CN108249614B - Method and device for treating high-concentration emulsion wastewater - Google Patents
Method and device for treating high-concentration emulsion wastewater Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 32
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- 238000000108 ultra-filtration Methods 0.000 claims abstract description 88
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 74
- 230000003647 oxidation Effects 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 64
- 230000003197 catalytic effect Effects 0.000 claims abstract description 60
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000001914 filtration Methods 0.000 claims abstract description 27
- 239000012141 concentrate Substances 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000012466 permeate Substances 0.000 claims abstract description 7
- 239000003921 oil Substances 0.000 claims description 43
- 239000003054 catalyst Substances 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000007800 oxidant agent Substances 0.000 claims description 9
- 230000001590 oxidative effect Effects 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
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- 229910052751 metal Inorganic materials 0.000 claims description 4
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
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- 241001391944 Commicarpus scandens Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
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- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
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- 150000001868 cobalt Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000002390 heteroarenes Chemical class 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
- C02F2101/327—Polyaromatic Hydrocarbons [PAH's]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a method for treating high-concentration emulsion wastewater, which comprises the following steps: filtering the high-concentration emulsion wastewater by an inorganic membrane to perform oil-water separation to obtain an inorganic membrane concentrated solution and a clear solution; the clear liquid enters a catalytic oxidation system for catalytic oxidation treatment; the effluent after catalytic oxidation treatment is adsorbed by activated carbon and then enters an ultrafiltration membrane device for ultrafiltration treatment, so that ultrafiltration concentrate and ultrafiltration membrane effluent are obtained; the ultrafiltration concentrated solution returns to the catalytic oxidation system, and is mixed with clear liquid to be oxidized again; the effluent of the ultrafiltration membrane enters a reverse osmosis membrane device for reverse osmosis treatment to obtain reverse osmosis concentrated solution and permeate, and the reverse osmosis concentrated solution returns to a catalytic oxidation system for oxidation treatment. The inorganic membrane separation method can resist high-oil and high-solid content treatment, and the whole system has better stability and stronger impact resistance; the catalytic oxidation technology has small dosage of medicament, is a pure chemical treatment technology, and finally cannot generate pollutants such as concentrated solution, sludge and the like.
Description
Technical Field
The invention belongs to the field of wastewater treatment, and particularly relates to a method and a device for treating high-concentration emulsion wastewater.
Background
The emulsion is widely used in metal processing processes such as grinding, forging and the like, and mainly has the functions of lubrication, cooling, surface cleaning and corrosion prevention. With the extension of the service time, the alternation of cold and heat and the degradation of microorganisms can cause the deterioration of the waste liquid, and the original characteristics and the utility are lost, so the waste liquid which needs to be treated is continuously generated.
The emulsion comprises base oil (mineral oil, vegetable oil and synthetic oil), fatty acid, surfactant (nonionic and anionic), auxiliary surfactant, anticorrosive, antibacterial agent and various additives. The applications are different, and thus the kinds and components are very different depending on the providers even if the applications are the same. Furthermore, each emulsion is protected by patent, and the specific chemical composition is unknown, which increases the difficulty of wastewater treatment. Generally, emulsions are classified into Q/W type and W/O type according to the degree of combination of the surfactant with water and oil. At present, the emulsion commonly used in metal processing is of the Q/W type, and is more difficult to treat than other emulsions due to stable chemical properties and very complex physicochemical properties.
The existing emulsion wastewater treatment generally adopts a chemical demulsification, air floatation/coagulation sedimentation and biochemical process, or the demulsification, air floatation sedimentation and other wastewater are mixed and diluted to enter a biochemical system. However, these conventional solutions all have the following drawbacks:
1. the demulsification effect is unstable, the oil content of clear liquid after air floatation precipitation is high, and the subsequent treatment process is influenced;
2. the air floatation or coagulating sedimentation can only be used for dangerous waste treatment, wherein the water content is higher, so that the treatment cost is higher;
3. the sediment is difficult to be dehydrated and solidified by adopting a conventional process, and the normal operation of dehydration equipment (plate and frame filter pressing) is seriously influenced;
4. the biochemical system is unstable in operation, and the oxygen content in the water body is low due to the large oil content, so that the biochemical system is easy to break down.
