CN107986281A - A kind of Application way of gangue waste material - Google Patents
A kind of Application way of gangue waste material Download PDFInfo
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- CN107986281A CN107986281A CN201711205954.6A CN201711205954A CN107986281A CN 107986281 A CN107986281 A CN 107986281A CN 201711205954 A CN201711205954 A CN 201711205954A CN 107986281 A CN107986281 A CN 107986281A
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- gangue
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
Coordinate the method for comprehensive utilization of the waste and old cathode carbon block of aluminium electrolytic industry the present invention relates to a kind of gangue waste material.It is concretely comprised the following steps：Gangue and waste and old cathode carbon block are smashed into powdering, dispensing according to a certain percentage after drying, the alkali soluble impurity in batch mixing is removed using aqueous alkali, hot water is washed to neutrality, after drying under inertia or reducing atmosphere, it is heated to 1,400 1700 DEG C, the mixed powder of silicon carbide-containing is obtained after insulation a period of time, then by powder, oxidizing fire removes remaining powdered carbon under oxidizing atmosphere, obtained powder is scattered in hydrofluoric acid and removes remaining silica, silicon carbide powder is can obtain after cleaning-drying.Gained silicon carbide products purity of the invention is high, and particle diameter is small, and there is high industrial applicability to be worth.Meanwhile using the Coal Refuse of industry and waste and old cathode carbon block as raw material, waste pollution is being reduced, environmental protection and resource recycling direction have positive effect.
Description
Technical field：
The present invention relates to a kind of Application way of gangue waste material, more particularly to gangue waste material combination aluminium electrolytic industry
The harmless processing of waste and old cathode carbon block and the technical field of resource regeneration.
Background technology：
Gangue is entrained in the rock in coal measure strata, in coalification course with coal seam association, symbiosis it is a kind of carbon containing
Amount black rock low compared with coal, harder than coal, the mixture being made of inanimate matter and a small amount of organic matter.China's spoil accumulates
Up to 7,000,000,000 t, take up an area 70km2, and increased with the speed of 1.5 hundred million t of annual emissions.And the comprehensive utilization of gangue still less than
15%, remaining gangue is stacked loosely in mine surrounding naturally using circular cone type or cheuch Dumpage type more.Become China
Discharge one of maximum waste residue.A large amount of stack of gangue can cause surrounding environment following influence：
(1) large amount of land resources are taken.As the waste of coal mining, gangue can be deposited in around mining area by enterprise,
Form many gangues " mountain ".According to incompletely statistics, to 2015, China adds up about 4,500,000,000 tons of the gangue stacked, scale
Larger coal gangue hill more than 2600, total floor space are that China's yield and accumulating amount are only second to construction waste more than 200,000 mu
Trade waste.
(2) environment is polluted.The gangue stacked for a long time can be changed into tiny loose dust particles under slacking, easily
Blown afloat by strong wind, form dust and sand weather, reduce air quality.In addition, contain the poisonous metals such as Cr, Ni, Cu, Pb member in gangue
Element, can enter in soil, rivers and lakes and underground water with precipitation after rain drop erosion, soil and water quality is being polluted.
(3) threaten to safety in the neighbourhood.The gangue of bulk deposition is there are avalanche, the danger of sliding, in bastard coal
Clitter slope is spent under big, experience precipitation and the effect of other external force and is easier that accident occurs.It is organic containing part in gangue
The combustible materials such as carbon, long-term air storage have the danger of spontaneous combustion under pressure itself and slacking, and gangue spontaneous combustion can be put
Go out CO, SO2、NOxDeng pernicious gas, big bastard coal clitter autoignition time is up to the more than ten years, to very harmful in the neighbourhood.
At present, the utilization ways of gangue are concentrated mainly on following aspect：
(1) coal gangue power generation.Contain part organic carbon in gangue, there is certain calorific value.High-carbon gangue, such as coal separation
Gangue, has higher caloric value, is mixed after crushing with coal slime, may be used as the fuel of power plant fluidized-bed combustion boiler.Coal
Bastard coal lime after spoil burning may be used as cement spike, produce structure material.
(2) building material product is produced.The structure materials such as cement, clay brick, ceramics are the mixtures such as aluminosilicate through high temperature
Obtained building material product is handled, contains abundant SiO in gangue2、Al2O3, it is a kind of cheap aluminum silicate raw material, in addition
Due to containing part carbon in gangue, part calorific value can be provided during high-temperature firing, saves energy expenditure, reduces production
Cost.The coal amount that China is used to produce building material product accounts for gangue utilizes total amount 12%.
