the components are mixed by adding water and then extruded into a spherical or ellipsoidal shape, dried in an oven at the temperature of 60-110 ℃ for 12-24 hours, calcined in a muffle furnace at the temperature of 600-900 ℃ for 60-90 minutes and then cooled and molded. In the reaction process, concentrated sulfuric acid is added for multiple times to control the pH value of the sewage to be 4-6, an aeration device is started at the same time, dissolved oxygen is 2-4mg/L, after the reaction is carried out for 6-8 hours, the aeration device is closed, the sewage is discharged to a neutralization flocculation tank I, liquid caustic soda is added to adjust the pH value of the sewage to be 8-9, a flocculating agent II is added, the adding amount is 1.8mg/L, and the flocculating agent is formed by combining the following components in percentage by mass and is polymerized aluminum chloride: poly ferric chloride: sodium alginate: polyacrylamide 30: 15; 12: and 6, stirring for reaction for 1-2h, stopping stirring, standing for precipitation for 1-2h, and discharging the supernatant into the next unit.
A depth processing unit: discharging the sewage into a membrane bioreactor, controlling the dissolved oxygen to be 3-4mg/L, carrying out aeration reaction for 4-8h, discharging the wastewater into a final sedimentation tank, naturally settling, and discharging the wastewater up to the standard. The indexes of the treated sewage are as follows: COD concentration is 39-45mg/L, BOD concentration is 5-8mg/L, 3NH-N concentration 2-4mg/L, and the chroma is less than or equal to 30 times.
Claims (9)
1. A treatment method of comprehensive sewage in a fine chemical industry park is characterized by mainly comprising the following steps:
(1) front-end iron-carbon micro-electrolysis unit
(2) Composite hydrolysis acidification unit
(3) Composite biochemical treatment unit
(4) Rear iron-carbon micro-electrolysis unit
(5) And a depth processing unit.
2. The method for treating the integrated wastewater of the fine chemical industrial park as claimed in claim 1, wherein the method mainly comprises the following steps:
1) front-end iron-carbon micro-electrolysis unit
Collecting various sewage in an industrial park, then discharging the sewage into an adjusting tank, configuring a submersible stirrer inside the adjusting tank, homogenizing the water quality and adjusting the water quantity of the sewage, then discharging the sewage into a front-section iron-carbon micro-electrolysis reaction tank, configuring an iron-carbon combined filler I inside the adjusting tank, adding concentrated sulfuric acid to control the pH value of the sewage to be 3-5, starting an aeration device to dissolve oxygen to be 2-4mg/L, after reacting for 4-6h, closing the aeration device, discharging the sewage into a neutralization flocculation tank I, adding liquid alkali to adjust the pH value of the sewage to be 8-9, adding a flocculating agent I, stirring and reacting for 1-2h, closing stirring, standing and precipitating for 1-2h, and discharging supernatant into the next unit;
2) composite hydrolysis acidification unit
Discharging the sewage treated in the step (1) into a composite hydrolysis acidification reaction tank, configuring a submersible stirrer and biological suspension filler inside the tank, adding ferrous salt, light and bacteria into the tank, controlling the dissolved oxygen to be 0.5-1.0 mg/l, maintaining the hydraulic power for 24-36h, and discharging the supernatant into the next unit;
3) composite biochemical treatment unit
Discharging the sewage treated in the step (2) into an enzyme-adding anaerobic tank, configuring a submersible stirrer inside the tank, adding compound biological enzyme into the anaerobic tank, controlling dissolved oxygen to be 0.1-0.3mg/L, performing anaerobic digestion on organic matters in the sewage for 15-20 hours, discharging supernatant into an enzyme-adding aerobic tank, configuring an aeration device inside the tank, adding a microbial accelerant into the aerobic tank, controlling dissolved oxygen to be 3-5mg/L, removing most of the organic matters and ammonia nitrogen in the sewage, controlling the reaction time to be 8-10 hours, discharging effluent into a settling tank for natural settling, and discharging the supernatant into the next unit;
4) rear iron-carbon micro-electrolysis unit
Discharging the sewage treated in the step (3) into a rear-section iron-carbon micro-electrolysis unit, preparing an iron-carbon combined filler II inside the rear-section iron-carbon micro-electrolysis unit, adding concentrated sulfuric acid to control the pH value of the sewage to be 4-6, starting an aeration device to dissolve oxygen to be 2-4mg/L, after reacting for 6-8h, closing the aeration device, discharging the sewage into a neutralization flocculation tank II, adding liquid alkali to adjust the pH value of the sewage to be 8-9, adding a flocculating agent II, stirring and reacting for 1-2h, closing stirring, standing and precipitating for 1-2h, and discharging the supernatant into the next unit;
5) deep processing unit
And (4) discharging the sewage treated in the step (4) into a membrane bioreactor, controlling the dissolved oxygen to be 3-4mg/L, and discharging the wastewater into a final sedimentation tank for natural sedimentation after aeration reaction for 4-8h so as to achieve the standard and discharge.