With the continuous development of technology, membrane technology is increasingly used in the water treatment industry. Patent CN103030252A discloses a membrane treatment process of emulsion wastewater, and the method has better quality of final effluent water; however, this method can result in a membrane concentrate that is not handled and can cause environmental pollution.
The high-concentration emulsion wastewater is high-concentration nondegradable COD wastewater, and the conventional chemical demulsification, air floatation/coagulating sedimentation and biochemical process has a plurality of problems and disadvantages. Therefore, further research and exploration are necessary for the treatment process of the difficult-to-treat high-concentration emulsion wastewater.
Disclosure of Invention
The invention aims to provide a green and environment-friendly high-concentration emulsion wastewater treatment method, which does not need to add any medicament, adopts an inorganic membrane for pretreatment, and removes oil in the high-concentration emulsion wastewater in a pure physical process; inorganic membrane effluent is treated by an ECO catalytic oxidation system to remove most of COD and chromaticity, and finally the effluent can reach the discharge standard by ultrafiltration and reverse osmosis membrane treatment, and concentrated solution of the reverse osmosis membrane can be returned to the ECO catalytic oxidation system for treatment, so that no concentrated solution is generated.
In order to achieve the purpose of the invention, the following technical scheme is adopted:
a method for treating high-concentration emulsion wastewater comprises the following steps:
(1) Filtering the high-concentration emulsion wastewater by an inorganic membrane to perform oil-water separation to obtain an inorganic membrane concentrated solution and a clear solution;
(2) Introducing the clear liquid into a catalytic oxidation system for catalytic oxidation treatment;
(3) The effluent water after the catalytic oxidation treatment in the step (2) is absorbed by active carbon and then enters an ultrafiltration membrane device for ultrafiltration treatment, and large-particle suspended matters and partial COD are removed to obtain ultrafiltration concentrate and ultrafiltration membrane effluent water;
(4) Returning the ultrafiltration concentrated solution to a catalytic oxidation system, mixing the ultrafiltration concentrated solution with the clear solution obtained in the step (1), and carrying out oxidation treatment again; the effluent of the ultrafiltration membrane enters a reverse osmosis membrane device for reverse osmosis treatment to obtain reverse osmosis concentrated solution and permeate, and the reverse osmosis concentrated solution returns to a catalytic oxidation system for oxidation treatment; the permeate reaches the standard of reuse water and is directly reused.
The COD of the high-concentration emulsion wastewater is 100000 ～ 400000mg/L, and the oil content is 2000-10000 mg/L. The high-concentration emulsion wastewater contains at least one of the following intractable COD components: polycyclic aromatic hydrocarbons, heteroaromatic compounds, chlorinated aromatic compounds, nitroaromatic compounds, aromatic amines, aromatic olefins, aromatic esters, biphenyls or organic cyanides.
In the step (1), the high-concentration emulsion wastewater is filtered by an inorganic membrane in an inorganic membrane filter device to complete oil-water separation.
The inorganic film is a ceramic film, a metal film or a silicon carbide film and the like; the pore diameter of the inorganic membrane is between 0.1 and 1.0 mu m. The operating pressure of the inorganic membrane filtration is between 0.1 and 0.4 MPa. The inorganic membrane is high temperature resistant, and the temperature for filtering the inorganic membrane is unlimited. The high-concentration emulsified liquid wastewater is filtered by an inorganic membrane, and emulsified oil with the aperture larger than the membrane is intercepted by a screening principle, and aqueous solution with the aperture smaller than the membrane is permeated through the membrane to obtain concentrated solution and clear solution of the inorganic membrane.
The inorganic membrane concentrate has high oil content and is directly burnt.
