CN106179769A - The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in a kind of flotation - Google Patents
The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in a kind of flotation Download PDFInfo
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- CN106179769A CN106179769A CN201610831404.4A CN201610831404A CN106179769A CN 106179769 A CN106179769 A CN 106179769A CN 201610831404 A CN201610831404 A CN 201610831404A CN 106179769 A CN106179769 A CN 106179769A
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- flotation
- copper
- refractory materials
- waste refractory
- copper metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/04—Frothers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—Depressants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
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- 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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of flotation and reclaim the method for metallic copper in copper metallurgy waste refractory materials.The invention discloses a kind of flotation and reclaim the method for metallic copper in copper metallurgy waste refractory materials, after copper metallurgy waste refractory materials crushing raw ore, after carrying out wet ball-milling；As inhibitor, described ore pulp is carried out FLOTATION SEPARATION as foaming agent, sodium hexameta phosphate, obtain flotation concentrate and flotation tailing as supplementary catching agent, xanthate using kerosene as collecting agent, terpineol.The present invention not only solves the problem that existing copper metallurgy waste refractory bricks is stored up, moreover it is possible to comprehensively utilizes waste refractory bricks resource, turn waste into wealth.
Description
Technical field
The invention belongs to copper metallurgy waste refractory materials and recycle field, be specifically related to a kind of flotation recovery copper metallurgy and discard resistance to
The method of metallic copper in fire material.
Background technology
Waste refractory materials is a kind of quantity process big, extremely difficult, industrial waste the most disagreeableness to environment.According to statistics,
Only China's year waste refractory materials is just more than 8,000,000 tons, and these are by the waste refractory materials as rubbish, except only a few can
To return outside production line recycling, the exemplary process mode of major part waste refractory materials is buried or demotes use exactly.Both accounted for
By valuable land resource, cause again the waste of available resources and potential environmental pollution.
At present, Refractories For Non-ferrous Metal Industry is based on basic refractory, and magnesian-chrome efractoy is the most still
It it is so main product.China is copper-lead zinc big producing country, and nonferrous smelting system produces substantial amounts of discarded magnesia fire-protecting wall every year.
Within 2014, China's magnesia refractories yield is 4,000,000 tons, produces discarded nearly 3,000,000 tons of magnesia fire-protecting wall.
In nonferrous heavy metal smelting, Ore used mostly is cupric, nickel, lead, zinc sulfides ore deposit, and in smelting, refractory brick runs into
Melt not only have oxide slag, metal bath, also sulfide melt.Smelting non-ferrous metal all uses highly basic gonosome now
System and oxidizing atmosphere, the fusion temperature of melt is more much lower than steel-making melt, and its mobility is fine, easily penetrates into fire-resistant
In material.Because erosion is serious, the life-span is long, replacement frequency is high to cause the refractory brick used, and has permeated big in waste refractory bricks
The valuable metal of amount, such as Cu, Pb, Ag, Bi, Ni, Sb etc., potential age deduction is huge.
The common method of existing recovery waste refractory bricks, for waste refractory bricks is carried out artificial separation, corrodes serious part
After crushing, enter respective metal smelting furnace, reclaim valuable metal therein.The part not weathered returns dispensing, by certain
Ratio makes an addition in refractory brick raw materials for production.Although the method can solve the problem that a part of refractory brick heap is abandoned, but in a large number
High-melting-point material adds the stability greatly destroying fusion process in melting system, thus is unfavorable for the recovery of non-ferrous metal.
On the other hand, China's chromium resource is poor, and chromium resource is strategic materials, is unfavorable for being used for fire-resistant by substantial amounts of chrome ore
Manufacture of materials, refractory material produces and depends on import chrome ore.Containing Cr2O3Refractory material has a lot of unique advantageous property,
Although trivalent chromium is nontoxic, but Cr2O3-containing refractories is at oxidizing atmosphere and strong base substance such as Na2The a large amount of existence condition of O, CaO
Under, trivalent chromium oxidation is Cr VI.Hexavalent chromium compound is soluble in water, serious environment pollution.Therefore, cleaning recycles discarded
Refractory material becomes a problem in the urgent need to address of current non-ferrous metal metallurgy industry.
