CN103159299A - Porous titanium film photoelectrically-catalytic waste water reaction device - Google Patents
Porous titanium film photoelectrically-catalytic waste water reaction device Download PDFInfo
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- CN103159299A CN103159299A CN2013100912629A CN201310091262A CN103159299A CN 103159299 A CN103159299 A CN 103159299A CN 2013100912629 A CN2013100912629 A CN 2013100912629A CN 201310091262 A CN201310091262 A CN 201310091262A CN 103159299 A CN103159299 A CN 103159299A
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- 239000010936 titanium Substances 0.000 title claims abstract description 56
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 54
- 239000002351 wastewater Substances 0.000 title claims description 13
- 238000006243 chemical reaction Methods 0.000 title claims description 11
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 5
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 claims 4
- 229910052755 nonmetal Inorganic materials 0.000 claims 2
- 239000004065 semiconductor Substances 0.000 claims 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims 1
- 239000003054 catalyst Substances 0.000 claims 1
- 238000005229 chemical vapour deposition Methods 0.000 claims 1
- 238000005374 membrane filtration Methods 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 229910000510 noble metal Inorganic materials 0.000 claims 1
- 238000007747 plating Methods 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 14
- 238000005530 etching Methods 0.000 abstract description 9
- 238000003618 dip coating Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000010815 organic waste Substances 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 11
- 239000012528 membrane Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000000593 degrading effect Effects 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000003115 supporting electrolyte Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- -1 Methylene Chemical group 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Abstract
The invention provides a method for preparing electrodes from titanium film tubes, which comprises the following steps: etching a porous titanium film used as a substrate to ensure that the surface is coarser; then performing dip coating in different solutions, drying, and sintering to obtain electrodes having different properties; and finally preparing an electrochemical waste water treatment device and a photoelectrochemical waste water treatment device. According to the invention, the process is simple, convenient to operate and easy to realize large-scale production; and the prepared titanium film electrodes are stable in properties, and substances on the surfaces are less prone to fall. Thus, the invention has favorable application prospects in the photoelectrical organic waste water treatment aspect.
Description
Technical field
The present invention uses the porous titanium film pipe of different pore size, first pass through surface etch, then use thermal decomposition method different electrode activity oxide compound of load on porous titanium film pipe, obtain the porous titanium film pipe electrode of different performance, use at last sol-gel method or PECVD method at outside surface load one deck TiO of titanium film pipe electrode
2, sintering makes TiO
2Layer is better with the bonding force of titanium film pipe electrode.
Background technology
Metallic membrane is high due to its physical strength, membrane flux is high, heat-conductive characteristic good, easily is sealed to member, and stable chemical nature has obtained application in a lot of low pressure filter plants.Electrochemical oxidation process, only needs to add add on a small quantity or not chemical reagent as reactant with electronics, just can move at normal temperatures and pressures, and energy utilization efficiency is high, is a kind of cleaning, safety, sewage water treatment method effectively.Titanium film has multi-pore channel, and large specific surface area will have the metal oxide supported electrode of making of electro catalytic activity on the porous titanium film, can reduce equipment volume, conserve space.Simultaneously making outside surface load one deck TiO of POROUS TITANIUM membrane electrode
2, due to TiO
2Have photocatalysis, can decompose the pollutents such as greasy dirt that are deposited on the porous Surface of Titanium Film, reduce the obstruction of porous titanium film, increase work-ing life, reduce the filter operation cost.
Summary of the invention
The object of the present invention is to provide that a kind of technique is simple, easy to operate, the porous titanium film pipe wastewater treatment equipment of stable performance.The present invention realizes by following technological method: will repeatedly be immersed in the sol-gel solution of active substance through the porous titanium film pipe of oxalic acid etching processing, repeatedly lift and the heating for multiple times oxygenolysis, the activating oxide coating that has the electrocatalysis function at porous titanium film surface deposition one deck then can be used the PECVD method or brush TiO
2The methods such as sol-gel are at outside surface load one deck TiO of porous titanium film pipe
2, the porous titanium film pipe electrode that obtains at last having the photoelectrocatalysis function.
For achieving the above object, the present invention adopts following technical scheme, and POROUS TITANIUM membrane electrode reaction unit comprises:
1. water circulating pump that flow is controlled;
2. an end is with the stainless steel tube of hemispherical head, and the other end is with flange or lower end sealing and with the transparent glass tube of water-in, negative electrode titanium silk;
3. catch basin is one;
4. regulated power supply.