(3) subsidence area backfills and fills out hole and builds the road.This method is suitable for that content of organics is few, gangue of high mechanical strength,
It is the main path that current gangue utilizes, its gangue utilization accounts for 56% that gangue utilizes total amount.This method has work
The features such as skill is simple and practicable, adaptation is wide, utilization is big, but need to consider secondary pollution and gangue itself in practical applications
Feature, accomplishes adaptation to local conditions.
More than prevailing gangue utilization ways also there are environmental pollution, utilization rate be high, added value is low and
The shortcomings of scope of application is small, current trend are to explore new utilization of coal gangue approach for reducing or even eliminating gangue
Endanger, realize the sustainable development of changing rejected material to useful resource and society.
The content of the invention
It is difficult to the problems such as effective, high quality utilizes for existing gangue, there is provided a kind of product economic value is high, technique ring
The Application way of the gangue waste material of guarantor.
A kind of Application way of gangue waste material of the present invention, comprises the following steps：
Step 1
In mass ratio, mixture A：Lye=1:5-10, mixture A is placed in lye, stirred more than 70-90 DEG C to
Few 4h, filtering, cleans filter residue；Filter residue after cleaning obtains spare filter residue after drying process；The mixture A is by gangue
Waste material and waste and old cathode carbon block are compared according to quantity by matter, gangue waste material：Waste and old cathode carbon block≤5 form；In the lye, hydroxyl
Concentration be more than or equal to 3mol/L；
Step 2
Spare filter residue obtained by step 1 is placed in sintering furnace；1400-1700 is heated under inertia or reducing atmosphere
DEG C, be preferably 1450-1480 DEG C of insulation 3-10h, 800-1000 DEG C is then cooled to, and kept the temperature in oxygen-containing atmosphere, until zero
Valency carbon complete oxidation, then obtain silicon carbide powder after overpickling.
Industrially in application, taking gangue waste material, cathode carbon pieces to crush respectively；Cross 300 mesh sieves, be preferably 400 mesh
Sieve；In mass ratio, gangue waste material：Cathode carbon pieces=1:(0.5-2), be preferably 1:1-2 extracting screen underflows, are uniformly mixed；Obtain
Mixture A.
Industrially in application, in step 2, spare filter residue obtained by step 1 is placed in the containing in container of quartz material
And it is put into sintering furnace.
Industrially in application, in step 2,800-1000 DEG C is cooled to, and insulation 3-5h just can be real in oxygen-containing atmosphere
The complete oxidation of existing zeroth order carbon.At this time if extending soaking time, then can have a certain impact to the yield of product SiC.
A kind of Application way of gangue waste material of the present invention, the waste and old cathode carbon block are the waste and old cathode of aluminium electrolytic industry
Carbon block.
A kind of Application way of gangue waste material of the present invention, the gangue waste material SiO2More than or equal to 50wt%, Al2O3
Less than or equal to 30wt%.In the waste and old cathode carbon block, the content of carbon is more than or equal to 60wt%.As preferred；Described waste and old the moon
In the carbon block of pole, the content of carbon is more than or equal to 60wt%, less than or equal to 80wt%.
A kind of Application way of gangue waste material of the present invention, in step 1, in mass ratio, mixture A：Lye=1:5-
10, mixture A obtained by step 1 is placed in lye, 4-10h is stirred more than 70-90 DEG C, is filtered, cleans filter residue；After cleaning
Filter residue after drying process, obtain spare filter residue.
Preferably, a kind of Application way of gangue waste material of the present invention, in step 1, after filtering, with 70-90 DEG C of heat
Water washing filter residue, vacuum filtration, repeatedly, after washing liquid for pH value to 6.8-7.2, be then 100-300 in temperature
8-24h is dried under conditions of DEG C, obtains spare filter residue.In step 1, the filter residue after cleaning is in 100-300 DEG C of dry 8-24h.
100-300 DEG C of dry 8-24h is not only only capable of removing moisture content, moreover it is possible to which gangue waste material is activated.
A kind of Application way of gangue waste material of the present invention, in step 1, the speed of the stirring is 100r/min-
300r/min。
A kind of Application way of gangue waste material of the present invention, in the lye, concentration hydroxy is preferably 3-5mol/L.
Lye is at least one of potassium hydroxide solution, sodium hydroxide solution.Lye reusable edible.
