CN110734178A - coking wastewater membrane concentration salt separation zero-discharge treatment system and method - Google Patents

coking wastewater membrane concentration salt separation zero-discharge treatment system and method Download PDF

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CN110734178A
CN110734178A CN201810791252.9A CN201810791252A CN110734178A CN 110734178 A CN110734178 A CN 110734178A CN 201810791252 A CN201810791252 A CN 201810791252A CN 110734178 A CN110734178 A CN 110734178A
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nanofiltration
pump
concentration
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water
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张雄文
裘慕贤
金学文
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Baowu Carbon Material Technology Co ltd
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    • C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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    • 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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    • C02F2303/16—Regeneration of sorbents, filters
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Abstract

The invention belongs to the technical field of water treatment, and particularly relates to a coking wastewater membrane concentration salt separation zero-discharge treatment system and method, which comprises the following steps of coking wastewater pretreatment including full-automatic sand filtration, activated carbon adsorption regeneration, ultrafiltration and softening, membrane salt separation concentration treatment including low-pressure nanofiltration, high-pressure nanofiltration, purification nanofiltration and reverse osmosis treatment, concentration treatment, fluorine and silicon removal, electrodialysis concentration and evaporative crystallization to obtain an industrial-grade sodium chloride product with the purity of more than 92%, feeding a sodium sulfate concentrated solution into a freezing crystallization device to generate sodium sulfate, heating and melting the sodium sulfate, feeding the sodium sulfate into an evaporative crystallization, centrifugation and drying system to obtain an industrial-grade sodium sulfate product with the purity of more than 95%.

Description

coking wastewater membrane concentration salt separation zero-discharge treatment system and method
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to coking wastewater membrane concentration salt separation zero-discharge treatment technology, system and method.
Background
At present, most coking wastewater treatment processes adopt an A/O treatment method, namely an anoxic and aerobic method, mainly adopt a biological method to degrade COD, ammonia nitrogen and total nitrogen in the wastewater, the coking wastewater is directly discharged or sent to a steel unit for reuse after biochemical treatment (mostly used for blast furnace slag flushing and coke quenching), new coking enterprises and parts of areas with higher environmental requirements implement new standards (GB 16171-1612012 in table 2) and special discharge (GB 71-2012 in table 3) requirements, and unit product standard water discharge quantity is 1.0m from the prior art3The/t coke rises to 0.4m3A/t coke and 0.3m3The emission of waste water of most coking enterprises, especially newly built and modified coking enterprises, can not meet the new and special emission requirements. A small amount of coking enterprises perform evaporative crystallization on concentrated water obtained after membrane concentration of coking wastewater to obtain industrial water and mixed salt, and the mixed salt contains organic matters and other impurities, so that the mixed salt belongs to hazardous waste and is high in disposal cost. How to remove pollutants such as organic matters in the coking wastewater and purify salt substances in the coking wastewater as industrial products, and the technology for realizing zero discharge of the coking wastewater has great significance.
Disclosure of Invention
The invention aims to provide coking wastewater zero-discharge treatment systems, methods and technologies for removing organic matters, fluorine, silicon, calcium and magnesium in wastewater, separating and concentrating sodium chloride and sodium sulfate, and freezing and evaporating for crystallization to obtain industrial-grade salt products, so that zero discharge of coking wastewater is realized.
coking wastewater membrane concentration salt separation zero-discharge treatment method is characterized by comprising the following steps:
(1) pretreatment of coking wastewater: the pretreatment of the coking wastewater comprises full-automatic sand filtration, activated carbon adsorption regeneration, ultrafiltration and softening;
the quality indexes of the coking wastewater are as follows: pH of 7 to 8, COD of 300 to 550mg/l, Cl-8000-12000 mg/l of SO4 2-10000-14000 mg/l of Na+Is 11000 to 15000mg/l, F-50-200 mg/l of total cyanogen, 10-20 mg/l of total nitrogen, 200-500 mg/l of total nitrogen, 10-30 mg/l of calcium, 5-10 mg/l of magnesium, 20000-40000 mg/l of TDS, and 30-50 mg/l of suspended matters;
the coking wastewater is thrown into full-automatic sand for filtering, suspended matters in the coking wastewater are removed to be below 5mg/l, filtered water enters an activated carbon adsorption tower, and the activated carbon is coal-based briquette crushed granular carbon with the particle size: 5-50 meshes, the adsorption iodine value is 800-1100, the effluent of the activated carbon adsorption tower enters an ultrafiltration device (the ultrafiltration adopts a conventional ultrafiltration membrane), the ultrafiltration produced water enters 2 sets of softening systems connected in parallel, calcium and magnesium ions in the wastewater are removed through weak acid cation resin, the produced water calcium ions are less than 2mg/l, and the magnesium ions are less than 1 mg/l;
