CN105481062A - Electro-catalytic particle electrode for efficiently decomposing carbamazepine and preparation method of electro-catalytic particle electrode - Google Patents
Electro-catalytic particle electrode for efficiently decomposing carbamazepine and preparation method of electro-catalytic particle electrode Download PDFInfo
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- CN105481062A CN105481062A CN201610022393.5A CN201610022393A CN105481062A CN 105481062 A CN105481062 A CN 105481062A CN 201610022393 A CN201610022393 A CN 201610022393A CN 105481062 A CN105481062 A CN 105481062A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
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Abstract
The invention discloses an electro-catalytic particle electrode for efficiently decomposing carbamazepine and a preparation method of the electro-catalytic particle electrode and belongs to the technical field of wastewater treatment. Treated coal gangue, clay, a pore forming agent and an activator are taken as raw materials, mixed in a certain weight ratio and uniformly stirred, a mixed raw material is prepared, soaked in loaded reagent sol, dried, cooled to the room temperature and extruded to form raw pellets, the raw pellets are dried, heated, activated and calcined at the certain temperature, taken out after a period of time and cooled to the room temperature, and a finished product is obtained. The prepared electro-catalytic particle electrode for efficiently decomposing carbamazepine is porous, has a large specific surface area, high adsorption performance and excellent electro-catalytic property and can efficiently decompose carbamazepine. According to the electro-catalytic particle electrode for efficiently decomposing carbamazepine and the preparation method of the electro-catalytic particle electrode, solid waste, namely, coal gangue, discharged in the coal mining and coal washing process is sufficiently utilized, waste can be turned into wealth, and the problems about environment pollution, land occupation and the like can be solved.
Description
Technical field
The invention belongs to technical field of waste water processing, particularly a kind of Electrocatalytic particle electrode for the treatment of Carbamzepine in municipal effluent and preparation method thereof.
Background technology
Along with expanding economy, extensively exist from the heavy metal in trade effluent, phenolic compound and other not biodegradable emerging organic pollution materials at present in municipal effluent, these materials generally believe to have toxicity to human body and environment.Traditional waste water treatment process can not effectively be removed on the one hand, brings the secondary pollution on receiving water body and excess sludge disposal ground, and then affects water supply plant water source and local quality of groundwater; On the other hand, conventional handling technology of water supply coagulation, precipitation, filtration are to wherein a part of material not obvious effect.Although advanced oxidation and membrane sepn can remove the emerging organic pollution materials of part in water effectively, because many reasons are not applied in Water purification, poisonous emerging organic pollution materials must threaten water safety once enter water source.In order to alleviate this pollutant, human health being endangered, finding and being applicable to China's national situation and cost-effective city sewage deep treatment technology to remove these pollutents extremely urgent.
Carbamzepine (Carbamazepine) is a kind of medicine that can prevent or treat the sacred disease such as epileptics, manic depression, be used for the treatment of epilepsy grand mal and psychomotor seizure, also trigeminal neuralgia can be treated, chemistry 5H-dibenzo [b by name, f] azatropylidene-5-methane amide, it is white or off-white color crystalline powder, fusing point 189 ~ 192
0c, molecular formula is C
15h
12n
2o, molecular weight is 236.27, all frequently to be detected in environment receiving water body and concentrations is relatively high, there is potential eco-toxicity, it is PPCPs pollutant of greatest concern at present, it is heteroaromatic compound, belongs to the organism of difficult for biological degradation, and traditional sewage water treatment method is (as A
2the methods such as/O, absorption, ultraviolet) and the coagulation of routine, precipitation, filtration handling technology of water supply all can not effectively remove.
