CN104276814B - A kind of hole, slag Quito granule electrode - Google Patents

A kind of hole, slag Quito granule electrode Download PDF

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Publication number
CN104276814B
CN104276814B CN201310275570.7A CN201310275570A CN104276814B CN 104276814 B CN104276814 B CN 104276814B CN 201310275570 A CN201310275570 A CN 201310275570A CN 104276814 B CN104276814 B CN 104276814B
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slag
quito
dry
granule electrode
shale
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CN104276814A (en
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冯岩
胡栗
冯升
李妙婉
于衍真
姚赛
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University of Jinan
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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
    • C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
    • 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
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/132—Waste materials; Refuse; Residues
    • C04B33/138—Waste materials; Refuse; Residues from metallurgical processes, e.g. slag, furnace dust, galvanic waste
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • 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)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

A kind of hole, slag Quito granule electrode and preparation method thereof belongs to technical field of waste water processing。The present invention is with the slag after process, shale, pore former, activator for raw material, in constant weight ratio mixing and stirring, is squeezed into raw material ball, it is dried process, be placed under specified temp heat, activation, roasting, after a period of time take out, be cooled to room temperature and obtain finished product。Granule electrode porous prepared by the present invention, has very big specific surface area, very strong absorption property, good electric conductivity and catalytic performance, is a kind of new and effective granule electrode。A kind of hole, slag Quito provided by the invention granule electrode and preparation method thereof, makes full use of trade waste slag, both can turn waste into wealth, and can reduce again the pollution of environment, solve the problems such as land seizure。