(2) membrane salt separation concentration treatment: the membrane salt separation concentration treatment comprises low-pressure nanofiltration, high-pressure nanofiltration, purification nanofiltration and reverse osmosis treatment;
the softened wastewater is pumped into a low-pressure nanofiltration device, and the low-pressure nanofiltration capacity is 20-30 m3H, low-pressure nanofiltration is provided with 2-3 sections, an intersegmental pump is arranged in the middle, the low-pressure nanofiltration membrane separates -valent ions from divalent ions in the wastewater, concentrated water is concentrated by 2-4 times, and SO is added4 2-25000-45000 mg/l, TDS 50000-80000 mg/l, high-pressure nanofiltration is carried out on concentrated water, produced water is purified and nanofiltered, divalent salt in the low-pressure nanofiltration concentrated water is concentrated in steps through a high-pressure pump and the high-pressure nanofiltration membrane, the high-pressure nanofiltration is provided with 1-2 sections, the high-pressure pump is provided with a frequency conversion device, the pressure is 5-10 MPa, an energy recovery device is arranged behind the concentrated water and in front of the high-pressure nanofiltration pump, the concentrated water is concentrated by 2-4 times, and SO is recycled4 2-65000-90000 mg/l, TDS 100000-150000 mg/l, concentrated water as sodium sulfate freezing and evaporating crystallization material, and water producedPurifying and nano-filtering;
purified nanofiltration produced water enters a reverse osmosis device, and the reverse osmosis treatment capacity is 10-20 m3The reverse osmosis is arranged at 2-3 sections, the water inlet pump adopts a high-pressure variable-frequency pump, the section pump adopts an intersegmental pump, the pressure of the high-pressure pump is 2-5 MPa, the concentrated water is concentrated by 2-4 times, and Cl-15000-30000 mg/l, TDS 35000-60000 mg/l, SO4 2-100-200 mg/l;
(3) concentration treatment, fluorine and silicon removal, electrodialysis concentration and evaporative crystallization;
after the reverse osmosis membrane is concentrated, adding a calcium chloride solution with the concentration of 20-35%, magnesium oxide or magnesium chloride solution with the concentration of 5-20% and a sodium carbonate solution with the concentration of 10-25% into the wastewater respectively to generate solid precipitates, and removing the generated suspended matters by adopting a tubular microfiltration membrane; after defluorination, desilication and calcium and magnesium removal, the wastewater enters an electrodialysis device, the electrodialysis device adopts a parallel connection mode of 2-3 groups, concentrated solution is concentrated by 2-4 times, the concentrated solution is used as a sodium chloride evaporation crystallization raw material, and produced water is returned to the low-pressure nanofiltration inlet water for recycling;
directly feeding the electrodialysis concentrated solution into a sodium chloride evaporation crystallization, concentration, centrifugation and packaging system to obtain an industrial grade sodium chloride product with the purity of more than 92%; and (3) firstly putting the sodium sulfate concentrated solution into a freezing and crystallizing device to generate mirabilite, heating and melting the mirabilite, and then putting the mirabilite into an evaporation, crystallization, centrifugation and drying system to obtain an industrial-grade sodium sulfate product with the purity of more than 95%.
And , performing reverse cleaning by using filtered water, wherein the sand is quartz sand, the particle size of the filter material is 0.25-0.55 mm, and the filtering flow rate is 0.3-0.8 m/s.
, the filtered water stays in the activated carbon adsorption tower for about 1-3 hours.
And step , regenerating the adsorbed activated carbon by a regeneration furnace and then returning to be recycled, periodically supplementing the loss amount, and reducing the COD (chemical oxygen demand) of the wastewater treated by the activated carbon to 100-200 mg/l.
According to the coking wastewater membrane concentration salt separation zero-discharge treatment method, the SDI value of the water produced by the ultrafiltration system is less than 3.
According to the coking wastewater membrane concentration salt separation zero-discharge treatment method, SO in low-pressure nanofiltration and high-pressure nanofiltration produced water is purified, nanofiltered and separated4 2-In order to avoid affecting the purity of -valent sodium chloride, 2-3 sections are set for purification and nanofiltration according to the concentration requirement, and the water SO is produced by purification and nanofiltration4 2-30-80 mg/l, TDS is 10000-25000 mg/l.
According to the coking wastewater membrane concentration salt-separation zero-discharge treatment method, calcium chloride solution, magnesium oxide solution and sodium carbonate solution are respectively added into wastewater after reverse osmosis membrane concentration to generate solid precipitates, a tubular microfiltration membrane is adopted to remove suspended matters generated in the solid precipitates, and F in the wastewater after treatment is subjected to F-type microfiltration membrane concentration salt-separation zero-discharge treatment-SiO in an amount of 10 to 80mg/l2Ca in an amount of 10 to 30mg/l2+5-30 Mg/l of Mg2+The content is 1-10 mg/l, and the turbidity is less than 1 ntu.