A kind of Application way of gangue waste material of the present invention, in step 2, acid that pickling uses is hydrofluoric acid, concentration 4-
6mol/L。
A kind of Application way of gangue waste material of the present invention, the purity of gained silicon carbide powder are more than or equal to 93%.Through excellent
After changing process, the purity of gained silicon carbide powder is more than or equal to 98%.
A kind of Application way of gangue waste material of the present invention, the granularity of gained silicon carbide powder are less than or equal to 15 microns.Through
After optimize technique processing, the granularity of gained silicon carbide powder is mainly distributed as 400-800nm.
Beneficial effect：
The present invention has been attempted using gangue waste material and cathode carbon pieces as raw material first；Made by the collaboration of each conditional parameter
With, prepared micron level even Nano grade SiC.The present invention uses alkali leaching-hot wash method, to titanium dioxide in gangue
Silicon has certain activation, in addition, alkali soaks the porous carbon source after can also being activated, this is to obtain micron even nanoscale
Other high-quality silicon carbide provides necessary condition.Extraction temperature (especially aluminium electroloysis is strictly controlled waste and old cathode carbon block at the same time
Used in the process of cathode carbon pieces) this is primarily to provide the porous carbon source of suitable aperture and hole shape.It is preferred that when control 4-10 is small
Alkali leaching, the nanometer grade powder relatively narrow its object is to obtain particle diameter distribution.
The present invention has following clear superiority：
1st, without using high-purity powdered carbon and silicon dioxide powder, the production cost of silicon carbide products can be effectively reduced.
2nd, the method for the present invention synthesis material is given birth to using the dangerous solid waste-waste and old cathode carbon block and coal of aluminium electroloysis enterprise
Solid waste-gangue of enterprise is produced, the silicon carbide powder of higher degree can not only be synthesized, also handled the ring of Industrial Solid Waste
Border is polluted and problem of resource waste, carries out creating industrial value during harmless treatment, has great significance to environmental protection.
3rd, the method for the present invention prepare silicon carbide powder it is widely used, available for grinding materials and grinding tool, corrosion-and high-temp-resistant material,
Electronic apparatus etc., there is larger industrial applicability value.
Specific implementation method
In embodiment and comparative example, the component of gangue waste material used is:SiO2Content 61wt%, C content 23wt%, its
He includes Al by impurity2O3、MgO、Fe2O3；The component of waste and old cathode carbon block is：C content 75wt%, F content 20wt%, impurity master
To be SiO2And sodium silicate.
Embodiment 1
A kind of Application way of gangue waste material, comprises the following steps that：
1) waste and old cathode carbon block of gangue waste material and aluminium electrolytic industry is crushed respectively, grinding to -400 mesh, in temperature
To dry 24h under conditions of 300 DEG C, after its internal moisture all evaporation, gangue in mass ratio：Cathode carbon pieces=1:1 is equal
Even mixing, obtains mixed powder material；
2) the obtained mixed powder material of upper step is pressed into powder：Lye=1:Mixed powder is dispersed in dense by 10 mass ratio
Spend in the NaOH lye for 4mol/L, 10h, mixing speed 300r/min are stirred at a temperature of 90 DEG C；
3) by solidliquid mixture obtained above by filtering separation of solid and liquid, the mixed powder obtained after suction filtration is with 90 DEG C
Hot water washing, vacuum filtration, repeatedly, liquid reaches 7 for pH value after washing, mixed powder after being cleaned, in temperature
To dry 24h under conditions of 300 DEG C, treat that its internal moisture is all evaporated；
4) dried mixed powder addition silica crucible is obtained by above-mentioned, under the protective atmosphere of nitrogen, with 3 DEG C/min
Heating rate be warming up to 1600 DEG C, keep the temperature 3h, be then cooled to 1000 DEG C, keep the temperature 3h ashings in air atmosphere, then pass through
I.e. can obtain purity is higher than 98% silicon carbide powder after the hydrofluoric acid pickling of 6mol/L.The granularity of the silicon carbide powder is mainly divided
Cloth is 400-600nm.
