CN104276631B - A kind of iron scale basal granule sub-electrode and preparation method thereof - Google Patents

A kind of iron scale basal granule sub-electrode and preparation method thereof Download PDF

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Publication number
CN104276631B
CN104276631B CN201310275591.9A CN201310275591A CN104276631B CN 104276631 B CN104276631 B CN 104276631B CN 201310275591 A CN201310275591 A CN 201310275591A CN 104276631 B CN104276631 B CN 104276631B
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iron scale
electrode
granule
shale
dry
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CN104276631A (en
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冯岩
郭玉中
矫浩田
张栋
于衍真
谭娟
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University of Jinan
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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
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • 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
    • C02F2001/46152—Electrodes characterised by the shape or form
    • C02F2001/46157—Perforated or foraminous electrodes
    • C02F2001/46161—Porous electrodes
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

Iron scale 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 iron scale, shale, pore former, activator, by weight percentage, dry thin iron scale granule to be 50-60%, dry thin shale be 10-20%, pore former are 10-20%, activator is 10-20%。The present invention prepares granule electrode with iron scale for raw material, open the new way of iron scale application, achieve and recycle trade waste to greatest extent, improve the level of comprehensive utilization of iron scale, be conducive to the sustainable development of China's industry, solid waste " innoxious, minimizing, resource " is realized for China there is realistic meaning。

Description

A kind of iron scale basal granule sub-electrode and preparation method thereof
Technical field
The invention belongs to technical field of waste water processing, particularly to a kind of for iron scale basal granule sub-electrode of hardly degraded organic substance and preparation method thereof in Treating Municipal Sewage。
Background technology
Iron scale is when steel forging and hot rolling hot-working, due to the reaction formation of oxygen in iron and steel and air。If to these resource rational utilizations, it is possible to reduce production cost, environmental protection and energy saving effect can be played simultaneously。The main component of iron scale is Fe2O3、Fe3O4And FeO, these oxides are also exactly that activation prepared by granule electrode promotes composition。Carrying out the granule electrode of synthesizing efficient, environmental protection hence with the available oxide of these in iron scale, for Treating Municipal Sewage, iron scale can being made to be utilized effectively, thus reaching the purpose of " treatment of wastes with processes of wastes against one another ", it is thus achieved that good economic benefit。
Summary of the invention
It is an object of the invention to iron scale for substrate, it is provided that a kind of iron scale basal granule sub-electrode and preparation method thereof。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 iron scale basal granule sub-electrode, according to weight percent meter, dry thin iron scale granule 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 iron scale is when steel forging and hot rolling hot-working, and due to the reaction formation of oxygen in iron and steel and air, its main component is Fe2O3、Fe3O4And FeO, it is a kind of trade waste。
The preparation method of above-mentioned iron scale basal granule sub-electrode, comprises the steps:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak (washing, the purpose soaked are in that desorption of impurities), dry, then cross 60 mesh sieves, take dry thin iron scale granule standby in baking oven at 120 DEG C；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale standby；
C, by the dry thin iron scale granule 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 120 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 iron scale basal granule sub-electrode material。
According to weight percent meter, dry thin iron scale granule 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。
By iron scale basal granule sub-electrode prepared by above-mentioned preparation method, taking solid waste iron scale is raw material。Containing many oxide, wherein Fe in iron scale2O3、Fe3O4Higher with the content of FeO, these oxides are also exactly activation accelerator compositions prepared by granule electrode。Iron scale basal granule sub-electrode particle surface is rough, and the polluter in waste water has good absorption, removal effect。And, the stacking of iron scale not only needs fund and large-area storage yard, and contaminated environment。Utilize iron scale to make the particle-catalytic electrode of three-diemsnional electrode, it is possible to turn waste into wealth, reduce the pollution of environment, solve the problems such as appropriation of land。
Iron scale 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 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。
Detailed description of the invention
Embodiment one:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak (washing, the purpose soaked are in that desorption of impurities), dry, then cross 60 mesh sieves, take dry thin iron scale granule standby in baking oven at 120 DEG C；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale standby；
C, by the dry thin iron scale granule 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 120 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 iron scale basal granule sub-electrode material。
Taking the iron scale basal granule sub-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 dyeing waste water 45min, CODcr clearance reaches 95%。
Embodiment two:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak (washing, the purpose soaked are in that desorption of impurities), dry, then cross 60 mesh sieves, take dry thin iron scale granule standby in baking oven at 120 DEG C；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale standby；
C, by the dry thin iron scale granule 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 120 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 iron scale basal granule sub-electrode material。
Taking the iron scale basal granule sub-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 dyeing waste water 45min, CODcr clearance reaches 94%。
Embodiment three:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak (washing, the purpose soaked are in that desorption of impurities), dry, then cross 60 mesh sieves, take dry thin iron scale granule standby in baking oven at 120 DEG C；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale standby；
C, by the dry thin iron scale granule 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 120 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 iron scale basal granule sub-electrode material。
Taking the iron scale basal granule sub-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 dyeing waste water 45min, CODcr clearance reaches 94%。
Embodiment four:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak (washing, the purpose soaked are in that desorption of impurities), dry, then cross 60 mesh sieves, take dry thin iron scale granule standby in baking oven at 120 DEG C；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale standby；
C, by the dry thin iron scale granule 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 120 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 iron scale basal granule sub-electrode material。
Taking the iron scale basal granule sub-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 dyeing waste water 45min, CODcr clearance reaches 96%。
Embodiment five:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak (washing, the purpose soaked are in that desorption of impurities), dry, then cross 60 mesh sieves, take dry thin iron scale granule standby in baking oven at 120 DEG C；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale standby；
C, by percentage by weight according to 55%:15%:20%:10% of the dry thin iron scale granule 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 120 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 iron scale basal granule sub-electrode material。
Taking the iron scale basal granule sub-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 dyeing waste water 45min, CODcr clearance reaches 96%。
Embodiment six:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak (washing, the purpose soaked are in that desorption of impurities), dry, then cross 60 mesh sieves, take dry thin iron scale granule standby in baking oven at 120 DEG C；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale standby；
C, by percentage by weight according to 55%:15%:20%:10% of the dry thin iron scale granule 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 120 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 iron scale basal granule sub-electrode material。
Taking the iron scale basal granule sub-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 dyeing waste water 45min, CODcr clearance reaches 97%。
Embodiment seven:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak (washing, the purpose soaked are in that desorption of impurities), dry, then cross 60 mesh sieves, take dry thin iron scale granule standby in baking oven at 120 DEG C；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale standby；
C, by percentage by weight according to 55%:10%:15%:20% of the dry thin iron scale granule 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 120 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 iron scale basal granule sub-electrode material。
Taking the iron scale basal granule sub-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 dyeing waste water 45min, CODcr clearance reaches 94%。