In the step (2), clear liquid obtained by filtering through an inorganic membrane is filtered through a cartridge filter, is sequentially heated to 200-260 ℃ through a heat exchanger and a heat conducting oil heat exchanger, and enters a catalytic oxidation system for catalytic oxidation treatment. The catalytic oxidation treatment is CWAO catalytic wet oxidation treatment. The method for treating the CWAO by the catalytic wet oxidation method comprises the following steps: continuously introducing the clear liquid into a catalytic oxidation system for catalytic wet oxidation treatment, keeping the retention time for 1-2 h, carrying out oxidation reaction under the conditions of the temperature of 200-260 ℃ and the pressure of 5-8 MPa under the action of a catalyst, and oxidizing and decomposing organic matters into CO by using an oxidant 2 、H 2 O and N 2 Harmless substances are added, so that the aim of purification is fulfilled; wherein the catalyst takes one or a plurality of transition metal oxides in transition metal oxides as active ingredients and Al 2 O 3 The catalyst is supported, the loading of the metal oxide is 2-10 wt% or the transition metal salt; the catalyst is used in an amount of 250 to 350 g/ton of water, preferably 300 g/ton of water, based on the amount of the active ingredient (i.e., excluding the weight of the carrier); the oxidant is air, oxygen or hydrogen peroxide, and the like, and the oxidant is calculated by oxygenThe amount of air or oxygen is 2-3.5 m 3 /h, preferably 3m 3 /h。
The transition metal is selected from Cu, fe, ni, co, mn; the transition metal salt is selected from copper salt, ferrous salt, nickel salt, cobalt salt and manganese salt; specifically, the transition metal salt may be selected from hydrochloride, sulfate, nitrate, fluoroborate (BF 4 - ) Acetate.
In the step (3), the effluent after the catalytic oxidation treatment in the step (2) firstly enters a heat exchanger to exchange heat with clear liquid to be subjected to the catalytic oxidation, then enters a cooler to be further cooled to 20-40 ℃, and enters an ultrafiltration membrane device to carry out ultrafiltration treatment after being adsorbed by active carbon. The clear liquid to be fed into the catalytic oxidation system exchanges heat with the effluent of the catalytic oxidation system through the heat exchanger, so that the heat utilization rate is improved, and the energy consumption is reduced. The main purpose of the activated carbon adsorption is to reduce the chromaticity and COD content in the wastewater, reduce the pollution of organic matters to a membrane system and ensure the operation stability of a subsequent membrane system.
The ultrafiltration membrane adopted by the ultrafiltration membrane device is a hollow fiber ultrafiltration membrane, and the ultrafiltration membrane is made of polysulfone, polyvinyl chloride, polypropylene, polyacrylonitrile or polyvinylidene fluoride and the like. The average pore diameter of the ultrafiltration membrane is 5-100 nm, or the ultrafiltration membrane is a membrane with the molecular weight cut-off of 1000-200000 Da. The selection of the aperture of the ultrafiltration membrane has important influence on the ultrafiltration process, and too large aperture can lower the COD interception rate in the wastewater, so that the wastewater treatment is not up to standard, and too small aperture can lower the filtration flux and the wastewater treatment capacity.
The operation temperature of the ultrafiltration membrane device is controlled to be 20-40 ℃, the service life of the ultrafiltration membrane can be directly influenced by the excessively high temperature selection, and the excessively low temperature selection can lead to the excessively low flux of the filtration process.
The filtration pressure of the ultrafiltration membrane device is controlled to be 0.05-0.2 MPa, the pressure is too high, the energy consumption of the system is increased, membrane pollution is easy to form, and the operation of an ultrafiltration system is directly influenced; too low a pressure may result in too low a filtration flux of the ultrafiltration membrane system.
The membrane surface flow rate of the wastewater is between 0.5 and 10 m/s.
In the step (4), the reverse osmosis membrane of the reverse osmosis membrane device can be made of cellulose acetate, polyamide, polyester, polyimide, polysulfone, polyethersulfone or polyvinyl alcohol; the operation pressure of the reverse osmosis device is 0.5-3.0 MPa, and the operation temperature is 20-40 ℃. The reverse osmosis treatment mainly removes COD, chromaticity and salt in the wastewater.
The reverse osmosis concentrated solution contains more salt, has high organic matter content and high chromaticity value, and can be mixed with the clear liquid obtained by the inorganic membrane filtration in the step (1) and the ultrafiltration concentrated solution obtained in the step (2) and returned to the catalytic oxidation system for oxidation treatment.