Embodiment 2
A kind of Application way of gangue waste material, comprises the following steps that：
1) waste and old cathode carbon block of gangue waste material and aluminium electrolytic industry is crushed respectively, grinding sieves to obtain 300-400
Mesh powder, 12h is dried under conditions of being 150 DEG C in temperature, after its internal moisture all evaporation, gangue in mass ratio：It is cloudy
Pole carbon block=1:0.5 uniformly mixing, obtains mixed powder material；
2) the obtained mixed powder material of upper step is pressed into powder：Lye=1:Mixed powder is dispersed in dense by 5 mass ratio
Spend in the NaOH lye for 3mol/L, remove Al2O3Deng impurity, 5h, mixing speed 100r/ are stirred at a temperature of 70 DEG C
min；
3) by solidliquid mixture obtained above by filtering separation of solid and liquid, the mixed powder obtained after suction filtration is with 70 DEG C
Hot water washing, vacuum filtration, repeatedly, liquid reaches 7 for pH value after washing, mixed powder after being cleaned, in temperature
To dry 8h under conditions of 100 DEG C, treat that its internal moisture is all evaporated；
4) dried mixed powder addition silica crucible is obtained by above-mentioned, in the protective atmosphere of nitrogen, with 5 DEG C/min
Heating rate be warming up to 1400 DEG C, and keep the temperature 10h, be then cooled to 800 DEG C, 5h burn off carbon residues are kept the temperature in air atmosphere,
Silica is removed by the hydrofluoric acid of 4mol/L again, it is 97.5% silicon carbide powder to obtain purity.The silicon carbide powder
Granularity is mainly distributed as 400-600nm.
Embodiment 3
A kind of Application way of gangue waste material, comprises the following steps that：
1) waste and old cathode carbon block of gangue waste material and aluminium electrolytic industry is crushed respectively, grinding to -300 mesh, in temperature
To dry 8h under conditions of 100 DEG C, after its internal moisture all evaporation, gangue in mass ratio：Cathode carbon pieces=1:2.0
Even mixing, obtains mixed powder material；
2) the obtained mixed powder material of upper step is pressed into powder：Lye=1:Mixed powder is dispersed in dense by 8 mass ratio
Spend in the NaOH lye for 5mol/L, remove Al2O3Impurity, stirs 8h, mixing speed 200r/min at a temperature of 80 DEG C；
3) by solidliquid mixture obtained above by filtering separation of solid and liquid, the mixed powder obtained after suction filtration is with 80 DEG C
Hot water washing, vacuum filtration, repeatedly, liquid reaches 7 for pH value after washing, mixed powder after being cleaned, in temperature
To dry 12h under conditions of 200 DEG C, spare filter residue is obtained；
4) dried mixed powder addition silica crucible is obtained by above-mentioned, under the mixed atmosphere of hydrogen and nitrogen, with 4
DEG C/heating rate of min is warming up to 1550 DEG C, and keeps the temperature 6h, 850 DEG C are then cooled to, 5h ashings are kept the temperature in air atmosphere
Remaining powdered carbon is removed, is down to after room temperature and goes out remaining silica by the hydrofluoric acid of 6mol/L, obtain purity as 96% carbonization
Silicon powder.The granularity of the silicon carbide powder is mainly distributed as 500-800nm.
Comparative example 1
Other conditions are consistent with embodiment 1, and difference is to substitute waste and old cathode carbon block using 99% carbon dust；Its
The purity of products obtained therefrom is 98%, but the granularity of product is 20-85 microns.The finished product of the quality such as production, its cost are about implemented
1.2 times of example 1.
Comparative example 2
The uniform embodiment 1 of other conditions is consistent, and difference is to use purity to substitute bastard coal for 99% silica
Stone waste material, with 99% carbon dust substitute waste and old cathode carbon block；Not only alkali leaching is handled；The purity of its products obtained therefrom be more than 98%, but
The granularity of product is 100-150 microns.The finished product of the quality such as production, its cost are 2 times of embodiment 1.
Comparative example 3
The uniform embodiment 1 of other conditions is consistent, and difference is room temperature alkali soaks temperature in step 2；Products obtained therefrom grain
The D90 of footpath distribution is 180 microns, D50 is 95 microns, and D10 is 10 microns.And the purity of products obtained therefrom is 86%.
Comparative example 4
The uniform embodiment 1 of other conditions is consistent, difference in step 2 alkali concn be 1mol/L；Products obtained therefrom grain
The D90 of footpath distribution is 210 microns, D50 is 115 microns, and D10 is 18 microns.