Description

A kind of hole, slag Quito granule electrode
Technical field
The invention belongs to technical field of waste water processing, particularly to a kind of for hole, slag Quito granule electrode of hardly degraded organic substance and preparation method thereof in Treating Municipal Sewage。
Background technology
Slag is a kind of solid waste arranged after steel-making, the impurity such as silt particle brought into by oxidized rear oxide, the furnace lining being etched and fettling material, the metal charge generated of element each in metal charge and the slag making materials being intentionally added, such as the refuse that Calx, fluorite, deoxidizer etc. are formed。Slag comparison of ingredients is complicated, and slag processing is always up a difficult problem for puzzlement China steel-making industry。In the past, this solid waste major part is used as roadbed backfilling material, and utilization rate is always very low, has both taken a large amount of urban land, again environment, air is caused severe contamination。If able to obtain the development and utilization of profound level, not only can eliminate environmental pollution, but also huge economic benefit can be created。
Three-diemsnional electrode is a kind of novel advanced oxidization method, its conversion zone is no longer limited on the simple geometry surface of electrode, but carry out on the three dimensions surface of whole bed, it is particularly suited for the reaction system that degradation reaction speed is low or in system, limiting current density is little。The treatment effect of the performance appreciable impact 3 D electrode reactor of granule electrode, the mechanism of action according to granule electrode, in bipolar three-dimensional electrode system, when applying certain voltage in main electrode, it is filled in the granule electrode between the two poles of the earth, because electrostatic induction makes particle two ends with different electric charges, particle two ends respectively become yin, yang the two poles of the earth, and electrochemical reaction occurs thereon。Three conditions must be provided simultaneously with accordingly, as granule electrode: l) in electrostatic field can electrification by induction, this just requires that granule electrode has good electric conductivity, because insulator will not electrification by induction in electrostatic field;2) mutually insulated between particle, to avoid particle to be connected, forms short circuit;3) good catalytic and stability, degraded organic in waste water must be had good catalytic by granule electrode surface mass。For above analysis, the present invention utilizes slag, has invented hole, a kind of slag Quito granule electrode, for three dimensional particles Electrode treatment sewage。
Summary of the invention
The present invention is directed to above analysis, it is provided that a kind of hole, slag Quito granule electrodeAndPreparation method。Granule electrode material provided by the present invention as the working electrode of 3 D electrode reactor, can the effective Organic substance in degrading waste water, and current efficiency is high, and energy consumption is low。
A kind of hole, slag Quito granule electrode, according to weight percent meter, dry thin steel slag particle accounts for 50-60%, dry thin 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 resin (PVB), granules of polystyrene。
Described activator can be Fe3O4、Fe2O3、MnO2, one in ZnO。
Described slag is a kind of solid waste arranged after steel-making, the impurity such as silt particle brought into by oxidized rear oxide, the furnace lining being etched and fettling material, the metal charge generated of element each in metal charge and the slag making materials being intentionally added, such as the refuse that Calx, fluorite, deoxidizer etc. are formed, it it is a kind of trade waste。
The preparation method of hole, above-mentioned slag Quito granule electrode, comprises the steps:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks (washing, the purpose soaked are in that desorption of impurities), dry, then cross 80 mesh sieves, take dry thin steel slag particle standby in baking oven at 105 DEG C；
B, shale are put in baking oven 105 DEG C of drying, the soil sample dried are pulverized in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by the dry thin steel slag particle in step A, the dry thin shale in step B, pore former and activator according to certain percentage by weight, be mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours；
E, by step D 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 1050 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain hole, slag Quito granule electrode material。
According to weight percent meter, dry thin steel slag 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, polyvinyl alcohol (PVA), polyvinyl butyral resin (PVB), granules of polystyrene。
Described activator can be Fe3O4、Fe2O3、MnO2、ZnO、SnO2In one。
By hole, slag Quito granule electrode prepared by above-mentioned preparation method, taking solid waste is slag。The oxide generated after oxidized containing each element in slag, after mixing with pore former, activator, it is possible to produce good chemical reaction, makes particle surface form porous state, has good absorption property, it is possible to conduction, have certain catalytic performance。And, the garbage slag produced in iron and steel smelting process, it is stacked not only needs fund and large-area storage yard, and contaminated environment。Utilize 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。
Hole, slag Quito provided by the invention granule electrode 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 granule electrode。
Below in conjunction with detailed description of the invention, the invention will be further described。
Embodiment one:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks (washing, the purpose soaked are in that desorption of impurities), dry, then cross 80 mesh sieves, take dry thin steel slag particle standby in baking oven at 105 DEG C；
B, shale are put in baking oven 105 DEG C of drying, the soil sample dried are pulverized in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by the dry thin steel slag particle in step A, the dry thin shale in step B, powdered carbon and Fe3O4According to the percentage by weight of 50%:20%:20%:10%, it is mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours；
E, by step D dry after raw material ball, be placed in high temperature furnace and rise to 300 DEG C from room temperature with 120 DEG C/h, heat 2h, then rise to 550 DEG C with 60 DEG C/h, activate 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain hole, slag Quito granule electrode material。
Taking hole, the slag Quito granule electrode 5.0g of preparation in above-described embodiment, be filled in reactor, prepare 3 D electrode reactor, be 6.0V at voltage, when electric current is 0.2A, energising degraded 30ml municipal wastewater 30min, CODcr clearance reaches 95%。
Embodiment two:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks (washing, the purpose soaked are in that desorption of impurities), dry, then cross 80 mesh sieves, take dry thin steel slag particle standby in baking oven at 105 DEG C；
B, shale are put in baking oven 105 DEG C of drying, the soil sample dried are pulverized in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by the dry thin steel slag particle in step A, the dry thin shale in step B, saw dust and Fe2O3According to the percentage by weight of 55%:15%:15%:15%, it is mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours；
E, by step D dry after raw material ball, be placed in high temperature furnace and rise to 300 DEG C from room temperature with 120 DEG C/h, heat 2h, then rise to 550 DEG C with 60 DEG C/h, activate 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain hole, slag Quito granule electrode material。
Taking hole, the slag Quito granule electrode 5.0g of preparation in above-described embodiment, be filled in reactor, prepare 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%。
Embodiment three:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks (washing, the purpose soaked are in that desorption of impurities), dry, then cross 80 mesh sieves, take dry thin steel slag particle standby in baking oven at 105 DEG C；
B, shale are put in baking oven 105 DEG C of drying, the soil sample dried are pulverized in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by the dry thin steel slag particle in step A, the dry thin shale in step B, starch and MnO2According to the percentage by weight of 60%:15%:15%:10%, it is mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours；
E, by step D dry after raw material ball, be placed in high temperature furnace and rise to 300 DEG C from room temperature with 120 DEG C/h, heat 2h, then rise to 550 DEG C with 60 DEG C/h, activate 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain slag porous basal granule sub-electrode material。
Taking hole, the slag Quito granule electrode 5.0g of preparation in above-described embodiment, be filled in reactor, prepare 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%。
Embodiment four:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks (washing, the purpose soaked are in that desorption of impurities), dry, then cross 80 mesh sieves, take dry thin steel slag particle standby in baking oven at 105 DEG C；
B, shale are put in baking oven 105 DEG C of drying, the soil sample dried are pulverized in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by the dry thin steel slag particle in step A, the dry thin shale in step B, starch and MnO2According to the percentage by weight of 60%:10%:10%:20%, it is mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours。
E, by step D dry after raw material ball, be placed in high temperature furnace and rise to 300 DEG C from room temperature with 120 DEG C/h, heat 2h, then rise to 550 DEG C with 60 DEG C/h, activate 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain hole, slag Quito granule electrode material。
Taking hole, the slag Quito granule electrode 5.0g of preparation in above-described embodiment, be filled in reactor, prepare 3 D electrode reactor, be 6.0V at voltage, when electric current is 0.2A, energising degraded 30ml municipal wastewater 30min, CODcr clearance reaches 96%。
Embodiment five:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks (washing, the purpose soaked are in that desorption of impurities), dry, then cross 80 mesh sieves, take dry thin steel slag particle standby in baking oven at 105 DEG C；
B, shale are put in baking oven 105 DEG C of drying, the soil sample dried are pulverized in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by percentage by weight according to 55%:15%:20%:10% of the dry thin steel slag particle in step A, the dry thin shale in step B, polyvinyl alcohol (PVA) and ZnO, be mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours；
E, by step D dry after raw material ball, be placed in high temperature furnace and rise to 300 DEG C from room temperature with 120 DEG C/h, heat 2h, then rise to 550 DEG C with 60 DEG C/h, activate 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain hole, slag Quito granule electrode material。
Taking hole, the slag Quito granule electrode 5.0g of preparation in above-described embodiment, be filled in reactor, prepare 3 D electrode reactor, be 6.0V at voltage, when electric current is 0.2A, energising degraded 30ml municipal wastewater 30min, CODcr clearance reaches 96%。
Embodiment six:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks (washing, the purpose soaked are in that desorption of impurities), dry, then cross 80 mesh sieves, take dry thin steel slag particle standby in baking oven at 105 DEG C；
B, shale are put in baking oven 105 DEG C of drying, the soil sample dried are pulverized in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by percentage by weight according to 55%:15%:20%:10% of the dry thin steel slag particle in step A, the dry thin shale in step B, polyvinyl butyral resin (PVB) and ZnO, be mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours；
E, by step D dry after raw material ball, be placed in high temperature furnace and rise to 300 DEG C from room temperature with 120 DEG C/h, heat 2h, then rise to 550 DEG C with 60 DEG C/h, activate 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain hole, slag Quito granule electrode material。
Taking hole, the slag Quito granule electrode 5.0g of preparation in above-described embodiment, be filled in reactor, prepare 3 D electrode reactor, be 6.0V at voltage, when electric current is 0.2A, energising degraded 30ml municipal wastewater 30min, CODcr clearance reaches 97%。
Embodiment seven:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks (washing, the purpose soaked are in that desorption of impurities), dry, then cross 80 mesh sieves, take dry thin steel slag particle standby in baking oven at 105 DEG C；
B, shale are put in baking oven 105 DEG C of drying, the soil sample dried are pulverized in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by percentage by weight according to 55%:10%:15%:20% of the dry thin steel slag particle in step A, the dry thin shale in step B, polystyrene and ZnO, be mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours；
E, by step D dry after raw material ball, be placed in high temperature furnace and rise to 300 DEG C from room temperature with 120 DEG C/h, heat 2h, then rise to 550 DEG C with 60 DEG C/h, activate 20min, then rise to 1050 DEG C of roasting 30min with 300 DEG C/h, naturally cool to room temperature, obtain hole, slag Quito granule electrode material。
Taking hole, the slag Quito granule electrode 5.0g of preparation in above-described embodiment, be filled in reactor, prepare 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 (3)