The invention also aims to provide a treatment device for high-concentration emulsion wastewater, which comprises an inorganic membrane filtering device, a clean fluid tank, a cartridge filter, a catalytic oxidation system, an activated carbon tank, an intermediate water tank, an ultrafiltration membrane device and a reverse osmosis membrane device; the water inlet of the inorganic membrane filtering device is connected with a raw water tank for collecting high-concentration emulsion wastewater, the clear liquid outlet of the inorganic membrane filtering device is connected with a clear liquid tank, and the outlet of the clear liquid tank is connected with the water inlet of the catalytic oxidation system through a cartridge filter; the water outlet of the catalytic oxidation system is connected with the water inlet of the ultrafiltration membrane device through the active carbon tank, the water outlet of the ultrafiltration membrane device is connected with the water inlet of the reverse osmosis membrane device, the ultrafiltration membrane effluent is sent into the reverse osmosis membrane device for reverse osmosis treatment, and the concentrated solution outlet of the ultrafiltration membrane device is connected with the clear solution tank; and a concentrated solution outlet of the reverse osmosis membrane device is connected with a clear solution tank.
The catalytic oxidation system comprises a heat exchanger, a heat conduction oil heat exchanger, a catalytic reaction tower, a cooler and an oxidation water outlet tank, wherein the heat exchanger and the heat conduction oil heat exchanger are sequentially connected, a process medium outlet of the heat conduction oil heat exchanger is connected with an inlet of the catalytic reaction tower, a water outlet of the oxidation reaction tower is connected with a heat transfer medium inlet of the heat exchanger, and a heat transfer medium outlet of the heat exchanger is connected with the oxidation water outlet tank through the cooler so that effluent water of catalytic oxidation treatment enters the heat exchanger to exchange heat with clear liquid to be fed into the catalytic reaction tower, and then enters the cooler for further cooling to 20-40 ℃.
The heat conduction oil heat exchanger is connected with the matched oil furnace through a heat conduction oil inlet pipe and a heat conduction oil outlet pipe.
An oxidant input pipe is arranged on the process medium inlet pipe of the heat exchanger and used for inputting an oxidant.
And a concentrated solution outlet of the inorganic membrane filtering device is connected with a concentrated solution tank.
An intermediate water tank is arranged between the active carbon tank and the ultrafiltration membrane device; an ultrafiltration water producing tank is arranged on a connecting pipeline between the water outlet of the ultrafiltration membrane device and the water inlet of the reverse osmosis membrane device.
And a permeate outlet of the reverse osmosis membrane device is connected with a reverse osmosis water producing tank.
Compared with the prior art, the invention has the beneficial effects that:
the method for treating the high-concentration emulsion wastewater can lead the wastewater to reach the dischargeable standard, and is a green and environment-friendly treatment process. The concrete steps are as follows:
1. the inorganic membrane separation can resist high-oil and high-solid content treatment, the whole system has better stability and stronger impact resistance, the inorganic membrane is used for carrying out oil-water separation on the high-concentration emulsion wastewater, suspended matters and oil in the wastewater are removed, and the inorganic membrane concentrate is burnt.
2. The inorganic membrane clear liquid is treated by a catalytic oxidation system, the catalytic oxidation technology has small dosage of medicament, is a pure chemical treatment technology, removes most COD and chromaticity, and finally does not produce pollutants such as concentrated solution, sludge and the like.
3. The catalytic oxidation effluent is treated by activated carbon, so that COD and chromaticity values are further reduced, the quality of reverse osmosis effluent is improved, and the problems of reverse osmosis membrane pollution and low flux are solved. And then enters a double-membrane system to be subjected to ultrafiltration and reverse osmosis membrane treatment, the rejection rate of the reverse osmosis membrane is high, the color value removal rate is high, the flux is stable, and finally the effluent can reach the discharge standard. The ultrafiltration concentrated solution and the reverse osmosis concentrated solution can be returned to the catalytic oxidation system for treatment, and no concentrated solution is generated finally.
Drawings
FIG. 1 is a schematic diagram of an apparatus for treating emulsion waste water according to the present invention.