Summary of the invention
The present situation stored up in a large number for waste refractory materials in prior art, it is an object of the invention to provide a kind of warp
Ji, efficiently, cleaning, copper recovery is high, it is thus achieved that flotation concentrate in the comprehensive utilization copper metallurgy waste refractory materials of high grade of copper
The method of metallic copper is reclaimed in flotation.
Technical scheme:
The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in a kind of flotation, by copper metallurgy waste refractory materials crushing raw ore
After, carry out wet ball-milling, obtain ore pulp；Using kerosene as supplementary catching agent, xanthate is as collecting agent, and terpineol is as foaming
Agent, sodium hexameta phosphate as inhibitor, carries out FLOTATION SEPARATION to described ore pulp, obtains flotation concentrate and flotation tailing.
After flotation concentrate is dried, returning for copper metallurgy, flotation tailing is used for regenerating refractory material after drying.
The present invention farther includes following preferred technical scheme:
Preferably scheme, described FLOTATION SEPARATION includes one roughing, scans for twice and primary cleaning.
Preferably scheme, in rougher process, kerosene is 100-400g/t relative to the addition of raw ore, and xanthate is relative to raw ore
Addition is 400-600g/t, and terpineol is 30-80g/t relative to the addition of raw ore.
Preferably scheme, during once purging selection, xanthate is 200-300g/t relative to the addition of raw ore, and terpineol is relative
The addition of raw ore is 30～100g/t.
Preferably scheme, during secondary is scanned, xanthate is 100-200g/t relative to the addition of raw ore.
Preferably scheme, during primary cleaning, sodium hexameta phosphate is 200-400g/t relative to the addition of raw ore.
Preferably scheme, described copper metallurgy waste refractory materials raw ore is metal attack waste refractory materials, and copper metallurgy is discarded resistance to
Fire material crushing raw ore is less than 3mm to particle diameter.
Preferably scheme, by wet ball-milling, the particle diameter of 70%～90% granule is less than 0.074mm.
Preferably scheme, in rougher process, is initially charged kerosene, adds xanthate, be eventually adding terpineol, flotation 4-
8min；
During once purging selection, it is initially charged xanthate, adds terpineol, flotation 4-8min；
During secondary is scanned, add xanthate, flotation 3-6min；
Preferably scheme, during primary cleaning, adds sodium hexameta phosphate, flotation 3-6min.
Preferably scheme, described copper metallurgy waste refractory materials is that magnesium chromium firebrick is discarded in copper metallurgy.
Preferably scheme, uses sulfiding reagent to carry out prevulcanization before FLOTATION SEPARATION, described sulfiding reagent is selected from Na2S or
One in NaHS etc..
By prevulcanization, copper oxide therein is converted into hydrophobic sulfide, then carries out flotation recovery, to oxygen therein
Change copper to reclaim and have a facilitation, and the copper grade in the response rate of copper and flotation concentrate can be improved further.
Four flotation tailings that FLOTATION SEPARATION process obtains return to be continuing with during FLOTATION SEPARATION next time.
After flotation concentrate is dried, return for copper metallurgy.
The ultimate principle of the present invention and advantage:
The present situation stored up in a large number for waste refractory materials in prior art, the present invention is by selecting kerosene as selectivity
Supplementary catching agent, by reunion flotation, has reached the purpose to the microfine copper efficient recovery in waste refractory materials.Additionally,
By xanthate, sodium hexameta phosphate and the coordinated of terpineol, it is possible not only to make copper be attached to foam surface and reclaims, also
Can effectively suppress stone-like pulse magnesium oxide, improve the copper grade of flotation concentrate.