Concrete steps are as follows:
(1) etching processing of metal titanium membrane pipe: metal porous titanium film pipe is removed surface and oil contaminant with liquid detergent, ethanol, deionized water supersound washing respectively, then be that the oxalic acid of 5～20wt% is at 40～150 ℃ of lower constant temperature etching 60～180min with concentration, rinse dry for standby well with deionized water;
(2) dipping lifts: at first preparation contain Sn, Sb and Ce sol-gel solution (its mol ratio is 100: X: Y) or preparation contain the sol-gel solution of Sn, Ru, Sb (its mol ratio be 100: X: Y), then the porous titanium film pipe of etching processing being crossed is immersed in 5min in solution, dry in IR bake after slowly lifting out, repeat 3 times, then in retort furnace at 350～500 ℃ of lower sintering.Then flood again lift, oven dry, sintering, repeated several times obtains electrode at last.After last dipping lifted, dries, the POROUS TITANIUM membrane electrode is 500 ℃ of lower sintering 120min in retort furnace;
(3) load TiO on the POROUS TITANIUM membrane electrode
2(can be divided into 3 kinds of methods):
PECVD method: with tetra isopropyl titanate TIPT (Ti[OCH (CH
3)
2]
4) as depositing Ti O
2The starting materials of layer, O
2As carrier gas and reaction gas, TiO
2The film sample preparation is carried out in the PECVD reactor, at porous titanium film tube outer surface depositing Ti O
2Layer, after deposition process finishes, 500 ℃ of sintering 60min in retort furnace;
Brush sol-gel method: adopting tetrabutyl titanate (or titanium isopropylate, or titanium tetrachloride) etc. be the titanium source, and use ethanol (or Virahol, or propyl carbinol) etc. is solvent, adds appropriate HNO
3Make the colloidal sol of homogeneous transparent, then with brush, sol-gel is brushed porous titanium film pipe electrode outside surface, brush one deck, oven dry once, in this way after triplicate, 500 ℃ of sintering 30min in retort furnace, brushing again, oven dry several times, 500 ℃ of sintering 60min in retort furnace for the last time.
Description of drawings
Fig. 1 is the porous titanium film pipe reactor schematic diagram of making:
(1) waste water import; (2) wastewater outlet after electrolysis; (3) anode connection; (4) flange seal; (5) cathode connection; (6) POROUS TITANIUM of carrying active oxide compound is not; (7) with the stainless steel cathode of end socket
Fig. 2 is the electrochemical degradation waste water reaction device schematic diagram of making:
(1) tank; (2) water circulating pump; (3) reactor; (4) regulated power supply
Fig. 3 is the photoelectric catalysis degrading waste water reaction device schematic diagram of making:
(1) tank; (2) regulated power supply; (3) water circulating pump; (4) spinner-type flowmeter; (5) photoelectricity titanium film pipe reactor
Fig. 4 (a) and accompanying drawing 4 (b) are the degradation curves of the methylene blue of the tropeolin-D of POROUS TITANIUM membrane electrochemical degraded 10ppm of embodiment 1 preparation and 10ppm.
Fig. 5 (a) and accompanying drawing 5 (b) are the degradation curves of the methylene blue of the tropeolin-D of porous titanium film photoelectric catalysis degrading 10ppm of embodiment 2 preparation and 10ppm.
Embodiment
The present invention will be further described below by embodiment, and its purpose only is better to understand content of the present invention, but protection scope of the present invention is not limited by the cases cited.