Bipolar three-dimensional electrode is a kind of novel advanced oxidization method, and under the effect of catalyzer, can have the material such as hydroxyl radical free radical and hydrogen peroxide of strong oxidizing property at granule electrode Surface Creation, be the key substance of degradation of organic substances pollutent.Organic pollutant technology in bipolar three-dimensional electrode degrading waste water fails to realize industrialization so far, its major cause is that current efficiency is low, energy consumption is high, and the difficult point of process hardly degraded organic substance is two " time " problems: one is how the process electrocatalysis speed of degradation of organic substances and efficiency improve; Another is problem electrode life, and namely how the stability of electrode improves.For the former, to start with from the granule electrode of development high electrocatalytic active and efficient reactor design and solve; For the latter, then to start with research from the structure of granule electrode and preparation method.At present conventional several granule electrodes comprise gac, the metal of metal oxide and load or metal oxide, but these granule electrodes there are the following problems: the impedance of activated carbon granule is relatively little, fill in when running in 3 D electrode reactor and easily form short-circuit current, thus reduction current efficiency, and activated carbon particles also there will be powder phenomenon-tion in electrolytic process; Metal oxide particle electrode has some poisonous Ion release in electrolytic process, can become secondary pollutant, such as PbO
2granule electrode; The metal of load or metal oxide overcome the shortcoming of activated carbon grain sub-electrode, improve water treatment efficiency, but also there is loaded metal and be easy to problems such as coming off.Therefore, the technical problem to be solved in the present invention is for material Carbamzepine difficult in effluent of municipal sewage plant, there is provided a kind of persistence Electrocatalytic particle electrode and the preparation method with efficient degradation Carbamzepine, to solve the problem that existing Technology of Sewage process Carbamzepine is low, granule electrode stability is inadequate, the life-span is short, electrode material cost is higher.
Summary of the invention
The present invention is directed to above problem, a kind of efficient degradation Carbamzepine Electrocatalytic particle electrode and preparation method thereof is provided.Granule electrode material provided by the present invention is as the working electrode of 3 D electrode reactor, and difficult material Carbamzepine in effluent of municipal sewage plant of can effectively degrading, and current efficiency is high, energy consumption is low, and the granule electrode life-span is long.
One of technical scheme of the present invention is to provide one to be had efficient degradation Carbamzepine Electrocatalytic particle electrode and is made up of dry coal gangue particle, dry fine clay, pore former, activator, load agent.
Described pore former can be the one in powdered carbon, saw dust, starch.
Described activator can be Fe
3o
4, Fe
2o
3,mnO
2, one in CuO.
Described coal gangue is the solid waste discharged in coal mining process and coal washing process, a kind of black gray expandable rock lower, harder than coal with a kind of carbon content of coal seam association in coalification course, comprise choose from the spoil of extraction top board, base plate and interlayer and coal washing process in the digging gangue in tunnelling process, mining process wash spoil.Its main component is Al
2o
3, SiO
2, also contain the Fe that quantity does not wait in addition
2o
3, CaO, MgO, Na
2o, K
2o, P
2o
5, SO
3with micro-rare elements (gallium, vanadium, titanium, cobalt).
Described load agent is SnC1
45H
20 and Mn (NO
3)
2.
Two of technical scheme of the present invention is to provide a kind of preparation method with the granule electrode of efficient weather resistance electrocatalysis function, comprises the following steps:
A, coal gangue particle ball milling in ball mill, successively in diluted acid (10% hydrochloric acid), diluted alkaline (10% sodium hydroxide), boil half an hour after taking out, then use distilled water flushing, immersion, dry at 105 DEG C in baking oven, then cross 60 mesh sieves, get dry thin coal gangue particle for subsequent use;
B, clay are put in 105 DEG C of oven dry in baking oven, are pulverized by the clay of oven dry in mortar, then cross 60 mesh sieves, get dry fine clay for subsequent use;
C, by dry fine clay, pore former and the activator in thin for the drying in steps A coal gangue particle, step B according to certain weight percent, mix and stir, preparation mixed raw material;
D, by SnC1
45H
20 and Mn (NO
3)
2with amount of substance than being dissolved in hydrochloric acid for 82:45, then adding dehydrated alcohol wiring solution-forming, stirring, obtaining colloidal sol;
E, the mixed raw material in step C be impregnated in 4h in the colloidal sol that obtains in step D, then dry at 105 DEG C in baking oven, be cooled to room temperature, preparation load raw material;
F, the load raw material in step e are squeezed into raw material ball, and dry 24 hours at 120 DEG C in an oven;
G, by step F dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 10-30min, rise to 850 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain new and effective persistence Electrocatalytic particle electrode.