According to the coking wastewater membrane concentration salt-separation zero-emission treatment method, 2-3 groups of electrodialysis devices are connected in parallel, electrodialysis is composed of membranes, frames, electrodes, a high-frequency power supply, a matched tank and the like, and the amount of wastewater treated is 10-20 m3/h。
And , evaporating and crystallizing device including sodium chloride evaporating and crystallizing device, sodium sulfate freezing and crystallizing device, and evaporating and crystallizing device.
The invention also provides a coking wastewater membrane concentration and salt separation zero-emission treatment system which sequentially comprises a water inlet pump 1, a full-automatic double-tank sand filter 2, an adsorption water inlet pump 3, an adsorption tower 4, an ultrafiltration 5, a softening water inlet pump 6, a weak acid resin bed 7, a low-pressure nanofiltration water inlet pump 8, a low-pressure nanofiltration 9, a high-pressure nanofiltration water inlet pump 10, a high-pressure nanofiltration 11, a purification nanofiltration 14, a reverse osmosis water inlet pump 15, a re-concentration reverse osmosis 16, a fluorine, silicon and calcium magnesium removal 17, a tubular microfiltration circulating pump 18, a tubular microfiltration 19, an electrodialysis water inlet pump 20, an electrodialysis 21, a sodium chloride inlet pump 22 and a sodium chloride evaporative crystallization 23, wherein the high-pressure nanofiltration 11 is further sequentially connected with a sodium sulfate inlet pump 12, a sodium sulfate freezing crystallization and evaporative crystallization 13, an outlet of the purification nanofiltration 14 is further connected with the low-pressure water inlet pump 8, and the low-pressure nanofiltration 9 is further connected with an inlet of the purification nanofiltration 14.
The coking wastewater inlet water quality index is as follows: pH of 7 to 8, COD of 300 to 550mg/l, Cl-8000-12000 mg/l of SO4 2-10000-14000 mg/l of Na+Is 11000 to 15000mg/l, F-50-200 mg/l of total cyanogen, 10-20 mg/l of total nitrogen, 200-500 mg/l of total nitrogen, 10-30 mg/l of calcium, 5-10 mg/l of magnesium, 20000-40000 mg/l of TDS (total dissolved solids), 30-50 mg/l of suspended matters (SS), the pretreatment of coking wastewater comprises full-automatic sand filtration, activated carbon adsorption regeneration, ultrafiltration and softening, and the like, the full-automatic sand filter removes suspended matters (SS is less than 5mg/l) in the coking wastewater, the activated carbon filter intercepts and adsorbs colloids, metal ions and organic matters in the wastewater, the activated carbon is coal-based briquette crushed granular carbon, the particle size is 5-50 meshes, the adsorption iodine value is 800-1100, the adsorbed activated carbon is regenerated by a regeneration furnace and then returned for recycling, the loss amount is periodically supplemented, the COD is reduced to 100-200 mg/l, the wastewater is subjected to steps of dissolving granular substances, organic matters, micro-molecular biological ions and other components in the wastewater are separated from weak acid ion fluid, calcium ion fluid and calcium ion fluid is less than 3 mg/l, calcium ion is removed by a calcium ion production system, calcium ion production system is connected in parallel, and calcium ion production system, calcium ion production system is less than 2.
The membrane salt separation concentration treatment part comprises a low-pressure nanofiltration device, a high-pressure nanofiltration device, a purification nanofiltration device and a reverse osmosis device.
2-3 sections of low-pressure nanofiltration membrane are arranged, an intersegmental pump is arranged in the middle, and the low-pressure nanofiltration membrane is used for -valent (Cl) in the wastewater-) And divalent (SO)4 2-) Separating ions, concentrating the concentrated water by 2-4 times, and adding SO4 2-25000-45000 mg/l, TDS (total dissolved solids) is 50000-80000 mg/l, high-pressure nanofiltration is carried out through a high-pressure pump and a high-pressure nanofiltration membrane in steps to concentrate divalent salt in the low-pressure nanofiltration concentrated water, the high-pressure nanofiltration is provided with 1-2 sections, the high-pressure pump is provided with a frequency conversion device, the pressure is 5-10 MPa, and in order to utilize the energy of the high-pressure nanofiltration concentrated water, the high-pressure nanofiltration pump is arranged behind the concentrated water and in front of the high-pressure nanofiltration pumpEnergy recovery device, concentrated water concentration 2-4 times, SO4 2-65000-90000 mg/l, TDS (total dissolved solids) 100000-150000 mg/l, and concentrated water as sodium sulfate as raw material for freezing and evaporating crystallization. Purifying, nano-filtering and separating SO in low-pressure nano-filtering and high-pressure nano-filtering produced water4 2-In order to avoid affecting the purity of -valent sodium chloride, 2-3 sections are set for purification and nanofiltration according to the concentration requirement, and the water SO is produced by purification and nanofiltration4 2-30-80 mg/l, TDS (total dissolved solids) is 10000-25000 mg/l. Reverse osmosis is provided with 2-3 sections, a high-pressure variable frequency pump is adopted as a water inlet pump, an intersegmental pump is adopted, the pressure of the high-pressure pump is 2-5 MPa, concentrated water is concentrated by 2-4 times, and Cl is added-15000-30000 mg/l, TDS (total dissolved solids) 35000-60000 mg/l, SO4 2-Is 100 to 200 mg/l.