(1) be 30mm with external diameter, thickness is 2.5mm, and length is 125～450mm, the aperture be the porous titanium film pipe of 5～100 μ m at the oxalic acid of 10wt% at 100 ℃ of lower etching 120min, clean in deionized water for ultrasonic after taking out, dries in IR bake, standby;
(2) use dip-coating method and coating thermal decomposition method to prepare tin antimony coat electrode.Take propyl carbinol as solvent, preparation Sn: Sb: Ce=100: the electrode coating solution A of 10: 3 (mol ratio).To be immersed in 3～4min in solution A through the porous titanium film pipe of etching processing, and slowly lift out, dry in IR bake, repeat 3 times.Porous titanium film pipe after then drying is for the first time at N
2The lower 350 ℃ of sintering 60min of atmosphere.Then flood after taking-up and lift, every repetition 3 times, 350 ℃ of sintering 60min in retort furnace, dipping lifts 12～18 times altogether, for the last time at 500 ℃ of lower sintering 120min;
(1) be 30mm with external diameter, thickness is 2.5mm, and length is 125～450mm, the aperture be the porous titanium film pipe of 5～100 μ m at the oxalic acid of 10wt% at 100 ℃ of lower etching 120min, clean in deionized water for ultrasonic after taking out, dries in IR bake, standby;
(2) use dip-coating method and coating thermal decomposition method to prepare tin antimony coat electrode.Take propyl carbinol as solvent, preparation Ru: Sn=6: the electrode coating solution A of 5 (mol ratios).To be immersed in 3～4min in solution A through the porous titanium film pipe of etching processing, and slowly lift out, dry in IR bake, repeat 3 times.Porous titanium film pipe after then drying is for the first time at N
2The lower 350 ℃ of sintering 60min of atmosphere.Then flood after taking-up and lift, every repetition 3 times, 350 ℃ of sintering 60min in retort furnace, dipping lifts 10～12 times altogether, for the last time at 500 ℃ of lower sintering 120min;
(3) volatile pulverous tetra isopropyl metatitanic acid fat TIPT (Ti[OCH (CH is adopted in research
3)
2]
4) as depositing Ti O
2Layer original material, purity are 97%, and boiling point is 232 ℃.Due to the volatile characteristic of TIPT, TIPT must first preheat before entering reaction chamber, and must adopt other gas to carry out the conveying of TIPT.When TIPT is heated to about 55 ℃, as the O of transportation gas
2Just be filled in the heating container of TIPT, TIPT, is reacted in reaction chamber by oxygen delivery, last outside deposition one deck TiO at porous titanium film pipe
2, the flow of gas can pass through the flowmeter survey gained.With load TiO
2Electrode burn 60min under 500 ℃.
Can find out from Fig. 4 (a) and Fig. 4 (b), when supporting electrolyte concentration was identical, 5min was many, and mass concentration is respectively the colourity decreasing ratio of the tropeolin-D of 10ppm and methylene blue all near 100%.Therefore can find out that electrode pair tropeolin-D and the methylene blue prepared have good degradation effect.
Can find out from Fig. 5 (a) and Fig. 5 (b), when supporting electrolyte concentration was identical, 4min was many, and mass concentration is respectively the colourity decreasing ratio of the tropeolin-D of 10ppm and methylene blue all near 100%.
Compare with Fig. 5 (a) with Fig. 4 (a) simultaneously, can find out from Fig. 4 (b) and Fig. 5 (b): under the same conditions, load has TiO
2Methylene blue and the tropeolin-D ratio of electrode degrading equal in quality concentration there is no TiO
2The electrode required time short, current consumption is little when the methylene blue of processing same concentrations and tropeolin-D.When therefore carrying out extensive degrading waste water, photoelectrochemical degradation waste water has advantage more than independent electric degrading waste water.
Claims (7)
1. porous titanium film photoelectrocatalysis waste water reaction device, it comprises (1) tank, (2) water circulating pump, (3) under meter, (4) porous titanium film pipe reactor, (5) reactor adjustable DC power supply, (6) constant flow pump regulated power supply.
2. electrocatalysis waste water reaction device according to claim 1, is characterized in that, described anode tube can be the porous titanium film pipe of pore diameter range at 4～10 μ m, and wall thickness is 2.5～5mm.
3. the activating oxide of porous titanium film tube anode load is PbO according to claim 1
2, SnO
2, RuO
2, IrO
2, Sb
2O
5, TiO
2, Cr
2O
3Or be the combined electrode of metal oxide.
4. photoelectrocatalysis wastewater treatment porous titanium film tube reaction device according to claim 1, it is characterized in that, the photocatalyst material of described photo cathode load is to UV-light (UV) or to visible light-responded photocatalyst, and photocatalyst material can be coml TiO
2(P25), the TiO of self-control, doping vario-property
2(metal ion mixing, surperficial noble metal loading, semi-conductor are compound, nonmetal doping, metal-nonmetal codoped and TiO
2Photochemical catalysis) or other semiconductor light-catalyst, its pattern can be powdery, and is bar-shaped, tubulose, any one or a few in spherical.