Mixed raw material is according to weight percent meter, and dry carefully coal gangue particle accounts for 50-60%, dry fine clay accounts for 10-20%, pore former accounts for 10-20%, activator accounts for 10-20%.
Described pore former can be the one in powdered carbon, saw dust, starch.
Described activator can be Fe
3o
4, Fe
2o
3,mnO
2, one in CuO.
Described coal gangue is the solid waste discharged in coal mining process and coal washing process, a kind of black gray expandable rock lower, harder than coal with a kind of carbon content of coal seam association in coalification course, comprise choose from the spoil of extraction top board, base plate and interlayer and coal washing process in the digging gangue in tunnelling process, mining process wash spoil.Its main component is Al
2o
3, SiO
2, also contain the Fe that quantity does not wait in addition
2o
3, CaO, MgO, Na
2o, K
2o, P
2o
5, SO
3with micro-rare elements (gallium, vanadium, titanium, cobalt).
The efficient degradation Carbamzepine Electrocatalytic particle electrode prepared by above-mentioned preparation method, getting solid waste is coal gangue.Containing the Fe with electrocatalysis in coal gangue
2o
3with micro-rare elements (gallium, vanadium, titanium, cobalt), after together with pore former, activator mix, good electrocatalytic reaction can be produced, particle surface is made to form porous state, there is good absorption property, can conduct electricity, there is certain catalytic performance, preparation technology adopts the technical process of first load reshaping, the work-ing life of granule electrode can be ensured, in electrolytic process, produce the materials such as the hydroxyl radical free radical having strong oxidizing property and hydrogen peroxide, the dissolved oxygen in electrolyzer is reduced into H on anode simultaneously
2o
2.Carbamzepine one side and active intermediate generation electrochemical combustion are CO by mineralising
2and H
2o; Another aspect and active intermediate generation electrochemical conversion, organism is oxidized to a series of low-carbon (LC) intermediate product.And the solid waste coal gangue discharged in coal mining process and coal washing process, its stacking not only needs fund and large-area storage yard, and contaminate environment.Utilize coal gangue to make the particle-catalytic electrode of three-diemsnional electrode, can turn waste into wealth, reduce the problem such as pollution, appropriation of land of environment.
Efficient degradation Carbamzepine Electrocatalytic particle electrode provided by the invention and preparation method thereof, meets the environmental protection policy of current national energy-saving and emission-reduction.The granule electrode porous of preparation, and aperture is large, having very large specific surface area, very strong absorption property, good electroconductibility and catalytic performance is a kind of new and effective persistence Electrocatalytic particle electrode.
Below in conjunction with embodiment, the invention will be further described
Embodiment one:
A, coal gangue particle ball milling in ball mill, successively in diluted acid (10% hydrochloric acid), diluted alkaline (10% sodium hydroxide), boil half an hour after taking out, then use distilled water flushing, immersion, dry at 105 DEG C in baking oven, then cross 60 mesh sieves, get dry thin coal gangue particle for subsequent use;
B, clay are put in 105 DEG C of oven dry in baking oven, are pulverized by the clay of oven dry in mortar, then cross 60 mesh sieves, get dry fine clay for subsequent use;
C, by dry fine clay, powdered carbon and the Fe in thin for the drying in steps A coal gangue particle, step B
3o
4according to the weight percent of 50%:20%:20%:10%, mix and stir, preparation mixed raw material;
D, by SnC1
45H
20 and Mn (NO
3)
2with amount of substance than being dissolved in hydrochloric acid for 82:45, then adding dehydrated alcohol wiring solution-forming, stirring, obtaining colloidal sol;
E, the mixed raw material in step C be impregnated in 4h in the colloidal sol that obtains in step D, then dry at 105 DEG C in baking oven, be cooled to room temperature, preparation load raw material;
F, the load raw material in step e are squeezed into raw material ball, and dry 24 hours at 120 DEG C in an oven;
G, by step F dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 10-30min, rise to 850 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain new and effective degraded Carbamzepine Electrocatalytic particle electrode.