1. hole, slag Quito granule electrode, it is characterized in that: according to weight percent meter, including dry thin steel slag particle 50-60%, dry thin shale 10-20%, pore former 10-20%, activator 10-20%, its preparation method is characterised by, comprises the following steps:
A, steel slag particle ball milling in ball mill, washs after taking-up, soaks, dry in baking oven at 105 DEG C, then crosses 80 mesh sieves, takes dry thin steel slag particle standby；
B, shale are put in baking oven 105 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 80 mesh sieves, take dry thin shale standby；
C, by the dry thin steel slag particle in step A, the dry thin shale in step B, pore former and activator according to certain percentage by weight, account for 50-60% including dry thin steel slag particle, dry thin shale accounts for 10-20%, pore former accounts for 10-20%, activator accounts for 10-20%, it is mixed and stirred for uniformly, being squeezed into raw material ball；
D, will at the raw material ball in step C in an oven 105 DEG C dry 24 hours；
E, by step D 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 1050 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain hole, slag Quito granule electrode material。
2. hole, slag Quito as claimed in claim 1 granule electrode, it is characterised in that: pore former is the one in powdered carbon, saw dust, starch, polyvinyl alcohol (PVA), polyvinyl butyral resin (PVB), granules of polystyrene。
3. hole, slag Quito as claimed in claim 1 granule electrode, it is characterised in that: activator is Fe3O4、Fe2O3、MnO2, one in ZnO。
CN201310275570.7A 2013-07-03 2013-07-03 A kind of hole, slag Quito granule electrode Expired - Fee Related CN104276814B (en)

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CN1924102A (en) * 2006-09-05 2007-03-07 陕西科技大学 Preparation method of lead dioxide porous electrode

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