CN103539232B - Fluidized bed type three-phase electrode reactor and method for treating high-concentration organic wastewater by using reactor - Google Patents
Fluidized bed type three-phase electrode reactor and method for treating high-concentration organic wastewater by using reactor Download PDFInfo
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- CN103539232B CN103539232B CN201310525852.8A CN201310525852A CN103539232B CN 103539232 B CN103539232 B CN 103539232B CN 201310525852 A CN201310525852 A CN 201310525852A CN 103539232 B CN103539232 B CN 103539232B
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Abstract
The invention discloses a fluidized bed type three-phase electrode reactor, belonging to the technical field of electrochemical treatment on high-concentration organic wastewater. The reactor consists of an electrolytic tank, electrode slots, a supporting Pt-doped SrO-PbO MgO film-plated titanium-based anode plate, a stainless steel cathode plate, supporting Ag-doped SnO2-CeO2 active alumina particle electrodes containing a MnO2 middle layer, a baffle, a gas distribution plate, a gas inlet pipe, an electric wire and a voltage-stabilizing and current-stabilizing power supply. An insertion hole of the gas inlet pipe is formed in the middle-lower middle part of the side wall of the electrolytic tank; the gas distribution plate is mounted at the bottom of the electrolytic tank, and the baffle is mounted above the gas distribution plate; four electrode slots are formed in the electrolytic tank in total, the stainless steel cathode plate and the supporting Pt-doped SrO-PbO MgO film-plated titanium-based anode plate are inserted into the four electrode slots, and the supporting Ag-doped SnO2-CeO2 active alumina particle electrodes containing the MnO2 middle layer are uniformly fed into a gap between the cathode plate and the anode plate. The fluidized bed type three-phase electrode reactor disclosed by the invention has the advantages of high treatment efficiency on high-concentration organic wastewater, low cost and simplicity in operation.
Description
Technical field
The invention belongs to the electrochemical treatment technical field of high concentrated organic wastewater, be specifically related to a kind of method of fluidized bed type three-phase electrode reactor and processing high concentrated organic wastewater thereof.
Background technology
Electro-catalytic oxidation technology carrys out the organic pollutant in degrading waste water by producing the active group of the strong oxidizing properties such as hydroxyl radical free radical, there is non-secondary pollution, cost is low, suitability is strong, efficiency high, has application potential processing aspect high density, bio-refractory waste water.For strengthening the electrocatalysis treatment effect of bio-refractory waste water, improving electrolyzer unit volume effecting reaction area, mass transfer effect and current efficiency is very crucial problem, therefore needs the efficient electric catalysis reactor of development of new.Meanwhile, the exploitation of reactor and the electrode preparation that matches are with it combined and carried out, it is one of emphasis of research at present that the catalytic efficiency of electrode is not fully exerted.Therefore select applicable electrode materials and to its modification, to improve the surface catalysis performance of electrode, just become the new problem of electrochemist's research.Over nearly 30 years, titanium substrate anode plate has developed into the principal mode of metal oxide electrode, modifies at present the metal oxide that titanium electrode uses and mainly contains ruthenium oxide, manganese oxide, plumbous oxide, platinum oxide, iridium oxide, tin-antimony oxide etc.The surface microstructure of electro catalytic electrode and state are the important factors that affects electrocatalysis characteristic, and the preparation method of electrode directly has influence on the surface tissue of electrode, thereby to select suitable electrode preparation method be to improve the vital key link of electrode electro catalytic activity.Also lack at present the research of being prepared by the exploitation of reactor and the electrode that matches with it to the aspect that combines.
Summary of the invention
A kind of method that the object of this invention is to provide fluidized bed type three-phase electrode reactor and processing high concentrated organic wastewater thereof.Particular content of the present invention is as follows:
Fluidized bed type three-phase electrode reactor is plated MgO film titanium substrate anode plate (3), stainless steel cathode plate (4), is contained MnO by electrolyzer (1), electrode slot (2), supporting Pt doping SrO-PbO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode (5), baffle plate (6), air distribution plate (7), inlet pipe (8), electric wire (9), current regulator power supply (10) form.In the sidewall middle and lower part of electrolyzer (1), offer the jack of inlet pipe (8); Air distribution plate (7) is installed in bottom at electrolyzer (1), evenly offers the qi-emitting hole that aperture is lmm on air distribution plate (7), and air distribution plate (7) is positioned at the top of inlet pipe (8); Baffle plate (6) is installed in top at air distribution plate (7), evenly offers the aperture that aperture is 2mm on baffle plate (6); 4 electrode slots (2) are installed altogether on electrolyzer (1), every two slots are a pair of, lay respectively on the front and opposite walls of electrolyzer (1), on slot, be uniformly distributed the screens that width is 2mm, be used for inserting stainless steel cathode plate (4) and supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate (3), the spacing of screens is 10mm; With electric wire (9), stainless steel cathode plate (4) is connected with current regulator power supply (10) with supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate (3); Finally will be containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode (5) evenly drops in the space between stainless steel cathode plate (4) and supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate (3).When using fluidized bed type three-phase electrode reactor for treatment high concentrated organic wastewater, best working conditions is: pH value is 4.5, and voltage is 12V, and the treatment time is 150min.
