CN104276812B - A kind of sulfate slag basal granule sub-electrode and preparation method thereof - Google Patents
A kind of sulfate slag basal granule sub-electrode and preparation method thereof Download PDFInfo
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- CN104276812B CN104276812B CN201310275580.0A CN201310275580A CN104276812B CN 104276812 B CN104276812 B CN 104276812B CN 201310275580 A CN201310275580 A CN 201310275580A CN 104276812 B CN104276812 B CN 104276812B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
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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
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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
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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
- C02F2001/46133—Electrodes characterised by the material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Electrochemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
Sulfate slag basal granule sub-electrode that the present invention relates to a kind of 3 D electrode reactor and preparation method thereof: be made up of sulfate slag, shale, pore former, activator, by weight percentage, dry thin sulfate slag particle is 50-60%, dry thin shale is 10-20%, pore former is 10-20%, activator is 10-20%.The present invention is that granule electrode prepared by raw material with sulfate slag, open the new way of sulfate slag application, recycle trade waste to greatest extent, improve the level of comprehensive utilization of sulfate slag, be conducive to the Sustainable development of China's industry, solid waste " innoxious, minimizing, resource utilization " is realized for China there is realistic meaning.
Description
Technical field
The invention belongs to technical field of waste water processing, particularly a kind of sulfate slag basal granule sub-electrode for the treatment of hardly degraded organic substance in municipal effluent and preparation method thereof.
Background technology
Sulfate slag dries slag or slag also known as pyrite, and be that pyrite manufactures the waste residue of discharging in sulfuric acid or sulfurous acid process, main chemical compositions is Fe
2o
3: 20-50%, SiO
2: 15-65%, Al
2o
3: 10%, CaO:5%, MgO<5%, S:1-2%, generally also containing Cu, Co etc.The different utilization ways of its chemical composition is also different, and it is as iron-smelting raw material that probe into Processing high Iron and Sulfur acid sludge the most effectively utilizes, and sulfate slag then can be used as cement raw material, brick producing material etc.Some country has accomplished whole utilization at present, and China's utilization only has about 50%, and all the other all enter environment, piles up and then occupies farmland, contaminated land, enter rivers then polluted-water.Be that raw material preparation is efficient, the granule electrode of environmental protection with sulfate slag, for the treatment of municipal effluent, sulfate slag can be made to be utilized effectively, thus reach the object of " treatment of wastes with processes of wastes against one another ", obtain good economic benefit.
Summary of the invention
The object of the invention is with sulfate slag is matrix, provides a kind of sulfate slag basal granule sub-electrode and preparation method thereof.Granule electrode material provided by the present invention, can organism effectively in degrading waste water as the working electrode of 3 D electrode reactor, and current efficiency is high, and energy consumption is low.
A kind of sulfate slag basal granule sub-electrode, according to weight percent meter, dry thin sulfate slag particle accounts for 50-60%, dry carefully shale 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, polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), granules of polystyrene.
Described activator can be Fe
3o
4, Fe
2o
3,mnO
2, one in ZnO.
Described sulfate slag pyrite manufactures the waste residue of discharging in sulfuric acid or sulfurous acid process, is a kind of trade waste.
The preparation method of above-mentioned sulfate slag basal granule sub-electrode, comprises the steps:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin sulfate slag particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, pore former and the activator in thin for the drying in steps A sulfate slag particle, step B according to certain weight percent, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 1050 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
According to weight percent meter, dry thin sulfate slag particle accounts for 50-60%, dry carefully shale 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, polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), granules of polystyrene.
Described activator can be Fe
3o
4, Fe
2o
3,mnO
2, one in ZnO.
The sulfate slag basal granule sub-electrode prepared by above-mentioned preparation method, getting solid waste sulfate slag is raw material.Containing many oxide, wherein Fe in sulfate slag
2o
3, Fe
3o
4higher with the content of FeO, these oxide compounds are also exactly activation promotor compositions prepared by granule electrode.Sulfate slag basal granule sub-electrode particle surface is rough, have good absorption, removal effect, and the stacking of sulfate slag not only needs fund and large-area storage yard to the pollution substance in waste water, and contaminate environment.Utilize sulfate slag 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.
Sulfate slag basal granule sub-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 granule electrode.
Below in conjunction with embodiment, the invention will be further described.