F in wastewater after reverse osmosis membrane concentration-、SiO2And the concentration of calcium and magnesium ions is increased, calcium fluoride, magnesium silicate and calcium hydroxide and magnesium hydroxide solid precipitates are generated by adding a calcium chloride solution, a magnesium oxide solution and a sodium carbonate solution respectively, and suspended matters generated above are removed by adopting a tubular microfiltration membrane. F in the wastewater treated by the method-SiO in an amount of 10 to 80mg/l2Ca in an amount of 10 to 30mg/l2+5-30 Mg/l of Mg2+The content is 1-10 mg/l, and the turbidity is less than 1 ntu.
The homogeneous electrodialysis device adopts 2-3 groups of parallel connection mode, the concentration of the concentrated solution is 2-4 times, and Cl-60000-95000 mg/l, TDS (total dissolved solids) 115000-150000 mg/l, SO4 2-500-2000 mg/l, and the concentrated solution is used as a sodium chloride evaporation crystallization raw material.
The evaporative crystallization device comprises a sodium chloride evaporative crystallization device, a sodium sulfate freezing crystallization device and an evaporative crystallization device, and the electrodialysis concentrated solution directly enters a sodium chloride evaporative crystallization, concentration, centrifugation and packaging system to obtain an industrial-grade sodium chloride product with the purity of more than 92%. In order to ensure the purity of sodium chloride salt, a small amount of concentrated solution is periodically discharged from a sodium chloride evaporation crystallization kettle, the concentrated solution is discharged to wastewater activated sludge after the miscellaneous salt is evaporated and concentrated, and the quantity of miscellaneous salt is less than 0.03m3H/ton of concentrated water; sodium sulfate concentrated solution is firstly put into a freezing and crystallizing device to generateNatrii sulfas (Na)2SO4 -r10H2And O), heating and melting mirabilite, and then entering an evaporation crystallization, centrifugation and drying system to obtain an industrial-grade sodium sulfate product with the purity of more than 95%. The evaporative crystallization device adopts MVR (mechanical vapor recompression) technology, so that the energy consumption is reduced to the maximum extent.
The invention has the beneficial effects that:
by adopting the coal particle activated carbon adsorption and regeneration technology, COD which is difficult to degrade in the coking wastewater is adsorbed to activated carbon particles, the COD is decomposed by a regeneration furnace, the COD in the wastewater is reduced to 100-200 mg/l, and the pollution and blockage of a subsequent membrane salt separation concentration system are prevented.
calcium chloride solution, magnesium oxide solution, sodium carbonate solution and sodium hydroxide solution with fixed concentration are prepared to respectively remove F-、SiO2Calcium and magnesium ions, and a technology of removing suspended matters by using a tubular microfiltration membrane, so that pollutants influencing the operation of the membrane are removed, and the stable operation of electrodialysis and a membrane system is ensured.
The high-pressure nanofiltration technology (the pressure is 5-10 MPa) is adopted, the high recovery rate of the sodium sulfate is ensured, the concentration reaches more than 12%, the high-pressure nanofiltration concentration of the sulfate with high concentration is the first creation of domestic engineering (the high-pressure nanofiltration module is used for the first time of industrialization, and the concentration of the sodium sulfate to more than 12% by adopting the high-pressure nanofiltration module is also the first achievement at home and abroad). In order to utilize the energy of the high-pressure nanofiltration concentrated water, an energy recovery device is arranged behind the concentrated water and in front of the high-pressure nanofiltration pump, so that the power and the operation energy consumption of the high-pressure pump are greatly reduced.
The combined technology of low-pressure nanofiltration, high-pressure nanofiltration, purification nanofiltration, reverse osmosis and electrodialysis is adopted to efficiently separate sodium chloride and sodium sulfate in the coking wastewater, and the sodium chloride (with the mass concentration of more than 15%) and sodium sulfate (with the mass concentration of more than 12%) solutions are concentrated to the maximum extent, so that the evaporation (freezing) crystallization amount is reduced, and the investment cost and the operation energy consumption of the whole device are reduced. Industrial-grade salt is obtained through an evaporation (freezing crystallization) system and can be sold as a product, zero discharge of coking wastewater is realized, and the process technology is an innovative process (first application) for zero discharge of coking wastewater at home and abroad.