Wherein, described supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate is prepared by the following method:
(1) with No. 240 aluminum oxide water-proof abrasive papers, titanium plate surface is polished to occurring metalluster, then put it in culture dish, pour 50mL acetone into, in 40kHz ultrasonic washing instrument, with detergent solution, clean oil removing 30min, take out and first with tap water, rinse, use again deionized water rinsing, be then placed on and in 40kHz ultrasonic washing instrument, use washed with de-ionized water 15min;
(2) titanium sheet step (1) being obtained is placed on etching 2h in 10% oxalic acid solution, then take out and first with tap water, rinse, with being placed on after deionized water rinsing in 40kHz ultrasonic instrument, use washed with de-ionized water 15min again, after drying, be kept in dehydrated alcohol standby;
(3) titanium plate surface that utilizes glow discharge to obtain step (2) carries out pre-treatment 10min, then on MS56A type high-vacuum multi-target magnetic control sputtering machine, complete magnetron sputtering platinum plating and obtain substance A, wherein cathode targets is platinized platinum, titanium sheet is as anode substrate, operator scheme is radio-frequency sputtering, and vacuum tightness is 8.0 * 10
-2pa, power is 100W, argon pressure is 1pa;
(4) propyl carbinol, Virahol, isopropylcarbinol, dehydrated alcohol are mixed in equal-volume ratio, obtain solution A; By Sr (NO
3)
2soluble in waterly make the solution that concentration is 0.5mol/L, add 5 nitric acid in case hydrolysis obtains solution B; By Pb (NO
3)
2soluble in waterly make the solution that concentration is 0.5mol/L, add 5 nitric acid in case hydrolysis obtains solution C; By Mg (NO
3)
26H
2o is soluble in water makes the solution that concentration is 0.5mol/L, adds 5 nitric acid in case hydrolysis obtains solution D;
(5) solution B, solution C, solution D 10: 10: 1 are by volume mixed, obtain solution E 1, by solution E 1 with solution A equal-volume than mixing, after shaking up, be divided into 4 parts of equivalent, obtain solution F1-1, solution F1-2, solution F1-3, solution F1-4;
(6) solution B, solution C, solution D 5: 5: 1 are by volume mixed, obtain solution E 2, by solution E 2 with solution A equal-volume than mixing, after shaking up, be divided into 2 parts of equivalent, obtain solution F2-1, solution F2-2;
(7) solution B, solution C, solution D 1: 1: 1 are by volume mixed, obtain solution E 3, by solution E 3 with solution A equal-volume than mixing, after shaking up, be divided into 3 parts of equivalent, obtain solution F3-1, solution F3-2, solution F3-3;
(8) solution B, solution C, solution D 1: 1: 5 are by volume mixed, obtain solution E 4, by solution E 4 with solution A equal-volume than mixing, after shaking up, be divided into 2 parts of equivalent, obtain solution F4-1, solution F4-2;
(9) solution B, solution C, solution D 1: 1: 10 are by volume mixed, obtain solution E 5, by solution E 5 with solution A equal-volume than mixing, after shaking up, be divided into 4 parts of equivalent, obtain solution F5-1, solution F5-2, solution F5-3, solution F5-4;
(10) substance A step (3) being obtained is immersed in solution F1-1, and evenly floods under magnetic stirring apparatus effect, after 3h, takes out and dries, and then dry 10h under 100 ℃ of conditions, obtains substance B 1;
(11) substance B 1 is immersed in solution F1-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance B 2;
(12) substance B 2 is immersed in solution F1-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains substance B 3;
(13) substance B 3 is immersed in solution F1-4, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance B 4;
(14) substance B 4 is immersed in solution F2-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains substance C 1;
(15) substance C 1 is immersed in solution F2-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance C 2;
(16) substance C 2 is immersed in solution F3-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material D1;
(17) material D1 is immersed in solution F3-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material D2;
(18) material D2 is immersed in solution F3-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material D3;
(19) material D3 is immersed in solution F4-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material E1;
(20) material E1 is immersed in solution F4-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material E2;
(21) material E2 is immersed in solution F5-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material F1;
(22) material F1 is immersed in solution F5-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material F2;
(23) material F2 is immersed in solution F5-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material F3;
(24) material F3 is immersed in solution F5-4, and evenly flood under magnetic stirring apparatus effect, after 3h, take out and dry, then under 100 ℃ of conditions, be dried 10h, dried material is placed in to retort furnace roasting 4h under 780 ℃ of conditions, and the material obtaining is supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate.
