CN105621543A - Electrocatalytic particle electrode for efficiently degrading bezafibrate in wastewater and preparation method thereof - Google Patents
Electrocatalytic particle electrode for efficiently degrading bezafibrate in wastewater and preparation method thereof Download PDFInfo
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- CN105621543A CN105621543A CN201610022345.6A CN201610022345A CN105621543A CN 105621543 A CN105621543 A CN 105621543A CN 201610022345 A CN201610022345 A CN 201610022345A CN 105621543 A CN105621543 A CN 105621543A
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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
- C02F1/46114—Electrodes in particulate form or with conductive and/or non conductive particles between them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
The invention relates to an electrocatalytic particle electrode for efficiently degrading bezafibrate in wastewater and a preparation method thereof, belonging to the technical field of wastewater treatment. The preparation method comprises the following steps: uniformly mixing and stirring treated nonferrous metal slag, clay, a pore forming agent and an activator used as raw materials according to a certain weight ratio to prepare a mixed crude material, impregnating the mixed crude material in a carrier sol, drying, cooling to room temperature, extruding to obtain fresh pellets, drying, heating at specific temperature for activation and roasting for some time, taking out, and cooling to room temperature to obtain the finished product. The electrocatalytic particle electrode for efficiently degrading bezafibrate is porous, has large specific area, high adsorbability and favorable electrocatalytic property, and can degrade bezafibrate efficiently. The electrocatalytic particle electrode and preparation method thereof fully utilize the nonferrous metal slag, thereby changing the waste into valuable substances, reducing the environmental pollution and solving the problems of land occupation and the like.
Description
Technical field
The invention belongs to technical field of waste water processing, particularly to a kind of for Electrocatalytic particle electrode of bezafibrate and preparation method thereof in Treating Municipal Sewage.
Background technology
Along with expanding economy, being widely present at present from the heavy metal in industrial wastewater, phenolic compound and other not biodegradable emerging organic pollution materials in municipal sewage, these materials generally believe that human body and environment are had toxicity. Traditional waste water treatment process can not effectively be removed on the one hand, brings receiving water body and the secondary pollution on excess sludge disposal ground, and then affects water supply plant water source and local quality of groundwater; On the other hand, a portion material is not had obvious effect by the handling technology of water supply coagulation of routine, precipitation, filtration. Although advanced oxidation and membrance separation can remove the emerging organic pollution materials of part in water effectively, but do not apply in Water purification because of many reasons, poisonous emerging organic pollution materials must threaten water safety once enter water source. In order to alleviate this pollutant, human health being endangered, it is extremely urgent that the applicable China's national situation of searching and cost-effective city sewage deep treatment technology remove these pollutant.
Bezafibrate (Bezafibrate) is the medicine that a kind of chlorine shellfish butanoic acid derivative class regulates blood fat, it is mainly used in the treatment of hyperlipemia, Chinese another name is 2-[4-[2-(4-chIorobenzoyIamino) ethyl] phenoxy group]-2 Methylpropionic acid, it is white or off-white color crystallization or crystalline powder, fusing point 180 ~ 1840C, molecular formula is C19H20ClNO4, molecular weight is 361.82, environment receiving water body is frequently detected, and concentrations is of a relatively high, there is potential eco-toxicity, it it is PPCPs pollutant of greatest concern at present, it is heteroaromatic compound, belong to the Organic substance of difficult for biological degradation, traditional sewage water treatment method is (such as A2The methods such as/O, absorption, ultraviolet) and the coagulation of routine, precipitation, filtration handling technology of water supply be unable to effective removal.