The device comprises a 1-inorganic membrane filter device, a 2-clean liquid tank, a 3-concentrated liquid tank, a 4-security filter, a 5-heat exchanger, a 6-heat conduction oil heat exchanger, a 7-oil furnace, an 8-catalytic reaction tower, a 9-cooler, a 10-oxidation water outlet tank, a 11-active carbon tank, a 12-intermediate water tank, a 13-ultrafiltration membrane device, a 14-ultrafiltration water production tank, a 15-reverse osmosis membrane device, a 16-reverse osmosis water production tank, a 17-raw water tank and an 18-oxidant input pipe.
Detailed Description
In order to further explain the technical scheme of the invention, the invention is explained in detail by specific examples.
As shown in fig. 1, a treatment device for high-concentration emulsion wastewater comprises an inorganic membrane filtering device 1, a clear liquid tank 2, a concentrated liquid tank 3, a cartridge filter 4, a catalytic oxidation system, an activated carbon tank 11, an intermediate water tank 12, an ultrafiltration membrane device 13, an ultrafiltration water producing tank 14 and a reverse osmosis membrane device 15; the water inlet of the inorganic membrane filtering device 1 is connected with a raw water tank 17 for collecting high-concentration emulsion wastewater, the clear liquid outlet of the inorganic membrane filtering device 1 is connected with a clear liquid tank 2, and the concentrated liquid outlet of the inorganic membrane filtering device 1 is connected with a concentrated liquid tank 3; the outlet of the clean liquid tank 2 is connected with the water inlet of the catalytic oxidation system through a cartridge filter 4; the catalytic oxidation system comprises a heat exchanger 5, a heat conduction oil heat exchanger 6, an oil furnace 7 matched with the heat conduction oil heat exchanger 6, a catalytic reaction tower 8, a cooler 9 and an oxidation water outlet tank 10, wherein a process medium inlet of the heat exchanger 5 is connected with a water outlet of a security filter 4, an oxidant input pipe 18 is arranged on a process medium inlet pipe of the heat exchanger 5 and is used for inputting an oxidant, the heat exchanger 5 and the heat conduction oil heat exchanger 6 are sequentially connected, a process medium outlet of the heat conduction oil heat exchanger 6 is connected with an inlet of the catalytic reaction tower 8, a water outlet of the oxidation reaction tower 8 is connected with a heat transfer medium inlet of the heat exchanger 5, and a heat transfer medium outlet of the heat exchanger 5 is connected with the oxidation water outlet tank 10 through the cooler 9 so that effluent water subjected to catalytic oxidation treatment enters the heat exchanger 5 to exchange heat with clear liquid to be fed into the catalytic reaction tower and then enters the cooler 9 for further cooling to 20-40 ℃; the water outlet of the oxidation water outlet tank 10 in the catalytic oxidation system is connected with the water inlet of the ultrafiltration membrane device 13 through the activated carbon tank 11, the water outlet of the ultrafiltration membrane device 13 is connected with the ultrafiltration water producing tank 14, the water outlet of the ultrafiltration water producing tank 14 is connected with the water inlet of the reverse osmosis membrane device 15, the ultrafiltration membrane water outlet is sent into the reverse osmosis membrane device 15 for reverse osmosis treatment, and the concentrated solution outlet of the ultrafiltration membrane device 14 is connected with the clear solution tank 2; the concentrated solution outlet of the reverse osmosis membrane device 15 is connected with the clear solution tank 2, and the permeate outlet of the reverse osmosis membrane device 15 is connected with the reverse osmosis water producing tank 16.
The heat conduction oil heat exchanger 6 is connected with the matched oil furnace 7 through a heat conduction oil inlet pipe and a heat conduction oil outlet pipe.
An intermediate water tank 12 is arranged between the activated carbon tank 11 and the ultrafiltration membrane device 13.
