CN103539227B - Preparation process of Ag-supported and MnO2-CeO2 doped activated alumina particle electrode containing CuO interlayer - Google Patents
Preparation process of Ag-supported and MnO2-CeO2 doped activated alumina particle electrode containing CuO interlayer Download PDFInfo
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Abstract
The invention discloses a preparation process of an Ag-supported and MnO2-CeO2 doped activated alumina particle electrode containing a CuO interlayer. The preparation process comprises the following steps of adding AgNO3 to isopropanol to obtain a solution A, adding treated Al2O3 to the solution A, filtering the solution to obtain a particle B and micro-emulsion X, and washing the particle B with ethanol, thus obtaining a particle D; adding the particle D to X to obtain a particle F after filtration; utilizing Ce(NO3)2, CuCl2 and MnCl2 to prepare solutions B1, B2, B3, B4, B5, C, D, E and F; treating the particle F with the solutions B1, B2, B3, B4, B5 in sequence, thus obtaining a particle I; adding the particle I to the solution C, filtering the solution, then washing the obtained particle with ethanol, and drying the particle, thus obtaining a particle K; adding the particle K to the solution D, filtering the solution, then washing the obtained particle with ethanol, and drying the particle, thus obtaining a particle M; adding M to the solution E, filtering the solution, then washing the obtained particle with ethanol, and drying the particle, thus obtaining a particle O; adding the particle O to the solution F, filtering the solution, then washing the obtained particle with ethanol, drying the particle, and roasting the obtained particle at 580 DEG C for four hours, thus obtaining the Ag-supported and MnO2-CeO2 doped activated alumina particle electrode containing the CuO interlayer.
Description
Technical field
The invention belongs to the chemically modified electrode technical field of By Electrocatalytic Oxidation process waste water, particularly a kind of loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2the preparation technology of activated alumina granule electrode.
Background technology
Electro-catalytic oxidation technology carrys out the organic pollutant in degrading waste water by the active group producing the strong oxidizing properties such as hydroxyl radical free radical, in process high density, bio-refractory waste water aspect has non-secondary pollution, cost is low, suitability is strong, efficiency high, wherein three-dimensional electro-catalytic oxidation technology, by adding the granule electrode with catalytic activity between the anode and negative electrode of two-dimensional electrode, make the granular electrode surface of filling charged by certain mode, its useful area improving two-dimensional electrode is little, mass transfer effect is poor, the defects such as current efficiency is low, be applicable to the waste water of various concentration, even if the waste water very low to Pollutant levels also has good treatment effect, it is a kind of catalytic oxidation water technology that research is more at present.Based on Three-dimensional Electrode Method is applied to wastewater treatment, and its treatment effect is not only closely related with main electrode performance, and has much relations with the performance of granule electrode, and the catalytic performance therefore how improving granule electrode becomes the focus of Recent study.
Conventional granule electrode material mainly contains metallic conductor, metal oxide, the glass sphere being coated with metal level or baton round, graphite particle, active oxidation aluminum particulate, carbon fibre material and activated carbon granule etc.The resistance of traditional electrode is comparatively large, electric conductivity is low is make it current efficiency is low in the treatment of waste water, stability is inadequate, the life-span is short, electrode material cost is higher, and technology for preparing electrode is complicated, limit the development of granule electrode material, so the research of novel granule electrode material also needs further reinforcement.Adopt dipping-thermal decomposition method to prepare loading type granule electrode to be in recent years subject to increasing scholar and to pay attention to, but also exist and reuse the shortcomings such as weak effect, electrode efficiency are low, also lack the research of granule electrode preparation technology aspect at present.
