CN104276626B - A kind of gold tailings basal granule sub-electrode and preparation method thereof - Google Patents

A kind of gold tailings basal granule sub-electrode and preparation method thereof Download PDF

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Publication number
CN104276626B
CN104276626B CN201310275592.3A CN201310275592A CN104276626B CN 104276626 B CN104276626 B CN 104276626B CN 201310275592 A CN201310275592 A CN 201310275592A CN 104276626 B CN104276626 B CN 104276626B
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gold tailings
electrode
dry
shale
thin
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CN104276626A (en
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冯岩
姚赛
李妙婉
范丽莎
于衍真
郭玉中
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University of Jinan
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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
    • C02F1/46114—Electrodes in particulate form or with conductive and/or non conductive particles between them
    • 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)
  • Manufacture And Refinement Of Metals (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

Gold tailings 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 gold tailings, shale, pore former, activator, by weight percentage, dry thin gold tailings particle is 50-60%, dry thin shale is 10-20%, pore former is 10-20%, activator is 10-20%.Utilize gold tailings to prepare gold tailings basal granule sub-electrode, not only can make full use of the effective constituent in gold tailings, and effectively hew out the new way of gold tailings minimizing, resource utilization, eliminate the problem of environmental pollution that it brings, reduce floor space.Gold tailings 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.

Description

A kind of gold tailings basal granule sub-electrode and preparation method thereof
Technical field
The invention belongs to technical field of waste water processing, particularly a kind of gold tailings basal granule sub-electrode for the treatment of hardly degraded organic substance in municipal effluent and preparation method thereof.
Background technology
Three-diemsnional electrode is a kind of novel advanced oxidization method, its conversion zone is no longer confined to the simple geometry of electrode on the surface, but carry out on the surface at the three-dimensional space of whole bed, be particularly useful for the reaction system that in the low or system of DeR speed, limit current density is little.The treatment effect of the performance remarkably influenced 3 D electrode reactor of granule electrode, for using three-dimensional electrodes system, in order to improve current efficiency, on the basis of understanding three-diemsnional electrode mechanism of catalytic reaction in depth, having good electroconductibility, adsorptivity and catalytic performance granule electrode under designing and be prepared in normal temperature and pressure conditions is modern key issue urgently to be resolved hurrily.
Gold tailings is the waste that Gold Ore discharges after the levigate fine ore that extracts gold from, and in yellow powder, has less granularity and relatively uniform size-grade distribution, containing more SiO 2, CaO, Fe 2o 3, Al 2o 3, MgO, have higher surface energy and potential reaction active.Gold ore Gold Content is extremely low, and manufacturing enterprise almost output how many ores just discharges how many mine tailings.The mine tailing that China's gold system is discharged every year is more than 2,450 ten thousand tons.Current comprehensive utilization of tailing rate is very low; be approximately 7%; generally still adopt stacked arrangement process; not only take a large amount of soils; cause Tailings Dam ambient contamination; and substantial contribution need be dropped into for Tailings Dam build and maintenance, therefore gold tailings comprehensive utilization is become to the important topic of gold mine comprehensive utilization of resources and aspect of preserving the ecological environment.
SiO contained in gold tailings 2, CaO, Fe 2o 3, Al 2o 3, the oxide compound such as MgO, the major ingredient of granule electrode exactly, therefore the granule electrode of these utilized units usually synthesizing efficient, the environmental protection in flyash is utilized, for the treatment of municipal effluent, flyash 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
In order to solve gold tailings disposal of resources problem, the invention provides a kind of gold tailings 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 gold tailings basal granule sub-electrode, according to weight percent meter, dry thin gold tailings 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 gold tailings is the waste that Gold Ore discharges after the levigate fine ore that extracts gold from, and in yellow powder, has less granularity and relatively uniform size-grade distribution, containing more SiO 2, CaO, Fe 2o 3, Al 2o 3, MgO, having higher surface energy and potential reaction active, is a kind of slag.
The preparation method of above-mentioned gold tailings basal granule sub-electrode, comprises the steps:
A, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
According to weight percent meter, dry thin gold tailings 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.
Gold tailings is utilized to prepare gold tailings basal granule sub-electrode, not only can make full use of the effective constituent in gold tailings, improve resource utilization, and effectively hew out the new way of gold tailings minimizing, resource utilization, alleviate or eliminate the problem of environmental pollution that it brings.
Gold tailings 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, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
Get the gold tailings 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, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
Get the gold tailings 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, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
Get the gold tailings 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, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
Get the gold tailings 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, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
Get the gold tailings 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, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
Get the gold tailings 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, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
Get the gold tailings 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 (3)

1. a gold tailings basal granule sub-electrode, is characterized in that: according to weight percent meter, comprises dry thin gold tailings particle 50-60%, dry thin shale 10-20%, pore former 10-20%, activator 10-20%; The preparation method of this gold tailings basal granule sub-electrode, comprises the following steps:
A, gold tailings 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 gold tailings 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 gold tailings 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 gold tailings basal granule sub-electrode material.
2. gold tailings 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. gold tailings 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.
CN201310275592.3A 2013-07-03 2013-07-03 A kind of gold tailings basal granule sub-electrode and preparation method thereof Expired - Fee Related CN104276626B (en)

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JP3020553B2 (en) * 1990-05-12 2000-03-15 コニカ株式会社 Fixed-bed type three-dimensional electrode type electrolytic cell
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