Drawings
FIG. 1 is a flow chart of kinds of coking wastewater zero-discharge treatment, comprising:
1-water inlet pump, 2-full-automatic double-tank sand filter, 3-adsorption water inlet pump, 4-adsorption tower, 5-ultrafiltration, 6-softening water inlet pump, 7-weak acid resin bed, 8-low pressure nanofiltration water inlet pump, 9-low pressure nanofiltration, 10-high pressure nanofiltration water inlet pump, 11-high pressure nanofiltration, 12-sodium sulfate feed pump, 13-sodium sulfate freezing crystallization and evaporative crystallization, 14-purification nanofiltration, 15-reverse osmosis water inlet pump, 16-re-concentration reverse osmosis, 17-fluorine removal, silicon removal, calcium removal and magnesium removal, 18-tubular microfiltration circulating pump, 19-tubular microfiltration, 20-electrodialysis water inlet pump, 21-electrodialysis, 22-sodium chloride feed pump and 23-sodium chloride evaporative crystallization.
Detailed Description
The present invention is further illustrated in the following examples, which are to be construed as merely illustrative and not limitative of the remainder of the disclosure in any way whatsoever, and which are to be interpreted as open ended labels.
As shown in the figure, the coking wastewater amount after biochemical treatment is 120m3Perh, the coking wastewater water volume after the active carbon adsorption, softening and ultrafiltration and reverse osmosis membrane concentration treatment is 25m3The water quality index is as follows: pH 7.5, COD 550mg/l, Cl-9000mg/l, SO4 2-12000mg/l, Na+13000mg/l, F-150mg/l, 15mg/l of total cyanogen, 300mg/l of total nitrogen, 30mg/l of calcium, 10mg/l of magnesium, 30000mg/l of TDS (total dissolved solids) and 50mg/l of suspended matters (SS), pumping the wastewater into full-automatic sand filtration to remove the suspended matters (SS) to be below 5mg/l, wherein the full-automatic sand filtration comprises 2 filter tanks, backwashing is carried out by adopting filtered water, the filtered water enters an activated carbon adsorption tower, the activated carbon is coal-based briquetting crushed granular carbon, the grain size is 20-40 meshes, the adsorption iodine value is 1000, the activated carbon removes organic matters and SS in the wastewater by steps, the COD (chemical oxygen demand) water is reduced to 150mg/l, the activated carbon after adsorption saturation is regenerated and returned for use, the loss of about 5 percent of the activated carbon is supplemented by new carbon, the wastewater after the activated carbon adsorption enters 2 sets of ultrafiltration devices connected in parallel, and the ultrafiltration treatment capacity of each set is 20m3The step of ultrafiltration is to remove the particulate matters, macromolecular organic matters, microorganisms and the like in the wastewater from the fluid and dissolve the particulate matters, the macromolecular organic matters, the microorganisms and the likeThe components are separated, and the SDI value of the produced water of the ultrafiltration system is less than 3. The ultrafiltration water enters 2 sets of softening systems connected in parallel, calcium and magnesium ions in the wastewater are removed through weak acid cation resin, the calcium ions in the produced water are less than 2mg/l, the magnesium ions are less than 1mg/l, the resin saturated in adsorption is regenerated by hydrochloric acid and sodium hydroxide, and the regenerated waste liquid is neutralized and softened and then returns to the raw water for water inlet.
Pumping softened wastewater into a low-pressure nanofiltration device with the low-pressure nanofiltration treatment capacity of 26m3H, low-pressure nanofiltration is divided into 2 sections, the pressure of a feed pump is 1.8MPa, the highest outlet pressure of an intersegmental pump is 0.8MPa, and the low-pressure nanofiltration leads Cl in the wastewater to be-And SO4 2-Separation, concentrated water SO4 2-35000mg/l, TDS (total dissolved solids) 70000mg/l, and concentrated water amount 8.5m3H, removing high-pressure nanofiltration, and removing purification and nanofiltration of produced water. High pressure nanofiltration processing capacity of 12.5m3H, treating the low-pressure nanofiltration concentrated water and the concentrated water after subsequent freezing crystallization to obtain 4.0m3H, the highest outlet pressure of the high-pressure nanofiltration feed pump is 7MPa, the membrane group is sections, an energy recovery device is arranged behind the concentrated water and in front of the high-pressure nanofiltration pump, and the high-pressure nanofiltration concentrated water SO is4 2-85000mg/l, TDS (total dissolved solids) 135000mg/l, removing sodium sulfate from concentrated water, freezing and crystallizing, and purifying and nano-filtering the produced water. The water produced by low-pressure nanofiltration and high-pressure nanofiltration is used as raw material for purification and nanofiltration, and the treatment capacity is 36m3H, the highest outlet pressure of the feed pump is 1.0MPa, and in order to ensure the sulfate radical separation rate, 3 sections of purification and nanofiltration are separated, and the water SO produced by purification and nanofiltration are obtained4 2-80mg/l, TDS (total dissolved solids) is 1500mg/l, the water reuse rate is more than 90 percent, purified nanofiltration produced water enters a reverse osmosis device, and the reverse osmosis treatment capacity is 14m3The water inlet pump of the th section adopts a plunger pump, the highest outlet pressure is 3.8MPa, the highest outlet pressure of the interstage pump is 1.8MPa, the recovery rate of the produced water is more than 58 percent, the produced water meets the index requirement of industrial water, and concentrated water Cl is used-25000mg/l TDS (Total dissolved solids) 45000mg/l, SO4 2-It was 150 mg/l.