According to claim 3 with the described photoelectrocatalysis wastewater treatment of claim 4 porous titanium film tube reaction device, it is characterized in that, the method of the activating oxide of described porous titanium film tube anode load is sol-gel thermal decomposition method, electrochemical plating, CVD method, and the carrying method of described photocatalyst is TiO
2Sol-gel thermal decomposition method or PECVD method.
6. electrochemical treatment waste water porous titanium film pipe reactor according to claim 1, it is characterized in that, the porous titanium film pipe for preparing is fixed on the blind flange that the materials such as nonconducting tetrafluoroethylene or resin make, on the water outlet of titanium film pipe with anode connection, flange and an end are connected (seal head is with water-in) with the stainless steel tube of seal head, with cathode connection, seal with the O RunddichtringO between blind flange and flange on the stainless steel tube outer wall.
7. photoelectrocatalysis wastewater treatment porous titanium film tube reaction device according to claim 1, it is characterized in that, when device flowed to the waste water of upper end by the lower end when operation, the reactor through serial or parallel connection had carried out POROUS TITANIUM membrane filtration, electrocatalysis and the triple technical finesses of surface light catalysis simultaneously.
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|---|---|---|---|
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|---|---|---|---|
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| CN103159299B CN103159299B (en) | 2015-10-07 |
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Cited By (8)
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| CN103395865A (en) * | 2013-07-30 | 2013-11-20 | 南京理工大学 | Titanium-base tubular ruthenium dioxide coating membrane electrode and preparation method thereof |
| CN105217743A (en) * | 2015-10-30 | 2016-01-06 | 南京桐纳新材料科技有限公司 | The method of catalytic oxidation process methyl alcohol and formaldehyde industrial wastewater |
| CN105565442A (en) * | 2014-10-09 | 2016-05-11 | 南京理工大学 | Titanium-based lead dioxide porous tubular membrane electrode and its preparation method and use |
| CN106186205A (en) * | 2016-07-18 | 2016-12-07 | 南京理工大学 | A kind of micropore titanio tubular type multidimensional nano-pore embeds stannum antimony membrane electrode and preparation method thereof |
| CN106861666A (en) * | 2017-02-17 | 2017-06-20 | 深圳大学 | A kind of electro-catalysis membrane and preparation method thereof, wastewater treatment equipment |
| CN108147599A (en) * | 2018-02-28 | 2018-06-12 | 中国人民解放军陆军军医大学 | Water purification film |
| CN109650494A (en) * | 2019-01-24 | 2019-04-19 | 华禹环保(南京)有限公司 | A kind of negative pressure electro-flotation sewage treatment device and technique |
| CN115594259A (en) * | 2022-10-08 | 2023-01-13 | 青岛理工大学（Cn） | Multipurpose electrochemical device for water treatment and application |
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Cited By (9)
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| CN103395865A (en) * | 2013-07-30 | 2013-11-20 | 南京理工大学 | Titanium-base tubular ruthenium dioxide coating membrane electrode and preparation method thereof |
| CN105565442A (en) * | 2014-10-09 | 2016-05-11 | 南京理工大学 | Titanium-based lead dioxide porous tubular membrane electrode and its preparation method and use |
| CN105217743A (en) * | 2015-10-30 | 2016-01-06 | 南京桐纳新材料科技有限公司 | The method of catalytic oxidation process methyl alcohol and formaldehyde industrial wastewater |
| CN105217743B (en) * | 2015-10-30 | 2018-03-30 | 南京桐纳新材料科技有限公司 | The method that electrocatalytic oxidation handles methanol and formaldehyde industrial wastewater |
| CN106186205A (en) * | 2016-07-18 | 2016-12-07 | 南京理工大学 | A kind of micropore titanio tubular type multidimensional nano-pore embeds stannum antimony membrane electrode and preparation method thereof |
| CN106861666A (en) * | 2017-02-17 | 2017-06-20 | 深圳大学 | A kind of electro-catalysis membrane and preparation method thereof, wastewater treatment equipment |
| CN108147599A (en) * | 2018-02-28 | 2018-06-12 | 中国人民解放军陆军军医大学 | Water purification film |
| CN109650494A (en) * | 2019-01-24 | 2019-04-19 | 华禹环保(南京)有限公司 | A kind of negative pressure electro-flotation sewage treatment device and technique |
| CN115594259A (en) * | 2022-10-08 | 2023-01-13 | 青岛理工大学（Cn） | Multipurpose electrochemical device for water treatment and application |
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