The specific techniques or conditions are not specified in the examples, and are carried out according to techniques or conditions described in the literature in the art (for example, refer to Xu Naping et al, inorganic membrane separation techniques and applications, chemical industry Press, 2003) or according to the product specifications. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The emulsified liquid wastewater (COD 200g/L, chromaticity 800, salt content 0.5% and oil content 5600 mg/L) is first filtered by an inorganic ceramic membrane filter, the pore diameter of the ceramic membrane is 50nm, and oil-water separation is carried out under the operating pressure of 0.3MPa to obtain inorganic membrane concentrated solution and clear solution. The oil content of the inorganic membrane concentrate is 60g/L, and the inorganic membrane concentrate is directly burnt; clear liquid (COD 31200mg/L, chromaticity 790, salt content 0.5%, oil content 300 mg/L) is heated by a heat exchanger and a heat-conducting oil heat exchanger in sequence, and then the temperature reaches 230 ℃, and is continuously introduced into a catalytic reaction tower, and CuO/Al is filled in the catalytic reaction tower 2 O 3 The catalyst has a CuO loading of 4.46 wt%, and the catalyst is 300 g/ton of wastewater to be treated based on the active ingredient CuO of the catalyst, and pure oxygen is continuously introduced into the system (the introducing amount is 3 m) 3 And/h), the residence time of the wastewater in the catalytic reaction tower is 1h, and the catalytic oxidation reaction is carried out at 230 ℃ and 5.0 MPa. The effluent (COD content is 200mg/L, conductivity 8000 mu s/cm, chromaticity 50) of the catalytic reaction tower exchanges heat with the clear liquid to be introduced into the catalytic reaction tower in a heat exchanger and then enters a cooler for further introductionCooling to 30-40 ℃, sending into an active carbon tank, pumping into an ultrafiltration membrane device (the ultrafiltration membrane is a hollow fiber ultrafiltration membrane with the average pore diameter of 100nm and the membrane surface flow rate of 5 m/s) for ultrafiltration after adsorption by active carbon, controlling the filtration temperature of the ultrafiltration membrane to be 30-40 ℃, controlling the transmembrane pressure difference to be 0.1MPa, returning ultrafiltration concentrate to a catalytic reaction tower, and mixing the ultrafiltration concentrate with the obtained clear liquid for oxidation treatment again; filtering the effluent of the ultrafiltration membrane in a reverse osmosis membrane device (the reverse osmosis membrane is made of cellulose acetate), controlling the filtering temperature to be 30-40 ℃ and the transmembrane pressure difference to be 1.5MPa; after the treatment by the double-membrane system, the COD content is reduced from 200mg/L to 1.1mg/L, the chromaticity is reduced from 50 to 1, the conductivity is reduced from 8000 mu s/cm to 200 mu s/cm, and the effluent can be directly recycled. And the COD content of the reverse osmosis concentrated solution is 650mg/L, and the reverse osmosis concentrated solution and the inorganic membrane filtered clear solution can be mixed and then enter a catalytic oxidation tower again for treatment.
Example 2
The emulsified liquid wastewater (COD 250g/L, chromaticity 900, salt content 0.6% and oil content 6000 mg/L) is firstly filtered by an inorganic ceramic membrane filter device, the pore diameter of the ceramic membrane is 50nm, and oil-water separation is carried out under the operating pressure of 0.3MPa to obtain inorganic membrane concentrated solution and clear solution. The oil content of the inorganic membrane concentrate is 65g/L, and the inorganic membrane concentrate is directly subjected to incineration treatment; clear liquid (COD 25200mg/L, chromaticity 850, salt content 0.6%, oil content 330 mg/L) is heated by a heat exchanger and a heat transfer oil heat exchanger in sequence, and then the temperature reaches 240 ℃, the clear liquid is continuously introduced into a catalytic reaction tower, and the catalytic reaction tower is filled with CuO-MnO/Al 2 O 3 The catalyst (CuO loading 3.53 wt%, mnO loading 2.34 wt%, based on the total amount of the active ingredients CuO and MnO of the catalyst, the catalyst dosage is 300 g/ton of wastewater to be treated), and pure oxygen is continuously introduced into the system (the introduction amount is 3 m) 3 And/h), the residence time of the wastewater in the catalytic reaction tower is 1.5h, and the catalytic oxidation reaction is carried out at 240 ℃ and 4.5 MPa. The effluent (COD content is 180mg/L, conductivity 9300 mu s/cm, chroma 60) of the catalytic oxidation tower is subjected to heat exchange with clear liquid which is to enter the catalytic reaction tower in a heat exchanger, then enters a cooler for further cooling to 30-40 ℃, is sent into an activated carbon tank, is adsorbed by activated carbon and is pumped into an ultrafiltration membrane device (the ultrafiltration membrane is a hollow fiber ultrafiltration membrane, average pore diameter is 100 nm),The flow rate of the membrane surface is 6 m/s), the filtration temperature of an ultrafiltration membrane is controlled to be 30-40 ℃, the transmembrane pressure difference is 0.1MPa, the ultrafiltration concentrated solution is returned to a catalytic reaction tower, and the ultrafiltration concentrated solution is mixed with the obtained clear solution for oxidation treatment again; filtering the effluent of the ultrafiltration membrane in a reverse osmosis membrane device (the reverse osmosis membrane is made of cellulose acetate), controlling the filtering temperature to be 30-40 ℃ and the transmembrane pressure difference to be 1.5MPa; after the treatment by the double-membrane system, the COD content is reduced from 180mg/L to 1mg/L, the chromaticity is reduced from 50 to 1, the conductivity is reduced from 9300 mu s/cm to 230 mu s/cm, and the effluent can be directly recycled. The COD content of the reverse osmosis concentrated solution is 630mg/L, and the reverse osmosis concentrated solution and the inorganic membrane filtered clear solution can be mixed and then enter a catalytic oxidation tower again for treatment.