3. The method according to claim 1, wherein the iron-carbon composite filler I of step (1) is composed of iron powder, activated carbon, metal, dispersant, binder and catalyst, and has an average particle size of 5-8cm and a loading amount of 0.1-0.5 times the volume of the wastewater. Preferably, the iron-carbon combined filler I is formed by combining the following components in percentage by mass: activated carbon powder: metal: dispersing agent: adhesive: catalyst = (30-40): (10-20): (5-10); (1-5): (1-5): (1-3); the metal is one or a composition of copper powder, molybdenum powder and zinc powder, the dispersing agent is one or a composition of lime powder, sodium carbonate and calcium oxide, the binder is one or a composition of sodium silicate, diatomite and bentonite, and the catalyst is one or a composition of aluminum oxide, ammonium chloride and sodium borate.
4. The method for treating the comprehensive sewage of the fine chemical industry park as claimed in claim 1, wherein the iron-carbon combined filler I is prepared by the steps of adding water for mixing, extruding and forming, drying at medium temperature, calcining at high temperature, cooling and forming and the like; the medium-temperature drying is drying for 12-24 hours in an oven at the temperature of 80-120 ℃, and the high-temperature calcination is calcining for 60-90 minutes in a muffle furnace at the temperature of 800-1000 ℃ by filling nitrogen. Preferably, the flocculating agent I in the step (1) is a composition of ferrous sulfate, aluminum sulfate, sodium alginate and polyacrylamide, and the adding amount of the flocculating agent I is 0.5-2.5 mg/L. Further preferably, the flocculating agent I is prepared by combining the following components in percentage by mass: aluminum sulfate: sodium alginate: polyacrylamide = (15-20): (10-15); (6-10): (1-5).
5. The method according to claim 1, wherein the ferrous salt in step (2) is sulfurOne or the combination of ferrous acid, ferrous chloride and ferrous carbonate, the total adding amount of ferrous salt is 0.3-0.5mg/l, and the concentration of the photosynthetic bacteria is more than 109One/ml of commercial photosynthetic bacteria suspension is added in an amount of 6-12 mg/l.
6. The method for treating integrated wastewater of a fine chemical industrial park as claimed in claim 1, wherein the anaerobic tank in the step (3) is one of an upflow anaerobic sludge tank, a baffled anaerobic tank and a sequencing batch anaerobic tank, and the aerobic tank is one of a sequencing batch activated sludge tank, a biological contact oxidation tank and a circulating activated sludge tank; the compound biological enzyme is a composition of yeast, sodium acetate and urea, and the microbial accelerant is a composition of glucose, urea, zinc acetate, monopotassium phosphate and vitamin C. Preferably, the adding amount of the compound biological enzyme is 3-5mg/L, and the mass ratio of the yeast: sodium acetate: urea = (80-100): (6-10): (1-3); the addition amount of the microbial accelerant is 5-10mg/L, calculated by mass ratio, glucose: urea: zinc acetate: potassium dihydrogen phosphate: vitamin = (50-100): (3-6): (5-10): (1-6): (1-3).
7. The method according to claim 1, wherein the iron-carbon composite filler II obtained in the step (4) is composed of iron powder, activated carbon, metal, a dispersant, a binder and a catalyst, and has an average particle size of 2-5cm and a filling amount of 0.1-0.5 times the volume of the wastewater. Preferably, the iron-carbon combined filler II is formed by combining the following components in percentage by mass: activated carbon powder: metal: dispersing agent: adhesive: catalyst = (20-30): (15-20): (8-12); (2-6): (1-5): (1-3); the metal is one or a composition of copper powder, aluminum powder and manganese powder, the dispersing agent is one or a composition of calcium carbonate, sodium carbonate and zinc oxide, the binder is one or a composition of phenolic resin, clay and diatomite, and the catalyst is one or a composition of zinc oxide, ammonium chloride and magnesium borate. More preferably, the iron-carbon combined filler II is subjected to steps of water mixing, extrusion forming, medium-temperature drying, high-temperature calcination, cooling forming and the like, wherein the medium-temperature drying is drying in an oven at the temperature of 60-110 ℃ for 12-24 hours, and the high-temperature calcination is calcining in a muffle furnace at the temperature of 600-900 ℃ for 60-90 minutes by filling nitrogen.
8. The method according to claim 2, wherein the flocculating agent II in the step (4) is a composition of polyaluminium chloride, polyferric chloride, sodium alginate and polyacrylamide, and the dosage of the flocculating agent II is 0.2-1.8 mg/L. Preferably, the flocculating agent II is prepared by combining the following components in percentage by mass: poly (ferric chloride): sodium alginate: polyacrylamide = (25-30): (10-15); (8-12): (2-6).
9. The method for treating the integrated wastewater of the fine chemical industrial park as claimed in claim 1, wherein the concentrated sulfuric acid is added in multiple steps in the steps (1) and (4), and the pH value is controlled to be 4-6 during the reaction process.
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