Embodiment
Embodiment one:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin sulfate slag particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, powdered carbon and the Fe in thin for the drying in steps A sulfate slag particle, step B
3o
4according to the weight percent of 50%:20%:20%:10%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 rise to 550 DEG C with 60 DEG C/h, activation 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
Get the sulfate slag basal granule sub-electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 95%.
Embodiment two:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin sulfate slag particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, saw dust and the Fe in thin for the drying in steps A sulfate slag particle, step B
2o
3according to the weight percent of 55%:15%:15%:15%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 rise to 550 DEG C with 60 DEG C/h, activation 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
Get the sulfate slag basal granule sub-electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 94%.
Embodiment three:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin sulfate slag particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, starch and the MnO in thin for the drying in steps A sulfate slag particle, step B
2according to the weight percent of 60%:15%:15%:10%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 rise to 550 DEG C with 60 DEG C/h, activation 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
Get the sulfate slag basal granule sub-electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 94%.
Embodiment four:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin sulfate slag particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, starch and the MnO in thin for the drying in steps A sulfate slag particle, step B
2according to the weight percent of 60%:10%:10%:20%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 rise to 550 DEG C with 60 DEG C/h, activation 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
Get the sulfate slag basal granule sub-electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 96%.
Embodiment five:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin sulfate slag particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, the thin shale of drying, polyvinyl alcohol (PVA) and ZnO by thin for the drying in steps A sulfate slag particle, step B, according to the weight percent of 55%:15%:20%:10%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 rise to 550 DEG C with 60 DEG C/h, activation 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
Get the sulfate slag basal granule sub-electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 96%.
Embodiment six:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin sulfate slag particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, the thin shale of drying, polyvinyl butyral acetal (PVB) and ZnO by thin for the drying in steps A sulfate slag particle, step B, according to the weight percent of 55%:15%:20%:10%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 rise to 550 DEG C with 60 DEG C/h, activation 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
Get the sulfate slag basal granule sub-electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 97%.
Embodiment seven:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin sulfate slag particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, polystyrene and the ZnO in thin for the drying in steps A sulfate slag particle, step B according to the weight percent of 55%:10%:15%:20%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 rise to 550 DEG C with 60 DEG C/h, activation 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
Get the sulfate slag basal granule sub-electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 94%.
Claims (6)
1. a sulfate slag basal granule sub-electrode, is characterized in that: according to weight percent meter, comprises dry thin sulfate slag particle 50-60%, dry thin shale 10-20%, pore former 10-20%, activator 10-20%.
2. sulfate slag basal granule sub-electrode as claimed in claim 1, is characterized in that: pore former is the one in powdered carbon, saw dust, starch, polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), granules of polystyrene.
3. sulfate slag basal granule sub-electrode as claimed in claim 1, is characterized in that: activator is Fe
3o
4, Fe
2o
3, MnO
2, one in ZnO.
4. a preparation method for sulfate slag basal granule sub-electrode, is characterized in that, comprises the following steps:
A, sulfate slag particle ball milling in ball mill, washing after taking out, immersion, dry at 120 DEG C in baking oven, then crosses 60 mesh sieves, gets dry thin sulfate slag particle;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale;
C, by the thin shale of drying, pore former and the activator in thin for the drying in steps A sulfate slag particle, step B according to certain weight percent, comprise dry thin sulfate slag particle 50-60%, dry thin shale 10-20%, pore former 10-20%, activator 10-20%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D 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 1050 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain sulfate slag basal granule sub-electrode material.
5. the preparation method of sulfate slag basal granule sub-electrode as claimed in claim 4, is characterized in that: described pore former is the one in powdered carbon, saw dust, starch, polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), granules of polystyrene.
6. the preparation method of sulfate slag basal granule sub-electrode as claimed in claim 4, is characterized in that: described activator is Fe
3o
4, Fe
2o
3, MnO
2, one in ZnO.
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| CN103113129A (en) * | 2013-01-31 | 2013-05-22 | 华南理工大学 | Preparation method and application of hierarchical porous bioactive ceramic |
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| CN103113129A (en) * | 2013-01-31 | 2013-05-22 | 华南理工大学 | Preparation method and application of hierarchical porous bioactive ceramic |
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