Bipolar three-dimensional electrode is a kind of novel advanced oxidization method, it is possible to the material such as hydroxyl radical free radical and the hydrogen peroxide at granule electrode Surface Creation under the effect of catalyst with strong oxidizing property, is the key substance of degradation of organic substances pollutant. Organic pollution technology in bipolar three-dimensional electrode degrading waste water fails to realize industrialization so far; its main cause is that current efficiency is low; energy consumption is high, and the difficult point processing hardly degraded organic substance is in that two " time " problems: one is process the electro-catalysis speed of degradation of organic substances and how efficiency improves; Another is problem electrode life, and namely how the stability of electrode improves. For the former, to start with from the granule electrode and efficient reactor design of developing high electrocatalytic active and solve; For the latter, then to start with research from the structure of granule electrode and preparation method. Several granule electrodes conventional at present include metal or the metal-oxide of activated carbon, metal-oxide and load, but these granule electrodes there are the following problems: the impedance of activated carbon granule is relatively small, fill in and easily form short circuit current when 3 D electrode reactor runs, thus reducing current efficiency, and activated carbon particles there is also powder phenomenon-tion in electrolytic process; Metal oxide particle electrode has the Ion release that some are poisonous in electrolytic process, can become secondary pollution, for instance PbO2Granule electrode; The metal of load or metal-oxide overcome the shortcoming of activated carbon grain sub-electrode, improve water treatment efficiency, but there is also carried metal and be prone to problems such as coming off. Therefore, the technical problem to be solved in the present invention is for material bezafibrate difficult in effluent of municipal sewage plant, there is provided a kind of persistency Electrocatalytic particle electrode with efficient degradation bezafibrate and preparation method, to solve the existing Technology of Sewage process problem that bezafibrate 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 problem above, it is provided that a kind of for Electrocatalytic particle electrode of bezafibrate and preparation method thereof in efficient degradation waste water. Granule electrode material provided by the present invention is as the working electrode of 3 D electrode reactor, and difficult material bezafibrate in effluent of municipal sewage plant of can effectively degrading, and current efficiency height, energy consumption is low, and the granule electrode life-span is long.
One of technical scheme be to provide one have efficient degradation bezafibrate Electrocatalytic particle electrode by drying non-ferrous metal solid impurity particle, dry fine clay, pore former, activator, load agent are constituted.
Described pore former can be the one in powdered carbon, saw dust, starch.
Described activator can be Fe3O4��Fe2O3��MnO2, one in CuO.
Described non-ferrous metal slag is non-ferrous metal slag is the waste residue that Non-ferrous minerals produces in smelting, belongs to the one of metallurgical slag. Two classes can be divided: the residue discharged in the molten slag formed in pyrometallurgical smelting and hydrometallurgy by production technology. By the character of metalliferous mineral, heavy metal slag (such as copper ashes, lead skim, cadmia, nickel slag etc.), light metal slag (as refined the red mud that aluminium oxide produces) and rare metal slag can be divided into.
Described load agent is SnC14��5H20 and Mn (NO3)2��
The preparation method that the two of technical scheme are to provide a kind of granule electrode with efficient durability electro-catalysis function, comprises the following steps:
A, non-ferrous metal solid impurity particle ball milling in ball mill, successively boil half an hour in diluted acid (10% hydrochloric acid), diluted alkaline (10% sodium hydroxide) after taking-up, then with distilled water flushing, immersion, dry at 105 DEG C in baking oven, then cross 60 mesh sieves, take dry thin non-ferrous metal solid impurity particle standby;
B, clay are put in baking oven 105 DEG C of drying, are pulverized by the clay dried in mortar, and then mistake 60 mesh sieves, take dry fine clay standby;
C, by the dry thin non-ferrous metal solid impurity particle in step A, the dry fine clay in step B, pore former and activator according to certain percentage by weight, be mixed and stirred for uniformly, prepare mixed raw material;
D, by SnC14��5H20 and Mn (NO3)2It is dissolved in hydrochloric acid with amount of substance ratio for 82:45, adds dehydrated alcohol wiring solution-forming, stir, obtain colloidal sol;
E, the mixed raw material in step C be impregnated in 4h in the colloidal sol obtained in step D, dry at 105 DEG C in baking oven, be cooled to room temperature, prepare 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, it is placed in high temperature furnace and rises 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 persistency Electrocatalytic particle electrode.
Mixed raw material is according to weight percent meter, and dry thin non-ferrous metal solid impurity 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 Fe3O4��Fe2O3��MnO2, one in CuO.
Described non-ferrous metal slag is the waste residue that Non-ferrous minerals produces in smelting, belongs to the one of metallurgical slag. Two classes can be divided: the residue discharged in the molten slag formed in pyrometallurgical smelting and hydrometallurgy by production technology. By the character of metalliferous mineral, heavy metal slag (such as copper ashes, lead skim, cadmia, nickel slag etc.), light metal slag (as refined the red mud that aluminium oxide produces) and rare metal slag can be divided into.