Described containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode is prepared by the following method:
(1) γ-Al that is 3-5mm by 300g particle diameter
2o
3ball 500ml deionized water wash, repeated washing 3 times, then puts into 200ml dehydrated alcohol and soaks 10h, and with after 500ml washed with de-ionized water 1 time, under 80 ℃ of conditions, dry 10h, obtains particulate matter A;
(2) AgNO that is 0.5mol/L by 50ml concentration
3add in 150ml Virahol, obtain solution A;
(3) particulate matter A step (1) being obtained adds in the solution A that step (2) obtains, and in shaking table, shake 3h, filtration obtains particulate matter B and microemulsion X, the washing with alcohol particulate matter B that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter C;
(4) particulate matter C step (3) being obtained is placed in retort furnace roasting 4h under 500 ℃ of conditions, obtains particulate matter D;
(5) particulate matter D step (4) being obtained adds in the microemulsion X that step (3) obtains, and in shaking table, shake 3h, remove by filter liquid and obtain particulate matter E, the washing with alcohol particulate matter E that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, is then placed in retort furnace roasting 4h under 500 ℃ of conditions, obtains particulate matter F;
(6) Ce (NO that is 0.5mol/L by 10ml concentration
3)
2the MnCl that solution and 200ml concentration are 0.5mol/L
2solution joins in 100ml Virahol and 10ml concentrated hydrochloric acid, and then to add 10ml concentration be the SnCl of 0.5mol/L
4solution, is divided into 5 parts of equivalent after shaking up, obtain solution B
1, solution B
2, solution B
3, solution B
4, solution B
5;
(7) solution B that particulate matter F step (5) being obtained adds step (6) to obtain
1in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G1, the washing with alcohol particulate matter G1 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
1;
(8) particulate matter H step (7) being obtained
1the solution B that adds step (6) to obtain
2in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G2, the washing with alcohol particulate matter G2 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
2;
(9) particulate matter H step (8) being obtained
2the solution B that adds step (6) to obtain
3in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G3, the washing with alcohol particulate matter G3 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
3;
(10) particulate matter H step (9) being obtained
3the solution B that adds step (6) to obtain
4in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G4, the washing with alcohol particulate matter G4 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
4;
(11) particulate matter H step (10) being obtained
4the solution B that adds step (6) to obtain
5in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G5, the washing with alcohol particulate matter G5 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
5; By H
5be placed in retort furnace roasting 4h under 500 ℃ of conditions, obtain particulate matter I;
(12) Ce (NO that is 0.5mol/L by 20ml concentration
3)
2the MnCl that solution and 70ml concentration are 0.5mol/L
2solution joins in 100ml Virahol and 5ml concentrated hydrochloric acid, and then to add 20ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution C;
(13) particulate matter I step (11) being obtained adds in the solution C that step (12) obtains, and in shaking table, shakes 3h; Remove by filter liquid and obtain particulate matter J, the washing with alcohol particulate matter J that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter K;
(14) Ce (NO that is 0.5mol/L by 25ml concentration
3)
2the MnCl that solution and 25ml concentration are 0.5mol/L
2solution joins in 125ml Virahol and 5ml concentrated hydrochloric acid, and then to add 25ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution D;
(15) particulate matter K step (13) being obtained adds in the solution D that step (14) obtains, and in shaking table, shakes 3h; Remove by filter liquid and obtain particulate matter L, the washing with alcohol particulate matter L that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter M;
(16) Ce (NO that is 0.5mol/L by 20ml concentration
3)
2the MnCl that solution and 10ml concentration are 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then to add 50ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution E;
(17) particulate matter M step (15) being obtained adds in the solution E that step (16) obtains, and in shaking table, shakes 3h; Remove by filter liquid and obtain particulate matter N, the washing with alcohol particulate matter N that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter O;
(18) Ce (NO that is 0.5mol/L by 15ml concentration
3)
2the MnCl that solution and 5ml concentration are 0.5mol/L
2solution joins in 100ml Virahol and 5ml concentrated hydrochloric acid, and then to add 80ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution F;
(19) particulate matter O step (17) being obtained adds in the solution F that step (18) obtains, and in shaking table, shakes 3h; Remove by filter liquid and obtain particulate matter P, the washing with alcohol particulate matter P that is 95% by 100mL mass concentration, repeated washing 2 times, then under 80 ℃ of conditions, be dried 10h, obtain particulate matter Q, Q is placed in to retort furnace roasting 4h under 500 ℃ of conditions, the particulate matter obtaining is containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode.