Claims (6)

1. an iron scale basal granule sub-electrode, it is characterised in that: according to weight percent meter, including dry thin iron scale granule 50-60%, dry thin shale 10-20%, pore former 10-20%, activator 10-20%。
2. iron scale basal granule sub-electrode as claimed in claim 1, 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. iron scale basal granule sub-electrode as claimed in claim 1, it is characterised in that: activator is Fe3O4、Fe2O3、MnO2, one in ZnO。
4. the preparation method of an iron scale basal granule sub-electrode, it is characterised in that comprise the following steps:
A, iron scale granule ball milling in ball mill, wash after taking-up, soak, dry in baking oven at 120 DEG C, then crosses 60 mesh sieves, takes dry thin iron scale granule；
B, shale are put in baking oven 120 DEG C of drying, are pulverized by the shale dried in mortar, and then mistake 60 mesh sieves, take dry thin shale；
C, by the dry thin iron scale granule in step A, the dry thin shale in step B, pore former and activator according to certain percentage by weight, including dry thin iron scale granule 50-60%, dry thin shale 10-20%, pore former 10-20%, activator 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 120 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 iron scale basal granule sub-electrode material。
5. the preparation method of iron scale basal granule sub-electrode as claimed in claim 4, it is characterised in that: described pore former is the one in powdered carbon, saw dust, starch, polyvinyl alcohol (PVA), polyvinyl butyral resin (PVB), granules of polystyrene。
6. the preparation method of iron scale basal granule sub-electrode as claimed in claim 4, it is characterised in that: described activator is Fe3O4、Fe2O3、MnO2, one in ZnO。
CN201310275591.9A 2013-07-03 2013-07-03 A kind of iron scale basal granule sub-electrode and preparation method thereof Expired - Fee Related CN104276631B (en)

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CN101698547A (en) * 2009-10-30 2010-04-28 华南理工大学 Composite electrolytic reactor and method for treating pulping waste liquid of chemi-mechanical pulp
CN102001737A (en) * 2010-10-26 2011-04-06 中山大学 Electrocatalysis particle for treating cyanide-containing waste water and method for treating cyanide-containing waste water
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