The reverse osmosis concentrated water sequentially enters a fluorine removal tank, a silicon removal tank and a calcium and magnesium removal tank, and the prepared calcium chloride solution (with the concentration of 28 percent) and the dissolved magnesium oxide (with the concentration of 5 at 60 ℃ C.) are used%) solution, 30% NaOH and 20% Na2CO3The solution is respectively added into a fluorine-removing tank, a silicon-removing tank and a calcium-magnesium-removing tank, each tank is provided with a stirring facility, the wastewater after the medicament treatment automatically flows into a tubular microfiltration water inlet tank, and sludge with high concentration is discharged from the bottom by gravity sedimentation to reach the concentration of 1.0m3Pumping the wastewater at the top of the tank into 2 sets of tubular microfiltration pumps which are operated in parallel to remove suspended matters in the wastewater, wherein the contents of fluorine, silicon dioxide, calcium and magnesium in the wastewater after the treatment are reduced to 50mg/l, and the SiO content is reduced to 50mg/l2Content of 15mg/l, Ca2+The content of Mg is 10Mg/l2+The content was 5mg/l and the turbidity was less than 1 ntu.
After defluorination, desilication and calcium and magnesium removal, the wastewater enters an electrodialysis device, 2 groups of electrodialysis are connected in parallel, 4 groups of electrodialysis are connected in series, the electrodialysis comprises a diaphragm, a frame, electrodes, a high-frequency power supply, a matched tank and the like, and the wastewater treatment capacity is 14m3H, concentrated water Cl after treatment-85000mg/l, TDS (Total dissolved solids) 135000mg/l, SO4 2-And (3) removing sodium chloride from the concentrated water to evaporate and crystallize the device at 1500mg/l, and returning the produced water to the low-pressure nanofiltration inlet water for recycling.
4.5m of concentrated water after high-pressure nanofiltration concentration3The mixture enters a sodium sulfate freezing and crystallizing system for generating 1.1 ton/hour (Na) of mirabilite2SO4 -r10H2O), 4m of crystallization refrigerating fluid3And/h, returning the mirabilite to the high-pressure nanofiltration feeding liquid, heating and melting the mirabilite, and then entering an evaporation crystallization, centrifugation and drying system to obtain an industrial-grade sodium sulfate -grade product with the purity of more than 95% at 0.5 ton/hour.
Concentrated water after electrodialysis concentration is 3m3And/h, entering an evaporation crystallization device, carrying out evaporation crystallization by adopting a conventional MVR mechanical vapor recompression technology to obtain 0.3 ton/hour of industrial secondary sodium chloride salt with the purity of more than 92 percent, simultaneously generating 2.6 ton/hour of industrial water and 0.1 ton/hour of miscellaneous salt concentrated solution, and sending the generated miscellaneous salt to a sludge device for wastewater treatment.
Through the technologies of wastewater pretreatment, membrane salt separation concentration, electrodialysis concentration and freezing evaporation crystallization, fluorine, calcium, magnesium and organic matters in wastewater are removed, a very small amount of sludge concentrated solution is removed to an original wastewater sludge system, industrial-grade sodium sulfate and sodium chloride products are obtained, and zero discharge of coking wastewater is realized.
Of course, persons skilled in the art should recognize that the above-described embodiments are illustrative only, and not limiting, and that changes and modifications to the above-described embodiments are intended to fall within the scope of the appended claims, as long as they fall within the true spirit and scope of the present invention.