The invention has the beneficial effects as follows, fluidized bed type three-phase electrode reactor is high to high concentrated organic wastewater processing efficiency, cost is low, simple to operate.
Accompanying drawing explanation
Accompanying drawing 1 is the skeleton view of fluidized bed type three-phase electrode reactor.In accompanying drawing 1,1 is electrolyzer, and 2 is electrode slot, and 3 is supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate, and 4 is stainless steel cathode plate, and 5 for containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode, 6 is baffle plate, and 7 is air distribution plate, and 8 is inlet pipe, and 9 is electric wire, 10 is current regulator power supply.
Embodiment
Embodiment
(1) preparation process of fluidized bed type three-phase electrode reactor is as follows:
The length of electrolyzer is 60mm, and wide is 50mm, and height is 120mm.On cell sidewall medullary ray, apart from 10mm place, bottom, offer the inlet pipe jack that aperture is 2mm.Air distribution plate be long for 56mm, wide for 46mm, thick be the thin plate of 3mm, on air distribution plate, evenly offer the qi-emitting hole that aperture is lmm, air distribution plate is 15mm apart from the distance of bottom of electrolytic tank.Baffle plate be long for 56mm, wide for 46mm, thick be the thin plate of 5mm, on baffle plate, evenly offer the aperture that aperture is 2mm, baffle plate is 20mm apart from the distance of bottom of electrolytic tank.Have 4 electrode slots, every two slots are a pair of, lay respectively on the front and opposite walls of electrolyzer, slot is below 35mm apart from the distance of bottom of electrolytic tank, slot is above 85mm apart from the distance of bottom of electrolytic tank, on each slot, be uniformly distributed the screens that width is 2mm, the spacing of screens is 10mm, for intubating length, is that 60mm, width are stainless steel cathode plate and the supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate that 40mm, thickness are 2mm.With electric wire, stainless steel cathode plate is connected with current regulator power supply with supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate.Finally will be containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode evenly drops in the space between stainless steel cathode plate and supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate.
(2) supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate is prepared by following process:
By length, be that 60mm, width are that the titanium sheet that 40mm, thickness are 2mm occurs metalluster with No. 240 aluminum oxide water-proof abrasive paper polishings to surface, then put it in culture dish, pour 50mL acetone into, in 40kHz ultrasonic washing instrument, with detergent solution, clean oil removing 30min, then take out first and rinse with 500mL tap water, use again 100mL deionized water rinsing, then be placed on and in 40kHz ultrasonic washing instrument, use washed with de-ionized water 15min; Then the titanium sheet after cleaning is placed on to l00mL mass concentration and is etching 2h in 10% oxalic acid solution, take out first and rinse with 500mL tap water, use again 100mL deionized water rinsing, be placed on again in 40kHz ultrasonic instrument and use washed with de-ionized water 15min, after drying, be kept in dehydrated alcohol standby;
Taking-up is kept at the titanium sheet in dehydrated alcohol, utilize glow discharge to carry out pre-treatment 10min to its surface, then on MS56A type high-vacuum multi-target magnetic control sputtering machine, complete magnetron sputtering platinum plating and obtain substance A, wherein cathode targets is platinized platinum, titanium sheet is as anode substrate, operator scheme is radio-frequency sputtering, and vacuum tightness is 8.0 * 10
-2pa, power is 100W, argon pressure is 1pa;
150mL propyl carbinol, 150mL Virahol, 150mL isopropylcarbinol and 150mL dehydrated alcohol are mixed, obtain 600mL solution A; By 21.2 grams of Sr (NO
3)
2be dissolved in 200mL water and make the solution that concentration is 0.5mol/L, add 5 nitric acid in case hydrolysis obtains solution B; By 33.1 grams of Pb (NO
3)
2be dissolved in 200mL water and make the solution that concentration is 0.5mol/L, add 5 nitric acid in case hydrolysis obtains solution C; By 25.6 grams of Mg (NO
3)
26H
2o is dissolved in 200mL water and makes the solution that concentration is 0.5mol/L, adds 5 nitric acid in case hydrolysis obtains solution D;