Summary of the invention
The object of this invention is to provide a kind of loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2the preparation technology of activated alumina granule electrode.Its concrete steps are as follows:
(1) by 300g particle diameter be the γ-Al of 3-5mm
2o
3ball 500ml deionized water wash, repeated washing 3 times, then puts into 200ml dehydrated alcohol and soaks 10h, and after 500ml washed with de-ionized water 1 time, dry 10h under 80 DEG C of conditions, obtains particulate matter A;
(2) be the AgNO of 0.5mol/L by 50ml concentration
3add in 150ml Virahol, obtain solution A;
(3) the particulate matter A that step (1) obtains is added in the solution A that step (2) obtains, and 3h is shaken in shaking table, filtration obtains particulate matter B and microemulsion X, with the washing with alcohol particulate matter B that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter C;
(4) the particulate matter C that step (3) obtains is placed in retort furnace roasting 4h under 500 DEG C of conditions, obtains particulate matter D;
(5) the particulate matter D that step (4) obtains is added in the microemulsion X that step (3) obtains, and 3h is shaken in shaking table, cross and filter liquid and obtain particulate matter E, with the washing with alcohol particulate matter E that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, is then placed in retort furnace roasting 4h under 500 DEG C of conditions, obtains particulate matter F;
(6) by 10ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 100ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 10ml concentration is 0.5mol/L
2solution, is divided into equivalent 5 parts, obtains solution B after shaking up
1, solution B
2, solution B
3, solution B
4, solution B
5;
(7) the particulate matter F that step (5) obtains is added the solution B that step (6) obtains
1in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G1 excessively, and be the washing with alcohol particulate matter G1 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
1;
(8) by particulate matter H that step (7) obtains
1add the solution B that step (6) obtains
2in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G2 excessively, and be the washing with alcohol particulate matter G2 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
2;
(9) by particulate matter H that step (8) obtains
2add the solution B that step (6) obtains
3in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G3 excessively, and be the washing with alcohol particulate matter G3 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
3;
(10) by particulate matter H that step (9) obtains
3add the solution B that step (6) obtains
4in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G4 excessively, and be the washing with alcohol particulate matter G4 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
4;
(11) by particulate matter H that step (10) obtains
4add the solution B that step (6) obtains
5in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G5 excessively, and be the washing with alcohol particulate matter G5 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
5; By H
5be placed in retort furnace roasting 4h under 580 DEG C of conditions, obtain particulate matter I;
(12) by 20ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 80ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 20ml concentration is 0.5mol/L
2solution, obtains solution C;
(13) the particulate matter I that step (11) obtains is added in the solution C that step (12) obtains, and shake 3h in shaking table; Crossing and filter liquid and obtain particulate matter J, is the washing with alcohol particulate matter J of 95% by 100mL mass concentration, repeated washing 2 times, and then dry 10h under 80 DEG C of conditions, obtains particulate matter K;
(14) by 40ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 40ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 40ml concentration is 0.5mol/L
2solution, obtains solution D;
(15) the particulate matter K that step (13) obtains is added in the solution D that step (14) obtains, and shake 3h in shaking table; Crossing and filter liquid and obtain particulate matter L, is the washing with alcohol particulate matter L of 95% by 100mL mass concentration, repeated washing 2 times, and then dry 10h under 80 DEG C of conditions, obtains particulate matter M;
(16) by 45ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and l5ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 60ml concentration is 0.5mol/L
2solution, obtains solution E;
(17) the particulate matter M that step (15) obtains is added in the solution E that step (16) obtains, and shake 3h in shaking table; Crossing and filter liquid and obtain particulate matter N, is the washing with alcohol particulate matter N of 95% by 100mL mass concentration, repeated washing 2 times, and then dry 10h under 80 DEG C of conditions, obtains particulate matter O;
(18) by 15ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 5ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 100ml concentration is 0.5mol/L
2solution, obtains solution F;
(19) the particulate matter O that step (17) obtains is added in the solution F that step (18) obtains, and shake 3h in shaking table; Cross and filter liquid and obtain particulate matter P, with the washing with alcohol particulate matter P that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtain particulate matter Q, Q is placed in retort furnace roasting 4h under 580 DEG C of conditions, the particulate matter obtained is the loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2activated alumina granule electrode.
The invention has the beneficial effects as follows, the obtained loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2activated alumina granule electrode has the features such as current efficiency is high, stability is strong, electrode life is long.
Embodiment
The invention provides a kind of loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2the preparation technology of activated alumina granule electrode, illustrates below by an example and in fact executes process.
Embodiment 1.
Be the γ-Al of 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 after 500ml washed with de-ionized water 1 time, dry 10h under 80 DEG C of conditions, obtains particulate matter A.
Be the AgNO of 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, with the washing with alcohol particulate matter B that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter C; Particulate matter C is placed in retort furnace roasting 4h under 500 DEG C of conditions, obtains particulate matter D; Particulate matter D is joined in microemulsion X, and 3h is shaken in shaking table, cross and filter liquid and obtain particulate matter E, be the washing with alcohol E of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, is then placed in retort furnace roasting 4h under 500 DEG C of conditions, obtains particulate matter F.