By efficient degradation bezafibrate Electrocatalytic particle electrode prepared by above-mentioned preparation method, taking solid waste is non-ferrous metal slag. Containing the Fe with electrocatalysis in non-ferrous metal slag2O3With trace rare element (gallium, vanadium, titanium, cobalt), after mixing with pore former, activator, 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 technological process of first load reshaping, can ensure that the service life of granule electrode, having the material such as hydroxyl radical free radical and hydrogen peroxide of strong oxidizing property in electrolytic process, the dissolved oxygen in electrolysis bath is reduced into H on anode simultaneously2O2. Bezafibrate one side and reactive intermediate generation electrochemical combustion, be mineralized as CO2And H2O; On the other hand with reactive intermediate generation electrochemical conversion, Organic substance is oxidized to a series of low-carbon (LC) intermediate product. And, the waste residue non-ferrous metal slag that Non-ferrous minerals produces in smelting, it is stacked not only needs fund and large-area storage yard, and contaminated environment. Utilize non-ferrous metal slag to make the particle-catalytic electrode of three-diemsnional electrode, it is possible to turn waste into wealth, reduce the problems such as the pollution of environment, appropriation of land.
Efficient degradation bezafibrate 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 big, having very big specific surface area, very strong absorption property, good electric conductivity and catalytic performance is a kind of new and effective persistency Electrocatalytic particle electrode.
Below in conjunction with detailed description of the invention, the invention will be further described
Embodiment one:
A, non-ferrous metal solid impurity particle ball milling in ball mill, successively boil half an hour in diluted acid (10% hydrochloric acid), diluted alkaline (10% sodium hydroxide) after taking-up, then with distilled water flushing, immersion, dry at 105 DEG C in baking oven, then cross 60 mesh sieves, take dry thin non-ferrous metal solid impurity particle standby;
B, clay are put in baking oven 105 DEG C of drying, are pulverized by the clay dried in mortar, and then mistake 60 mesh sieves, take dry fine clay standby;
C, by the dry thin non-ferrous metal solid impurity particle in step A, the dry fine clay in step B, powdered carbon and Fe3O4According to the percentage by weight of 50%:20%:20%:10%, it is mixed and stirred for uniformly, preparing mixed raw material;
D, by SnC14��5H20 and Mn (NO3)2It is dissolved in hydrochloric acid with amount of substance ratio for 82:45, adds dehydrated alcohol wiring solution-forming, stir, obtain colloidal sol;
E, the mixed raw material in step C be impregnated in 4h in the colloidal sol obtained in step D, dry at 105 DEG C in baking oven, be cooled to room temperature, prepare 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, it is placed in high temperature furnace and rises 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 the Electrocatalytic particle electrode of bezafibrate in new and effective degrading waste water.
Take the Electrocatalytic particle electrode 5.0g of bezafibrate in the efficient degradation waste water prepared in above-described embodiment, be filled in reactor, prepare 3 D electrode reactor, it is 6.0V at voltage, when electric current is 0.2A, energising degraded 30ml municipal wastewater 30min, bezafibrate clearance reaches 99%.
Embodiment two:
A, non-ferrous metal solid impurity particle ball milling in ball mill, successively boil half an hour in diluted acid (10% hydrochloric acid), diluted alkaline (10% sodium hydroxide) after taking-up, then with distilled water flushing, immersion, dry at 105 DEG C in baking oven, then cross 60 mesh sieves, take dry thin non-ferrous metal solid impurity particle standby;
B, clay are put in baking oven 105 DEG C of drying, are pulverized by the clay dried in mortar, and then mistake 60 mesh sieves, take dry fine clay standby;
C, by the dry thin non-ferrous metal solid impurity particle in step A, the dry fine clay in step B, saw dust and Fe2O3According to the percentage by weight of 55%:15%:15%:15%, it is mixed and stirred for uniformly, preparing mixed raw material;
D, by SnC14��5H20 and Mn (NO3)2It is dissolved in hydrochloric acid with amount of substance ratio for 82:45, adds dehydrated alcohol wiring solution-forming, stir, obtain colloidal sol;
E, the mixed raw material in step C be impregnated in 4h in the colloidal sol obtained in step D, dry at 105 DEG C in baking oven, be cooled to room temperature, prepare 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, it is placed in high temperature furnace and rises 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 the Electrocatalytic particle electrode of bezafibrate in new and effective degrading waste water.
Take a kind of of preparation in above-described embodiment and be filled in reactor for the Electrocatalytic particle electrode 5.0g of bezafibrate in efficient degradation waste water, prepare 3 D electrode reactor, it is 6.0V at voltage, when electric current is 0.2A, energising degraded 30ml municipal wastewater 30min, CODcr clearance reaches 96%.