Claims (9)
1. a kind of Application way of gangue waste material, it is characterised in that comprise the following steps：
Step 1
In mass ratio, mixture A：Lye=1:5-10, mixture A is placed in lye, is stirred at least more than 70-90 DEG C
4h, filtering, cleans filter residue；Filter residue after cleaning obtains spare filter residue after drying process；The mixture A is given up by gangue
Material and waste and old cathode carbon block are compared according to quantity by matter, gangue waste material：Waste and old cathode carbon block≤5 form；It is hydroxy in the lye
Concentration is more than or equal to 3mol/L；
Step 2
Spare filter residue obtained by step 1 is placed in sintering furnace；1400-1700 DEG C of guarantor is heated under inertia or reducing atmosphere
Warm 3-10h, is then cooled to 800-1000 DEG C, and is kept the temperature in oxygen-containing atmosphere, until zeroth order carbon complete oxidation, then through overpickling
Obtain silicon carbide powder afterwards.
A kind of 2. Application way of gangue waste material according to claim 1, it is characterised in that：The waste and old cathode carbon block
For the waste and old cathode carbon block of aluminium electrolytic industry.
A kind of 3. Application way of gangue waste material according to claim 1, it is characterised in that：The gangue waste material
SiO2More than or equal to 50wt%, Al2O3Less than or equal to 30wt%, in the waste and old cathode carbon block, the content of carbon is more than or equal to
60wt%, less than or equal to 80wt%.
A kind of 4. Application way of gangue waste material according to claim 1, it is characterised in that：Filter residue after cleaning exists
100-300 DEG C of dry 8-24h.
A kind of 5. Application way of gangue waste material according to claim 1, it is characterised in that：In step 1, by quality
Than mixture A：Lye=1:5-10, mixture A is placed in lye, and 4-10h is stirred more than 70-90 DEG C, is filtered, cleaning
Filter residue；Filter residue after cleaning obtains spare filter residue after drying process；In the lye, concentration hydroxy is 3-5mol/L；
The speed of the stirring is 100r/min-300r/min.
A kind of 6. Application way of gangue waste material according to claim 1, it is characterised in that：The lye is hydroxide
At least one of potassium solution, sodium hydroxide solution.
A kind of 7. Application way of gangue waste material according to claim 1, it is characterised in that：
In step 1, after filtering, filter residue is placed in 70-90 DEG C of hot water, after stirring 2-4h, vacuum filtration, repeatedly, directly
Liquid is pH value to 6.8-7.2 after to washing, dries 8-24h under conditions of being then 100-300 DEG C in temperature, obtains spare filter
Slag.
A kind of 8. Application way of gangue waste material according to claim 1, it is characterised in that：In step 3, pickling makes
Acid is hydrofluoric acid, concentration 4-6mol/L.
A kind of 9. Application way of gangue waste material according to claim 1, it is characterised in that：Gained silicon carbide powder
Purity is more than or equal to 93%；The granularity of gained silicon carbide powder is less than or equal to 15 microns.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711205954.6A CN107986281B (en) | 2017-11-27 | 2017-11-27 | Utilization method of coal gangue waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711205954.6A CN107986281B (en) | 2017-11-27 | 2017-11-27 | Utilization method of coal gangue waste |
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| CN107986281B CN107986281B (en) | 2020-05-19 |
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| CN201711205954.6A Active CN107986281B (en) | 2017-11-27 | 2017-11-27 | Utilization method of coal gangue waste |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502640A (en) * | 2011-10-28 | 2012-06-20 | 东北大学 | Method for synthetizing silicon carbide through microwave heating of pulverized fuel ash and aluminium electrolysis of waste cathode carbon blocks |
| CN104140121A (en) * | 2013-05-09 | 2014-11-12 | 中国科学院过程工程研究所 | Method for preparing sodium aluminate solution from coal-series kaolinite or coal gangue used as raw material |
-
2017
- 2017-11-27 CN CN201711205954.6A patent/CN107986281B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502640A (en) * | 2011-10-28 | 2012-06-20 | 东北大学 | Method for synthetizing silicon carbide through microwave heating of pulverized fuel ash and aluminium electrolysis of waste cathode carbon blocks |
| CN104140121A (en) * | 2013-05-09 | 2014-11-12 | 中国科学院过程工程研究所 | Method for preparing sodium aluminate solution from coal-series kaolinite or coal gangue used as raw material |
Non-Patent Citations (1)
| Title |
|---|
| JIE YUAN ET AL.: "Co-treatment of spent cathode carbon in caustic and acid leaching process under ultrasonic assisted for preparation of SiC", 《ULTRASONICS – SONOCHEMISTRY》 * |
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