Get the efficient degradation Carbamzepine Electrocatalytic particle electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, be 6.0V at voltage, when electric current is 0.2A, energising degraded 30ml municipal wastewater 30min, Carbamzepine clearance reaches 96%.
Embodiment two:
A, coal gangue particle ball milling in ball mill, successively in diluted acid (10% hydrochloric acid), diluted alkaline (10% sodium hydroxide), boil half an hour after taking out, then use distilled water flushing, immersion, dry at 105 DEG C in baking oven, then cross 60 mesh sieves, get dry thin coal gangue particle for subsequent use;
B, clay are put in 105 DEG C of oven dry in baking oven, are pulverized by the clay of oven dry in mortar, then cross 60 mesh sieves, get dry fine clay for subsequent use;
C, by dry fine clay, saw dust and the Fe in thin for the drying in steps A coal gangue particle, step B
2o
3according to the weight percent of 55%:15%:15%:15%, mix and stir, preparation mixed raw material;
D, by SnC1
45H
20 and Mn (NO
3)
2with amount of substance than being dissolved in hydrochloric acid for 82:45, then adding dehydrated alcohol wiring solution-forming, stirring, obtaining colloidal sol;
E, the mixed raw material in step C be impregnated in 4h in the colloidal sol that obtains in step D, then dry at 105 DEG C in baking oven, be cooled to room temperature, preparation load raw material;
F, the load raw material in step e are squeezed into raw material ball, and dry 24 hours at 120 DEG C in an oven;
G, by step F dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 10-30min, rise to 850 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain new and effective degraded Carbamzepine Electrocatalytic particle electrode.
Get the efficient degradation Carbamzepine Electrocatalytic particle electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, be 6.0V at voltage, when electric current is 0.2A, energising degraded 30ml municipal wastewater 30min, CODcr clearance reaches 94%.
Claims (8)
1. an efficient degradation Carbamzepine Electrocatalytic particle electrode, is characterized in that: according to weight percent meter, and carefully coal gangue particle accounts for 50-60%, dry fine clay accounts for 10-20%, pore former accounts for 10-20%, activator accounts for 10-20% to comprise drying.
2. efficient degradation Carbamzepine Electrocatalytic particle electrode as claimed in claim 1, is characterized in that: pore former can be the one in carbon dust, saw dust, starch.
3. efficient degradation Carbamzepine Electrocatalytic particle electrode as claimed in claim 1, is characterized in that: activator can be Fe
3o
4, Fe
2o
3,mnO
2, one in CuO.