50mL solution B, 50mL solution C, 5mL solution D are mixed, obtain 105mL solution E 1, the broad liquid E1 of 105mL is mixed with 105mL solution A, after shaking up, be divided into 4 parts of equivalent, obtain 52.5mL solution F1-1,52.5mL solution F1-2,52.5mL solution F1-3,52.5mL solution F1-4;
25mL solution B, 25mL solution C, 5mL solution D are mixed, obtain 55mL solution E 2,55mL solution E 2 is mixed with 55mL solution A, after shaking up, be divided into 2 parts of equivalent, obtain 55mL solution F2-1,55mL solution F2-2;
25mL solution B, 25mL solution C, 25mL solution D are mixed, obtain 75mL solution E 3,75mL solution E 3 is mixed with 75mL solution A, after shaking up, be divided into 3 parts of equivalent, obtain 50mL solution F3-1,50mL solution F3-2,50mL solution F3-3;
10mL solution B, 10mL solution C, 50mL solution D are mixed, obtain 70mL solution E 4,70mL solution E 4 is mixed with 70mL solution A, after shaking up, be divided into 2 parts of equivalent, obtain 70mL solution F4-1,70mL solution F4-2;
10mL solution B, 10mL solution C, 100mL solution D are mixed, obtain 120mL solution E 5,120mL solution E 5 is mixed with 120mL solution A, after shaking up, be divided into 4 parts of equivalent, obtain 60mL solution F5-1,60mL solution F5-2,60mL solution F5-3,60mL solution F5-4;
Substance A is immersed in 52.5mL solution F1-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains substance B 1;
Substance B 1 is immersed in 52.5mL solution F1-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance B 2;
Substance B 2 is immersed in 52.5mL solution F1-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains substance B 3;
Substance B 3 is immersed in 52.5mL solution F1-4, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance B 4;
Substance B 4 is immersed in 55mL solution F2-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains substance C 1;
Substance C 1 is immersed in 55mL solution F2-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance C 2;
Substance C 2 is immersed in 50mL solution F3-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material D1;
Material D1 is immersed in 50mL solution F3-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material D2;
Material D2 is immersed in 50mL solution F3-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material D3;
Material D3 is immersed in 70mL solution F4-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material E1;
Material E1 is immersed in 70mL solution F4-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material E2;
Material E2 is immersed in 60mL solution F5-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material F1;
Material F1 is immersed in 60mL solution F5-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material F2;
Material F2 is immersed in 60mL solution F5-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material F3;
Material F3 is immersed in 60mL solution F5-4, and evenly flood under magnetic stirring apparatus effect, after 3h, take out and dry, then under 100 ℃ of conditions, be dried 10h, dried material is placed in to retort furnace roasting 4h under 780 ℃ of conditions, and the material obtaining is supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate.
(3) containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode is prepared by the following method:
γ-the Al that is 3-5mm by 300g particle diameter
2o
3ball 500ml deionized water wash, repeated washing 3 times, then puts into 200ml dehydrated alcohol and soaks 10h, and with after 500ml washed with de-ionized water 1 time, under 80 ℃ of conditions, dry 10h, obtains particulate matter A.
The AgNO that is 0.5mol/L by 50ml concentration
3add in 150ml Virahol, obtain solution A.Particulate matter A is joined in solution A, and shake 3h in shaking table, filter and obtain particulate matter B and microemulsion X, the washing with alcohol particulate matter B that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter C; Particulate matter C is placed in to retort furnace roasting 4h under 500 ℃ of conditions, obtains particulate matter D; Particulate matter D is joined in microemulsion X, and in shaking table, shake 3h, remove by filter liquid and obtain particulate matter E, the washing with alcohol E that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, is then placed in retort furnace roasting 4h under 500 ℃ of conditions, obtains particulate matter F.
Ce (the NO that is 0.5mol/L by 10ml concentration
3)
2the MnCl that solution and 200ml concentration are 0.5mol/L
2solution joins in 100ml Virahol and 10ml concentrated hydrochloric acid, and then to add 10ml concentration be the SnCl of 0.5mol/L
4solution, is divided into 5 parts of equivalent after shaking up, obtain solution B
1, solution B
2, solution B
3, solution B
4, solution B
5.