Example 3
The emulsified liquid wastewater (COD 300g/L, chromaticity 700, salt content 0.4% and oil content 4800 mg/L) is first filtered by an inorganic ceramic membrane filter, the pore diameter of the ceramic membrane is 50nm, and oil-water separation is carried out under the operating pressure of 0.3MPa to obtain inorganic membrane concentrated solution and clear solution. The oil content of the inorganic membrane concentrate is 70g/L, and the inorganic membrane concentrate is directly burnt; clear liquid (COD 35000mg/L, chromaticity 680, salt content 0.4%, oil content 200 mg/L) is heated by a heat exchanger and a heat transfer oil heat exchanger in sequence to reach 245 ℃, and is continuously introduced into a catalytic reaction tower, and the CuSO is filled into the catalytic reaction tower according to 300 g/ton of wastewater to be treated 4 The ionic catalyst is continuously introduced into the system with pure oxygen (the introduced amount is 3m 3 And/h), the residence time of the wastewater in the catalytic oxidation tower is 1h, and the catalytic oxidation reaction is carried out at 245 ℃ and 5.0 MPa. The effluent (COD content is 280mg/L, conductivity is 7000 mu s/cm, chromaticity is 30) of the catalytic reaction tower is subjected to heat exchange with clear liquid to be fed into the catalytic reaction tower in a heat exchanger, then the clear liquid is fed into a cooler for further cooling to 30-40 ℃, the cooled clear liquid is fed into an activated carbon tank, and is pumped into an ultrafiltration membrane device (the ultrafiltration membrane is a hollow fiber ultrafiltration membrane, average pore diameter is 100nm and membrane surface flow rate is 5.5 m/s) for ultrafiltration after being adsorbed by the activated carbon, the filtration temperature of the ultrafiltration membrane is controlled to be 30-40 ℃, transmembrane pressure difference is 0.1MPa, ultrafiltration concentrate is returned to the catalytic reaction tower, and the ultrafiltration concentrate is mixed with the obtained clear liquid for oxidation treatment again; filtering the effluent of the ultrafiltration membrane in a reverse osmosis membrane device (the reverse osmosis membrane is made of cellulose acetate), and controlling the filtrationThe filtering temperature is 30-40 ℃, and the transmembrane pressure difference is 1.5MPa; after the treatment by the double-membrane system, the COD content is reduced from 280mg/L to 2mg/L, the chromaticity is reduced from 30 to 1, the conductivity is reduced from 7000 mu s/cm to 150 mu s/cm, and the effluent can be directly recycled. The COD content of the reverse osmosis concentrated solution is 700mg/L, and the reverse osmosis concentrated solution and the inorganic membrane filtered clear solution can be mixed and then enter the catalytic oxidation tower again for treatment.