Be the Ce (NO of 0.5mol/L by 10ml concentration
3)
2solution and 100ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 10ml concentration is 0.5mol/L
2solution, is divided into equivalent 5 parts, obtains solution B after shaking up
1, solution B
2, solution B
3, solution B
4, solution B
5;
Joined in solution B 1 by particulate matter F, and shake 3h in shaking table, filtering liquid obtains particulate matter G1 excessively, with the washing with alcohol particulate matter G1 that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
1; By particulate matter H
1join solution B
2in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G2 excessively, and be the washing with alcohol particulate matter G2 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
2; By particulate matter H
2join solution B
3in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G3 excessively, and be the washing with alcohol particulate matter G3 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
3; By particulate matter H
3join solution B
4in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G4 excessively, and be the washing with alcohol particulate matter G4 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
4; By particulate matter H
4join solution B
5in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G5 excessively, and be the washing with alcohol particulate matter G5 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
5; By H
5be placed in retort furnace roasting 4h under 580 DEG C of conditions, obtain particulate matter I.
Be the Ce (NO of 0.5mol/L by 20ml concentration
3)
2solution and 80ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 20ml concentration is 0.5mol/L
2solution, obtains solution C.
Particulate matter I is joined in solution C, and shake 3h in shaking table; Cross and filter liquid and obtain particulate matter J, be the washing with alcohol particulate matter J of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter K.
Be the Ce (NO of 0.5mol/L by 40ml concentration
3)
2solution and 40ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 40ml concentration is 0.5mol/L
2solution, obtains solution D.
Particulate matter K is joined in solution D, and shake 3h in shaking table; Cross and filter liquid and obtain particulate matter L, be the washing with alcohol particulate matter L of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter M.
Be the Ce (NO of 0.5mol/L by 45ml concentration
3)
2solution and 15ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 60ml concentration is 0.5mol/L
2solution, obtains solution E.
Particulate matter M is joined in solution E, and shake 3h in shaking table; Cross and filter liquid and obtain particulate matter N, be the washing with alcohol particulate matter N of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter O.
Be the Ce (NO of 0.5mol/L by 15ml concentration
3)
2solution and 5ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 100ml concentration is 0.5mol/L
2solution, obtains solution F.
Particulate matter O is joined in solution F, and shake 3h in shaking table; Cross and filter liquid and obtain particulate matter P, with the washing with alcohol particulate matter P that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtain particulate matter Q, Q is placed in retort furnace roasting 4h under 580 DEG C of conditions, the particulate matter obtained is the loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2activated alumina granule electrode.
Here is the loaded Ag doped with Mn O containing CuO middle layer using the inventive method to obtain
2-CeO
2activated alumina granule electrode has carried out Degrading experiment to coal chemical industrial waste water in 3 D electrode reactor, further illustrates the present invention.
The loaded Ag doped with Mn O containing CuO middle layer that the inventive method is obtained
2-CeO
2activated alumina granule electrode is seated in 3 D electrode reactor, has carried out Degrading experiment to coal chemical industrial waste water, and result shows that this electrode can COD efficiently in Treatment of Wastewater in Coking, when influent COD is 512mg/L, with the loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2active oxidation aluminum particulate is the 3rd pole, and pH is 4.5, and voltage is 12V, and the treatment time is 60min, and the COD after process in water outlet is reduced to 44mg/L, and processing efficiency reaches 91.41%.