Particulate matter F is joined to solution B
1in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G1, the washing with alcohol particulate matter G1 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
1; By particulate matter H
1join solution B
2in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G2, the washing with alcohol particulate matter G2 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
2; By particulate matter H
2join solution B
3in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G3, the washing with alcohol particulate matter G3 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
3; By particulate matter H
3join solution B
4in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G4, the washing with alcohol particulate matter G4 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
4; By particulate matter H
4join solution B
5in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G5, the washing with alcohol particulate matter G5 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
5; By H
5be placed in retort furnace roasting 4h under 500 ℃ of conditions, obtain particulate matter I.
Ce (the NO that is 0.5mol/L by 20ml concentration
3)
2the CuCl that solution and 80ml concentration are 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then to add 20ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution C.
Particulate matter I is joined in solution C, and shake 3h in shaking table; Remove by filter liquid and obtain particulate matter J, the washing with alcohol particulate matter J that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter K.
Ce (the NO that is 0.5mol/L by 40ml concentration
3)
2the CuCl that solution and 40ml concentration are 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then to add 40ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution D.
Particulate matter K is joined in solution D, and shake 3h in shaking table; Remove by filter liquid and obtain particulate matter L, the washing with alcohol particulate matter L that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter M.
Ce (the NO that is 0.Smol/L by 45ml concentration
3)
2the CuCl that solution and 15ml concentration are 0.Smol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then to add 60ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution E.
Particulate matter M is joined in solution E, and shake 3h in shaking table; Remove by filter liquid and obtain particulate matter N, the washing with alcohol particulate matter N that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter O.
Ce (the NO that is 0.5mol/L by 15ml concentration
3)
2the CuCl that solution and 5ml concentration are 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then to add 100ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution F.
Particulate matter O is joined in solution F, and in shaking table, shake 3h; Remove by filter liquid and obtain particulate matter P, the washing with alcohol particulate matter P that is 95% by 100mL mass concentration, repeated washing 2 times, then under 80 ℃ of conditions, be dried 10h, obtain particulate matter Q, Q is placed in to retort furnace roasting 4h under 500 ℃ of conditions, the particulate matter obtaining is containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode.
(4) degradation experiment
The fluidized bed type three-phase electrode reactor that uses the present invention to obtain has carried out Degrading experiment to high concentrated organic wastewater, result shows that this reactor can efficiently remove Coal Gas Washing Cycling Water organic compound, when influent COD is 856mg/L, at pH, be 4.5, voltage is 12V, treatment time is under 150min condition, and the COD after processing in water outlet is reduced to 82mg/L, and processing efficiency reaches 90.42%.
Claims (2)
1. a fluidized bed type three-phase electrode reactor, is characterized in that, this fluidized bed type three-phase electrode reactor is plated MgO film titanium substrate anode plate, stainless steel cathode plate, contained MnO by electrolyzer, electrode slot, supporting Pt doping SrO-PbO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode, baffle plate, air distribution plate, inlet pipe, electric wire and current regulator power supply form; In the sidewall middle and lower part of electrolyzer, offer the jack of inlet pipe; Air distribution plate is installed in bottom at electrolyzer, evenly offers the qi-emitting hole that aperture is 1mm on air distribution plate, and baffle plate is installed above air distribution plate, evenly offers the aperture that aperture is 2mm on baffle plate; 4 electrode slots are installed altogether on electrolyzer, for inserting stainless steel cathode plate and supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate; Containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode is evenly distributed in the space between negative plate and positive plate; Wherein, supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate is prepared by the following method:
(1) with No. 240 aluminum oxide water-proof abrasive papers, titanium plate surface is polished to occurring metalluster, then put it in culture dish, pour 50mL acetone into, in 40kHz ultrasonic washing instrument, with detergent solution, clean oil removing 30min, take out and first with tap water, rinse, use again deionized water rinsing, be then placed on and in 40kHz ultrasonic washing instrument, use washed with de-ionized water 15min;
(2) titanium sheet step (1) being obtained is placed on etching 2h in 10% oxalic acid solution, then take out and first with tap water, rinse, with being placed on after deionized water rinsing in 40kHz ultrasonic instrument, use washed with de-ionized water 15min again, after drying, be kept in dehydrated alcohol standby;
(3) titanium plate surface that utilizes glow discharge to obtain step (2) carries out pre-treatment 10min, then on MS56A type high-vacuum multi-target magnetic control sputtering machine, complete magnetron sputtering platinum plating and obtain substance A, wherein cathode targets is platinized platinum, titanium sheet is as anode substrate, operator scheme is radio-frequency sputtering, and vacuum tightness is 8.0 * 10
-2pa, power is 100W, argon pressure is 1pa;
(4) propyl carbinol, Virahol, isopropylcarbinol, dehydrated alcohol are mixed in equal-volume ratio, obtain solution A; By Sr (NO
3)
2soluble in waterly make the solution that concentration is 0.5mol/L, add 5 nitric acid in case hydrolysis obtains solution B; By Pb (NO
3)
2soluble in waterly make the solution that concentration is 0.5mol/L, add 5 nitric acid in case hydrolysis obtains solution C; By Mg (NO
3)
26H
2o is soluble in water makes the solution that concentration is 0.5mol/L, adds 5 nitric acid in case hydrolysis obtains solution D;
(5) solution B, solution C, solution D 10: 10: 1 are by volume mixed, obtain solution E 1, by solution E 1 with solution A equal-volume than mixing, after shaking up, be divided into 4 parts of equivalent, obtain solution F1-1, solution F1-2, solution F1-3, solution F1-4;
(6) solution B, solution C, solution D 5: 5: 1 are by volume mixed, obtain solution E 2, by solution E 2 with solution A equal-volume than mixing, after shaking up, be divided into 2 parts of equivalent, obtain solution F2-1, solution F2-2;
(7) solution B, solution C, solution D 1: 1: 1 are by volume mixed, obtain solution E 3, by solution E 3 with solution A equal-volume than mixing, after shaking up, be divided into 3 parts of equivalent, obtain solution F3-1, solution F3-2, solution F3-3;
(8) solution B, solution C, solution D 1: 1: 5 are by volume mixed, obtain solution E 4, by solution E 4 with solution A equal-volume than mixing, after shaking up, be divided into 2 parts of equivalent, obtain solution F4-1, solution F4-2;
(9) solution B, solution C, solution D 1: 1: 10 are by volume mixed, obtain solution E 5, by solution E 5 with solution A equal-volume than mixing, after shaking up, be divided into 4 parts of equivalent, obtain solution F5-1, solution F5-2, solution F5-3, solution F5-4;
(10) substance A step (3) being obtained is immersed in solution F1-1, and evenly floods under magnetic stirring apparatus effect, after 3h, takes out and dries, and then dry 10h under 100 ℃ of conditions, obtains substance B 1;
(11) substance B 1 is immersed in solution F1-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance B 2;
(12) substance B 2 is immersed in solution F1-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains substance B 3;
(13) substance B 3 is immersed in solution F1-4, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance B 4;
(14) substance B 4 is immersed in solution F2-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains substance C 1;
(15) substance C 1 is immersed in solution F2-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains substance C 2;
(16) substance C 2 is immersed in solution F3-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material D1;
(17) material D1 is immersed in solution F3-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material D2;
(18) material D2 is immersed in solution F3-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material D3;
(19) material D3 is immersed in solution F4-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material E1;
(20) material E1 is immersed in solution F4-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material E2;
(21) material E2 is immersed in solution F5-1, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material F1;
(22) material F1 is immersed in solution F5-2, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, is placed in retort furnace roasting 4h under 780 ℃ of conditions by dried material, obtains material F2;
(23) material F2 is immersed in solution F5-3, and evenly floods under magnetic stirring apparatus effect, after 3h, take out and dry, then dry 10h under 100 ℃ of conditions, obtains material F3;
(24) material F3 is immersed in solution F5-4, and evenly flood under magnetic stirring apparatus effect, after 3h, take out and dry, then under 100 ℃ of conditions, be dried 10h, dried material is placed in to retort furnace roasting 4h under 780 ℃ of conditions, and the material obtaining is supporting Pt doping SrO-PbO plating MgO film titanium substrate anode plate.