Claims (10)

1, kinds of coking wastewater membrane concentration divides salt zero release processing method, characterized by, including the following step:
(1) pretreatment of coking wastewater: the pretreatment of the coking wastewater comprises full-automatic sand filtration, activated carbon adsorption regeneration, ultrafiltration and softening;
the quality indexes of the coking wastewater are as follows: pH of 7 to 8, COD of 300 to 550mg/l, Cl-8000-12000 mg/l of SO4 2-10000-14000 mg/l of Na+Is 11000 to 15000mg/l, F-50-200 mg/l of total cyanogen, 10-20 mg/l of total nitrogen, 200-500 mg/l of total nitrogen, 10-30 mg/l of calcium, 5-10 mg/l of magnesium, 20000-40000 mg/l of TDS, and 30-50 mg/l of suspended matters;
the coking wastewater is thrown into full-automatic sand for filtering, suspended matters in the coking wastewater are removed to be below 5mg/l, filtered water enters an activated carbon adsorption tower, and the activated carbon is coal-based briquette crushed granular carbon with the particle size: 5-50 meshes, wherein the adsorption iodine value is 800-1100, the effluent of the activated carbon adsorption tower enters an ultrafiltration device, the ultrafiltration produced water enters 2 sets of softening systems connected in parallel, calcium and magnesium ions in the wastewater are removed through weak acid cation resin, the produced water calcium ions are less than 2mg/l, and the magnesium ions are less than 1 mg/l;
(2) membrane salt separation concentration treatment: the membrane salt separation concentration treatment comprises low-pressure nanofiltration, high-pressure nanofiltration, purification nanofiltration and reverse osmosis treatment;
the softened wastewater is pumped into a low-pressure nanofiltration device, and the low-pressure nanofiltration capacity is 20-30 m3H, low-pressure nanofiltration is provided with 2-3 sections, an intersegmental pump is arranged in the middle, and the low-pressure nanofiltration membrane is used for filtering the wastewater -valent and divalent ions in the wastewater are separated, the concentrated water is concentrated by 2-4 times, and SO is added4 2-25000-45000 mg/l, TDS 50000-80000 mg/l, high-pressure nanofiltration is carried out on concentrated water, produced water is purified and nanofiltered, divalent salt in the low-pressure nanofiltration concentrated water is concentrated in steps through a high-pressure pump and the high-pressure nanofiltration membrane, the high-pressure nanofiltration is provided with 1-2 sections, the high-pressure pump is provided with a frequency conversion device, the pressure is 5-10 MPa, an energy recovery device is arranged behind the concentrated water and in front of the high-pressure nanofiltration pump, the concentrated water is concentrated by 2-4 times, and SO is recycled4 2-65000-90000 mg/l, TDS 100000-150000 mg/l, concentrated water as sodium sulfate freezing and evaporation crystallization raw material, and produced water for purification and nanofiltration;
purified nanofiltration produced water enters a reverse osmosis device, and the reverse osmosis treatment capacity is 10-20 m3The reverse osmosis is arranged at 2-3 sections, the water inlet pump adopts a high-pressure variable-frequency pump, the section pump adopts an intersegmental pump, the pressure of the high-pressure pump is 2-5 MPa, the concentrated water is concentrated by 2-4 times, and Cl-15000-30000 mg/l, TDS 35000-60000 mg/l, SO4 2-100-200 mg/l;
(3) concentration treatment, fluorine and silicon removal, electrodialysis concentration and evaporative crystallization;
respectively adding a calcium chloride solution with the concentration of 20-35%, a magnesium oxide or magnesium chloride solution with the concentration of 5-20% and a sodium carbonate solution with the concentration of 10-25% into the wastewater after the concentration of the reverse osmosis membrane to generate solid precipitates, and removing the generated suspended matters by using a tubular microfiltration membrane; after defluorination, desilication and calcium and magnesium removal, the wastewater enters an electrodialysis device, the electrodialysis device adopts a parallel connection mode of 2-3 groups, concentrated solution is concentrated by 2-4 times, the concentrated solution is used as a sodium chloride evaporation crystallization raw material, and produced water is returned to the low-pressure nanofiltration inlet water for recycling;
directly feeding the electrodialysis concentrated solution into a sodium chloride evaporation crystallization, concentration, centrifugation and packaging system to obtain an industrial grade sodium chloride product with the purity of more than 92%; and (3) firstly putting the sodium sulfate concentrated solution into a freezing and crystallizing device to generate mirabilite, heating and melting the mirabilite, and then putting the mirabilite into an evaporation, crystallization, centrifugation and drying system to obtain an industrial-grade sodium sulfate product with the purity of more than 95%.
2. The coking wastewater membrane concentration salt separation zero-emission treatment method of claim 1, wherein the full-automatic sand filtration is a full-automatic double-tank sand filter, back washing is performed by using filtered water, quartz sand is used as the sand, the particle size of a filter material is 0.25-0.55 mm, and the filtering flow rate is 0.3-0.8 m/s.
3. The coking wastewater membrane concentration salt separation zero-emission treatment method of claim 1, wherein the residence time of the filtered water in the activated carbon adsorption tower is about 1-3 hours.
4. The coking wastewater membrane concentration salt separation zero-emission treatment method of claim 1, wherein the adsorbed activated carbon is regenerated by a regenerator and then is recycled, loss is periodically supplemented, and COD in the wastewater treated by the activated carbon is reduced to 100-200 mg/l.
5. The coking wastewater membrane concentration salt separation zero-emission treatment method of claim 1, wherein the SDI value of the water produced by the ultrafiltration system is less than 3.
6. The coking wastewater membrane concentration salt separation zero-discharge treatment method of claim 1, wherein the SO in the low-pressure nanofiltration and high-pressure nanofiltration product water is purified, separated by nanofiltration4 2-In order to avoid affecting the purity of -valent sodium chloride, 2-3 sections are set for purification and nanofiltration according to the concentration requirement, and the water SO is produced by purification and nanofiltration4 2-30-80 mg/l, TDS is 10000-25000 mg/l.