Claims (8)
1. one kind for the Electrocatalytic particle electrode of bezafibrate in efficient degradation waste water, it is characterized in that: according to weight percent meter, account for 50-60% including dry thin non-ferrous metal solid impurity particle, dry fine clay accounts for 10-20%, pore former accounts for 10-20%, activator accounts for 10-20%.
2. the Electrocatalytic particle electrode of bezafibrate in efficient degradation waste water as claimed in claim 1, it is characterised in that: pore former can be the one in carbon dust, saw dust, starch.
3. the Electrocatalytic particle electrode of bezafibrate in efficient degradation waste water as claimed in claim 1, it is characterised in that: activator can be Fe3O4��Fe2O3��MnO2, one in CuO.
4. one kind for the preparation method of the Electrocatalytic particle electrode of bezafibrate in efficient degradation waste water, it is characterised in that comprise the following steps:
A, non-ferrous metal solid impurity particle ball milling in ball mill, successively boil half an hour in diluted acid (10% hydrochloric acid), diluted alkaline (10% sodium hydroxide) after taking-up, then with distilled water flushing, immersion, dry at 105 DEG C in baking oven, then cross 60 mesh sieves, take dry thin non-ferrous metal solid impurity particle standby;
B, clay are put in baking oven 105 DEG C of drying, are pulverized by the clay dried in mortar, and then mistake 60 mesh sieves, take dry fine clay standby;
C, by the dry thin non-ferrous metal solid impurity particle in step A, the dry fine clay in step B, pore former and activator according to certain percentage by weight, be mixed and stirred for uniformly, prepare mixed raw material;
D, by SnC14��5H20 and Mn (NO3)2It is dissolved in hydrochloric acid with amount of substance ratio for 82:45, adds dehydrated alcohol wiring solution-forming, stir, obtain colloidal sol;
E, the mixed raw material in step C be impregnated in 4h in the colloidal sol obtained in step D, dry at 105 DEG C in baking oven, be cooled to room temperature, prepare 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, it is placed in high temperature furnace and rises 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 bezafibrate Electrocatalytic particle electrode.
5. the preparation method of the Electrocatalytic particle electrode of bezafibrate in efficient degradation waste water as claimed in claim 4, it is characterized in that: according to weight percent meter, dry thin non-ferrous metal solid impurity 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 the Electrocatalytic particle electrode of bezafibrate in efficient degradation waste water as claimed in claim 4, it is characterised in that: described pore former can be the one in powdered carbon, saw dust, starch.
7. the preparation method of the Electrocatalytic particle electrode of bezafibrate in efficient degradation waste water as claimed in claim 4, it is characterised in that: described activator can be Fe3O4��Fe2O3��MnO2, one in CuO.
8. the preparation method of the Electrocatalytic particle electrode of bezafibrate in efficient degradation waste water as claimed in claim 4, it is characterised in that: described load agent is SnC14��5H20 and Mn (NO3)2��
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| CN106745528A (en) * | 2016-11-29 | 2017-05-31 | 苏州聚智同创环保科技有限公司 | A kind of recycling sludge containing cupro-nickel prepares three dimensional particles electrode and preparation method thereof |
| CN110028135A (en) * | 2019-04-25 | 2019-07-19 | 郑州大学 | A kind of micro-electrolysis stuffing and application for isolation of purified water body organism |
| CN113277600A (en) * | 2020-02-20 | 2021-08-20 | 中国科学院大连化学物理研究所 | Red mud particle electrode and preparation method and application thereof |
| CN117756237A (en) * | 2024-01-26 | 2024-03-26 | 山东本源环境科技股份有限公司 | Three-dimensional electrocatalytic oxidation device |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745528A (en) * | 2016-11-29 | 2017-05-31 | 苏州聚智同创环保科技有限公司 | A kind of recycling sludge containing cupro-nickel prepares three dimensional particles electrode and preparation method thereof |
| CN110028135A (en) * | 2019-04-25 | 2019-07-19 | 郑州大学 | A kind of micro-electrolysis stuffing and application for isolation of purified water body organism |
| CN110028135B (en) * | 2019-04-25 | 2021-11-19 | 郑州大学 | Micro-electrolysis filler for separating and purifying water organic matters and application thereof |
| CN113277600A (en) * | 2020-02-20 | 2021-08-20 | 中国科学院大连化学物理研究所 | Red mud particle electrode and preparation method and application thereof |
| CN117756237A (en) * | 2024-01-26 | 2024-03-26 | 山东本源环境科技股份有限公司 | Three-dimensional electrocatalytic oxidation device |
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Application publication date: 20160601 |