4. a preparation method for efficient degradation Carbamzepine Electrocatalytic particle electrode, is characterized in that, comprises the following steps:
A, coal gangue particle ball milling in ball mill, successively in diluted acid (10% hydrochloric acid), diluted alkaline (10% sodium hydroxide), half an hour is boiled after taking out, use distilled water flushing, immersion (object is the impurity such as the organism of removal surface adsorption) again, dry at 105 DEG C in baking oven, then cross 60 mesh sieves, get dry thin coal gangue particle for subsequent use;
B, clay are put in 105 DEG C of oven dry in baking oven, are pulverized by the clay of oven dry in mortar, then cross 60 mesh sieves, get dry fine clay for subsequent use;
C, by dry fine clay, pore former and the activator in thin for the drying in steps A coal gangue particle, step B according to certain weight percent, mix and stir, preparation mixed raw material;
D, by SnC1
45H
20 and Mn (NO
3)
2with amount of substance than being dissolved in hydrochloric acid for 82:45, then adding dehydrated alcohol wiring solution-forming, stirring, obtaining colloidal sol;
E, the mixed raw material in step C be impregnated in 4h in the colloidal sol that obtains in step D, then dry at 105 DEG C in baking oven, be cooled to room temperature, preparation load raw material;
F, the load raw material in step e are squeezed into raw material ball, and dry 24 hours at 120 DEG C in an oven;
G, by step F dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 10-30min, rise to 850 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain efficient degradation Carbamzepine Electrocatalytic particle electrode.
5. the preparation method of efficient degradation Carbamzepine Electrocatalytic particle electrode as claimed in claim 4, it is characterized in that: according to weight percent meter, dry carefully coal gangue particle accounts for 50-60%, dry fine clay accounts for 10-20%, pore former accounts for 10-20%, activator accounts for 10-20%.
6. the preparation method of efficient degradation Carbamzepine Electrocatalytic particle electrode as claimed in claim 4, is characterized in that: described pore former can be the one in powdered carbon, saw dust, starch.
7. the preparation method of efficient degradation Carbamzepine Electrocatalytic particle electrode as claimed in claim 4, is characterized in that: described activator can be Fe
3o
4, Fe
2o
3, MnO
2, one in CuO.
8. the preparation method of efficient degradation Carbamzepine Electrocatalytic particle electrode as claimed in claim 4, is characterized in that: described load agent is SnC1
45H
20 and Mn (NO
3)
2.
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|---|---|---|---|
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|---|---|---|---|
| CN201610022393.5A CN105481062A (en) | 2016-01-14 | 2016-01-14 | Electro-catalytic particle electrode for efficiently decomposing carbamazepine and preparation method of electro-catalytic particle electrode |
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ID=55668397
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249523A (en) * | 2017-12-29 | 2018-07-06 | 桑德生态科技有限公司 | Activated carbon catalysis granule electrode of supported ferriferous oxide and preparation method thereof |
| CN114314763A (en) * | 2021-12-14 | 2022-04-12 | 安徽元琛环保科技股份有限公司 | Preparation method of environment-friendly three-dimensional particle electrode and prepared electrode |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890331A (en) * | 2010-07-30 | 2010-11-24 | 东华大学 | High strength dried regenerative CO2 adsorbent taking coal gangue as carrier and preparation thereof |
| CN102211807A (en) * | 2011-05-04 | 2011-10-12 | 南京工业大学 | High-density porous support for treating wastewater of biological fluidized bed and preparation method thereof |
| CN104276814A (en) * | 2013-07-03 | 2015-01-14 | 济南大学 | Red mud based particle electrode and preparation method thereof |
-
2016
- 2016-01-14 CN CN201610022393.5A patent/CN105481062A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890331A (en) * | 2010-07-30 | 2010-11-24 | 东华大学 | High strength dried regenerative CO2 adsorbent taking coal gangue as carrier and preparation thereof |
| CN102211807A (en) * | 2011-05-04 | 2011-10-12 | 南京工业大学 | High-density porous support for treating wastewater of biological fluidized bed and preparation method thereof |
| CN104276814A (en) * | 2013-07-03 | 2015-01-14 | 济南大学 | Red mud based particle electrode and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249523A (en) * | 2017-12-29 | 2018-07-06 | 桑德生态科技有限公司 | Activated carbon catalysis granule electrode of supported ferriferous oxide and preparation method thereof |
| CN114314763A (en) * | 2021-12-14 | 2022-04-12 | 安徽元琛环保科技股份有限公司 | Preparation method of environment-friendly three-dimensional particle electrode and prepared electrode |
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Application publication date: 20160413 |