2. a kind of fluidized bed type three-phase electrode reactor according to claim 1, is characterized in that, in this fluidized bed type three-phase electrode reactor containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode is prepared by the following method:
(1) γ-Al that is 3-5mm by 300g particle diameter
2o
3ball 500ml deionized water wash, repeated washing 3 times, then puts into 200ml dehydrated alcohol and soaks 10h, and with after 500ml washed with de-ionized water 1 time, under 80 ℃ of conditions, dry 10h, obtains particulate matter A;
(2) AgNO that is 0.5mol/L by 50ml concentration
3add in 150ml Virahol, obtain solution A;
(3) particulate matter A step (1) being obtained adds in the solution A that step (2) obtains, and in shaking table, shake 3h, filtration obtains particulate matter B and microemulsion X, the washing with alcohol particulate matter B that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter C;
(4) particulate matter C step (3) being obtained is placed in retort furnace roasting 4h under 500 ℃ of conditions, obtains particulate matter D;
(5) particulate matter D step (4) being obtained adds in the microemulsion X that step (3) obtains, and in shaking table, shake 3h, remove by filter liquid and obtain particulate matter E, the washing with alcohol particulate matter E that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, is then placed in retort furnace roasting 4h under 500 ℃ of conditions, obtains particulate matter F;
(6) Ce (NO that is 0.5mol/L by 10ml concentration
3)
2the MnCl that solution and 200ml concentration are 0.5mol/L
2solution joins in 100ml Virahol and 10ml concentrated hydrochloric acid, and then to add 10ml concentration be the SnCl of 0.5mol/L
4solution, is divided into 5 parts of equivalent after shaking up, obtain solution B
1, solution B
2, solution B
3, solution B
4, solution B
5;
(7) solution B that particulate matter F step (5) being obtained adds step (6) to obtain
1in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G1, the washing with alcohol particulate matter G1 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
1;
(8) particulate matter H step (7) being obtained
1the solution B that adds step (6) to obtain
2in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G2, the washing with alcohol particulate matter G2 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
2;
(9) particulate matter H step (8) being obtained
2the solution B that adds step (6) to obtain
3in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G3, the washing with alcohol particulate matter G3 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
3;
(10) particulate matter H step (9) being obtained
3the solution B that adds step (6) to obtain
4in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G4, the washing with alcohol particulate matter G4 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
4;
(11) particulate matter H step (10) being obtained
4the solution B that adds step (6) to obtain
5in, and in shaking table, shake 3h, and remove by filter liquid and obtain particulate matter G5, the washing with alcohol particulate matter G5 that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter H
5; By H
5be placed in retort furnace roasting 4h under 500 ℃ of conditions, obtain particulate matter I;
(12) Ce (NO that is 0.5mol/L by 20ml concentration
3)
2the MnCl that solution and 70ml concentration are 0.5mol/L
2solution joins in 100ml Virahol and 5ml concentrated hydrochloric acid, and then to add 20ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution C;
(13) particulate matter I step (11) being obtained adds in the solution C that step (12) obtains, and in shaking table, shakes 3h; Remove by filter liquid and obtain particulate matter J, the washing with alcohol particulate matter J that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter K;
(14) Ce (NO that is 0.5mol/L by 25ml concentration
3)
2the MnCl that solution and 25ml concentration are 0.5mol/L
2solution joins in 125ml Virahol and 5ml concentrated hydrochloric acid, and then to add 25ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution D;
(15) particulate matter K step (13) being obtained adds in the solution D that step (14) obtains, and in shaking table, shakes 3h; Remove by filter liquid and obtain particulate matter L, the washing with alcohol particulate matter L that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter M;
(16) Ce (NO that is 0.5mol/L by 20ml concentration
3)
2the MnCl that solution and 10ml concentration are 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then to add 50ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution E;
(17) particulate matter M step (15) being obtained adds in the solution E that step (16) obtains, and in shaking table, shakes 3h; Remove by filter liquid and obtain particulate matter N, the washing with alcohol particulate matter N that is 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 ℃ of conditions, obtains particulate matter O;
(18) Ce (NO that is 0.5mol/L by 15ml concentration
3)
2the MnCl that solution and 5ml concentration are 0.5mol/L
2solution joins in 100ml Virahol and 5ml concentrated hydrochloric acid, and then to add 80ml concentration be the SnCl of 0.5mol/L
4solution, obtains solution F;
(19) particulate matter O step (17) being obtained adds in the solution F that step (18) obtains, and in shaking table, shakes 3h; Remove by filter liquid and obtain particulate matter P, the washing with alcohol particulate matter P that is 95% by 100mL mass concentration, repeated washing 2 times, then under 80 ℃ of conditions, be dried 10h, obtain particulate matter Q, Q is placed in to retort furnace roasting 4h under 500 ℃ of conditions, the particulate matter obtaining is containing MnO
2the loaded Ag doping SnO in middle layer
2-CeO
2activated alumina granule electrode.
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