Claims (8)
1. The method for treating the emulsion wastewater is characterized by comprising the following steps of:
(1) Carrying out oil-water separation on the high-concentration emulsion wastewater through inorganic membrane filtration, wherein the aperture of the inorganic membrane is 0.1-1.0 mu m, and the operating pressure of the inorganic membrane filtration is 0.1-0.4 MPa, so as to obtain inorganic membrane concentrated solution and clear solution; the COD of the high-concentration emulsion wastewater is 100000 ～ 400000mg/L, and the oil content is 2000-10000 mg/L;
(2) Introducing the clear liquid into a catalytic oxidation system for catalytic oxidation treatment; the catalytic oxidation treatment is CWAO catalytic wet oxidation treatment: continuously introducing the clear liquid into a catalytic oxidation system for catalytic wet oxidation treatment, wherein the retention time is 1-2 h, and carrying out oxidation reaction under the conditions of the temperature of 200-260 ℃ and the pressure of 5-8 MPa under the action of a catalyst; wherein the catalyst takes one or more of transition metal oxides as active ingredients and Al 2 O 3 The transition metal is selected from Cu, fe, ni, co, mn, and the loading of the transition metal oxide is 2-10 wt%; the dosage of the catalyst is 250-350 g/ton of water based on the dosage of the active ingredients; the oxidant is air, oxygen or hydrogen peroxide, and the dosage of the air or the oxygen is 2-3.5 m based on the oxygen 3 /h；
(3) The effluent after the catalytic oxidation treatment in the step (2) is adsorbed by active carbon and then enters an ultrafiltration membrane device for ultrafiltration treatment, so as to obtain ultrafiltration concentrate and ultrafiltration membrane effluent;
(4) Returning the ultrafiltration concentrated solution to a catalytic oxidation system, mixing the ultrafiltration concentrated solution with the clear solution obtained in the step (1), and carrying out oxidation treatment again; the effluent of the ultrafiltration membrane enters a reverse osmosis membrane device for reverse osmosis treatment to obtain reverse osmosis concentrated solution and permeate, and the reverse osmosis concentrated solution returns to a catalytic oxidation system for oxidation treatment; the permeate reaches the standard of reuse water and is directly reused.
2. The method for treating wastewater from emulsion as claimed in claim 1, wherein in step (1), the inorganic film is a ceramic film, a metal film or a silicon carbide film.
3. The method for treating emulsion wastewater according to claim 1, wherein in the step (2), clear liquid obtained by filtering with an inorganic membrane is filtered by a cartridge filter, is sequentially heated to 200-260 ℃ by a heat exchanger and a heat transfer oil heat exchanger, and then enters a catalytic oxidation system for catalytic oxidation treatment.
4. The method for treating wastewater of emulsion as claimed in claim 3, wherein the catalyst is used in an amount of 300 g/ton of water based on the amount of the active ingredient; the air or oxygen is used in an amount of 3m based on oxygen 3 /h。
5. The method for treating emulsion wastewater according to claim 1, wherein in the step (3), the effluent treated by the catalytic oxidation in the step (2) firstly enters a heat exchanger to exchange heat with clear liquid to be subjected to the catalytic oxidation, then enters a cooler to be further cooled to 20-40 ℃, and enters an ultrafiltration membrane device to carry out ultrafiltration treatment after being adsorbed by active carbon;
the operation temperature of the ultrafiltration membrane device is controlled to be 20-40 ℃; the filtration pressure of the ultrafiltration membrane device is controlled to be 0.05-0.2 MPa; the membrane surface flow rate of the wastewater is between 0.5 and 10 m/s.
6. The method for treating emulsion wastewater according to claim 1, wherein in the step (3), the ultrafiltration membrane device adopts an ultrafiltration membrane made of polysulfone, polyvinyl chloride, polypropylene, polyacrylonitrile or polyvinylidene fluoride; the average pore diameter of the ultrafiltration membrane is 5-100 nm or the membrane with the molecular weight cut-off of 1000-200000 Da.
7. The method for treating wastewater in emulsion according to claim 1, wherein in the step (4), the reverse osmosis membrane of the reverse osmosis membrane device is made of cellulose acetate, polysulfone, polyethersulfone or polyvinyl alcohol.
8. The method for treating wastewater of emulsion as claimed in claim 1, wherein the reverse osmosis device is operated at a pressure of 0.5 to 3.0MPa and at a temperature of 20 to 40 ℃.
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