7. The method for membrane concentration, salt separation and zero discharge of coking wastewater according to claim 1, wherein F in wastewater after reverse osmosis membrane concentration is treated by adding calcium chloride solution, magnesium oxide solution and sodium carbonate solution respectively through tubular microfiltration membrane-SiO in an amount of 10 to 80mg/l2Ca in an amount of 10 to 30mg/l2+5-30 Mg/l of Mg2+The content is 1-10 mg/l, and the turbidity is less than 1 ntu.
8. The coking wastewater membrane concentration salt-separation zero-emission treatment method as claimed in claim 1, wherein the electrodialysis device adopts 2-3 groups of parallel connection, the electrodialysis device comprises a membrane, a frame, electrodes, a high-frequency power supply, a matching tank and the like, and the amount of wastewater treated is 10-20 m3/h。
9. The coking wastewater membrane concentration salt-separation zero-emission treatment method of claim 1, wherein the evaporative crystallization device comprises a sodium chloride evaporative crystallization device and a sodium sulfate freezing crystallization and evaporative crystallization device.
10, coking wastewater membrane concentration and salt separation zero-emission treatment system is characterized by sequentially comprising a water inlet pump (1), a 2-full-automatic double-tank sand filter (2), an adsorption water inlet pump (3), an adsorption tower (4), ultrafiltration (5), a softening water inlet pump (6), a weak acid resin bed (7), a low-pressure nanofiltration water inlet pump (8), a low-pressure nanofiltration pump (9), a high-pressure nanofiltration water inlet pump (10), a high-pressure nanofiltration pump (11), a purification nanofiltration pump (14), a reverse osmosis water inlet pump (15), a re-concentration reverse osmosis pump (16), a fluorine, silicon, calcium and magnesium removal pump (17), a tubular microfiltration circulating pump (18), a tubular microfiltration pump (19), an electrodialysis water inlet pump (20), electrodialysis (21), a sodium chloride feed pump (22) and a sodium chloride evaporative crystallization (23), wherein the high-pressure nanofiltration pump (11) is further sequentially connected with a sodium sulfate feed pump (12), a sodium sulfate freezing crystallization and an evaporative crystallization pump (13), an outlet of the purification nanofiltration pump (14) is further connected with the low-pressure nanofiltration water inlet of the purification nanofiltration pump.
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CN114195328B (en) * 2021-12-02 2024-03-19 北京拓凯化工技术有限公司 Advanced treatment method for steel industry sewage and wastewater
CN114906975A (en) * 2022-02-17 2022-08-16 北京欧美环境工程有限公司 Zero-discharge treatment process for coking wastewater
CN114656093A (en) * 2022-04-22 2022-06-24 倍杰特集团股份有限公司 Coking wastewater zero-discharge pretreatment device and method
US11611099B1 (en) 2022-05-09 2023-03-21 Rahul S Nana Reverse electrodialysis cell and methods of use thereof
US11502323B1 (en) 2022-05-09 2022-11-15 Rahul S Nana Reverse electrodialysis cell and methods of use thereof
US11563229B1 (en) 2022-05-09 2023-01-24 Rahul S Nana Reverse electrodialysis cell with heat pump
US11502322B1 (en) 2022-05-09 2022-11-15 Rahul S Nana Reverse electrodialysis cell with heat pump
US11699803B1 (en) 2022-05-09 2023-07-11 Rahul S Nana Reverse electrodialysis cell with heat pump
CN114751564A (en) * 2022-05-23 2022-07-15 浙江佰辰低碳科技有限公司 Coking wastewater treatment method
CN115340251A (en) * 2022-07-04 2022-11-15 哈尔滨工业大学（深圳） Carbon-neutralized zero-emission industrial water treatment system and treatment method
CN115093081A (en) * 2022-07-05 2022-09-23 中冶节能环保有限责任公司 Advanced treatment method and treatment system for coking wastewater of steel plant
CN115093081B (en) * 2022-07-05 2024-01-09 中冶节能环保有限责任公司 Deep treatment method and treatment system for coking wastewater of steel plant
CN115353237A (en) * 2022-07-29 2022-11-18 中冶焦耐(大连)工程技术有限公司 Process and system for realizing zero discharge and resource utilization of coking wastewater
US11855324B1 (en) 2022-11-15 2023-12-26 Rahul S. Nana Reverse electrodialysis or pressure-retarded osmosis cell with heat pump
CN116022965B (en) * 2023-02-01 2023-06-02 深圳永清水务有限责任公司北京分公司 Coking wastewater zero discharge treatment system and process
CN116022965A (en) * 2023-02-01 2023-04-28 深圳永清水务有限责任公司北京分公司 Coking wastewater zero discharge treatment system and process
CN117228906A (en) * 2023-11-15 2023-12-15 开源环境科技集团有限公司 Printing and dyeing wastewater treatment process
CN117228906B (en) * 2023-11-15 2024-02-20 开源环境科技集团有限公司 Printing and dyeing wastewater treatment process

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