Claims (1)
1. the loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2the preparation technology of activated alumina granule electrode, is characterized in that, the concrete steps of this technique are as follows:
(1) by 300g particle diameter be the γ-Al of 3-5mm
2o
3ball 500ml deionized water wash, repeated washing 3 times, then puts into 200ml dehydrated alcohol and soaks 10h, and after 500ml washed with de-ionized water 1 time, dry 10h under 80 DEG C of conditions, obtains particulate matter A;
(2) be the AgNO of 0.5mol/L by 50ml concentration
3add in 150ml Virahol, obtain solution A;
(3) the particulate matter A that step (1) obtains is added in the solution A that step (2) obtains, and 3h is shaken in shaking table, filtration obtains particulate matter B and microemulsion X, with the washing with alcohol particulate matter B that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter C;
(4) the particulate matter C that step (3) obtains is placed in retort furnace roasting 4h under 500 DEG C of conditions, obtains particulate matter D;
(5) the particulate matter D that step (4) obtains is added in the microemulsion X that step (3) obtains, and 3h is shaken in shaking table, cross and filter liquid and obtain particulate matter E, with the washing with alcohol particulate matter E that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, is then placed in retort furnace roasting 4h under 500 DEG C of conditions, obtains particulate matter F;
(6) by 10ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 100ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 10ml concentration is 0.5mol/L
2solution, is divided into equivalent 5 parts, obtains solution B after shaking up
1, solution B
2, solution B
3, solution B
4, solution B
5;
(7) the particulate matter F that step (5) obtains is added the solution B that step (6) obtains
1in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G1 excessively, is the washing with alcohol particulate matter G1 of 95% by 100mL mass concentration, repeated washing 2 times, and then dry 10h under 80 DEG C of conditions, obtains particulate matter H1;
(8) by particulate matter H that step (7) obtains
1add the solution B that step (6) obtains
2in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G2 excessively, and be the washing with alcohol particulate matter G2 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
2;
(9) by particulate matter H that step (8) obtains
2add in the solution B 3 that step (6) obtains, and shake 3h in shaking table, cross and filter liquid and obtain particulate matter G3, with the washing with alcohol particulate matter G3 that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
3;
(10) by particulate matter H that step (9) obtains
3add the solution B that step (6) obtains
4in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G4 excessively, and be the washing with alcohol particulate matter G4 of 95% by 100mL mass concentration, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtains particulate matter H
4;
(11) by particulate matter H that step (10) obtains
4add the solution B that step (6) obtains
5in, and 3h is shaken in shaking table, filtering liquid obtains particulate matter G5 excessively, is the washing with alcohol particulate matter G5 of 95% by 100mL mass concentration, repeated washing 2 times, and then dry 10h under 80 DEG C of conditions, obtains particulate matter H5; H5 is placed in retort furnace roasting 4h under 580 DEG C of conditions, obtains particulate matter I;
(12) by 20ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 80ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 20ml concentration is 0.5mol/L
2solution, obtains solution C;
(13) the particulate matter I that step (11) obtains is added in the solution C that step (12) obtains, and shake 3h in shaking table; Crossing and filter liquid and obtain particulate matter J, is the washing with alcohol particulate matter J of 95% by 100mL mass concentration, repeated washing 2 times, and then dry 10h under 80 DEG C of conditions, obtains particulate matter K;
(14) by 40ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 40ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 40ml concentration is 0.5mol/L
2solution, obtains solution D;
(15) the particulate matter K that step (13) obtains is added in the solution D that step (14) obtains, and shake 3h in shaking table; Crossing and filter liquid and obtain particulate matter L, is the washing with alcohol particulate matter L of 95% by 100mL mass concentration, repeated washing 2 times, and then dry 10h under 80 DEG C of conditions, obtains particulate matter M;
(16) by 45ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 15ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 60ml concentration is 0.5mol/L
2solution, obtains solution E;
(17) the particulate matter M that step (15) obtains is added in the solution E that step (16) obtains, and shake 3h in shaking table; Crossing and filter liquid and obtain particulate matter N, is the washing with alcohol particulate matter N of 95% by 100mL mass concentration, repeated washing 2 times, and then dry 10h under 80 DEG C of conditions, obtains particulate matter O;
(18) by 15ml concentration be the Ce (NO of 0.5mol/L
3)
2solution and 5ml concentration are the CuCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the MnCl that 100ml concentration is 0.5mol/L
2solution, obtains solution F;
(19) the particulate matter O that step (17) obtains is added in the solution F that step (18) obtains, and shake 3h in shaking table; Cross and filter liquid and obtain particulate matter P, with the washing with alcohol particulate matter P that 100mL mass concentration is 95%, repeated washing 2 times, then dry 10h under 80 DEG C of conditions, obtain particulate matter Q, Q is placed in retort furnace roasting 4h under 580 DEG C of conditions, the particulate matter obtained is the loaded Ag doped with Mn O containing CuO middle layer
2-CeO
2activated alumina granule electrode.
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CN108178247A (en) * | 2017-12-28 | 2018-06-19 | 光合强化(北京)生物科技有限公司 | The graphite electrode modified based on CrO-FeO-PbO and quinoline |
CN108163931A (en) * | 2017-12-28 | 2018-06-15 | 光合强化(北京)生物科技有限公司 | The graphite electrode modified based on CeO-ZrO-NiO and pyrazine |
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