In the whole processing procedure of the present invention, it is not necessary to additionally regulate pH, so it is possible not only to avoid substantial amounts of acid-alkali accommodation
A large amount of consumption of agent, are possible to prevent again waste refractory materials composition or structural damage.
In the flotation concentrate that the present invention obtains, copper grade is higher, can be directly as copper metallurgy raw material, the composition of flotation tailing
Essentially identical with refractory brick raw materials for production, it is possible to return refractory brick production system.
Flotation waste water can recycle after treatment, and agents useful for same is cheap pollution-free medicine, whole technical process
Zero-emission.The present invention is possible not only to solve the problem that existing copper metallurgy waste refractory materials is stored up, it is also possible to comprehensive utilization is discarded resistance to
Fire material, turns waste into wealth, walks sustainable development path for China's copper smelt industry and provide another reliable technical support.To working as
Modern non-ferrous metals industry changing rejected material to useful resource and harmlessness disposing provide reliable technical support and valuable application reference valency
Value.
In the present invention, copper recovery is up to 97.80%, it is thus achieved that be far superior to the effect of prior art.
Detailed description of the invention
Below in conjunction with instantiation, the present invention is further described, but the present invention is not limited to following embodiment.
A flotation in following one roughing correspondence embodiment, the secondary flotation in once purging selection correspondence embodiment, two
The secondary tertiary flotation scanned in corresponding embodiment, four flotation in primary cleaning correspondence embodiment.
Embodiment 1:
Using the Guangdong copper converter refractory brick that gives up is raw material, and the copper content of this refractory brick is 5.48%.This sample first warp
The sample crush-being milled to 86% is less than 0.074mm, is then poured into by levigate serosity and carries out float test in flotation cell；a、
Flotation: after the sample poured in flotation cell is sized mixing, is sufficiently stirred for, adds the kerosene of the 200g/t as supplementary catching agent
Rear stirring 8min, stirs 4min after adding penta xanthate of the 400g/t as collecting agent, is subsequently adding as foaming agent
Stir 2min, flotation 4min after the terpineol of 50g/t and obtain a flotation concentrate and a flotation tailing；B, secondary flotation:
Stir 4min after flotation tailing continues penta xanthate of interpolation 200g/t, add the Oleum Pini of the 30g/t as foaming agent
Stirring 2min, flotation 4min after alcohol and obtain secondary flotation concentrate and secondary flotation mine tailing, it is floating that secondary flotation concentrate will return next time
In flotation operation of choosing test；C, tertiary flotation: stir after continuing penta xanthate of interpolation 100g/t in secondary flotation mine tailing
Mixing 4min, flotation 3min and obtain tertiary flotation concentrate and flotation tailing, tertiary flotation concentrate will return the two of float test next time
In secondary flotation operation；D, four flotation: pouring in another flotation device selected through row by a flotation concentrate, first selected operation adds
Add the sodium hexameta phosphate of the 250g/t as inhibitor, after stirring 4min, flotation 3min, it is thus achieved that flotation concentrate and four flotation tails
Ore deposit, returns to four flotation tailings in a flotation operation of float test next time.After above-mentioned floatation process performs six times, often
Flotation concentrate that secondary test is obtained and the quality of flotation tailing and grade are basically unchanged, will stable after concentrate and tailings sampling
Analyze.
Flotation results shows: in flotation concentrate, copper grade is 24.70%, and the productivity of concentrate is 20.98%, and copper recovery is high
Reach 95.74%；In flotation tailing, copper content is only 0.29%, and this flotation tailing meets the composition of such magnesium chromium firebrick production to be wanted
Ask.
Embodiment 2:
Using the Hubei copper converter magnesium chromium firebrick that gives up is raw material, and the copper content of this refractory brick is 4.82%.This sample is first
Levigate serosity, less than 0.074mm, is then poured into and is carried out flotation examination in flotation cell by the first sample through crush-being milled to 82%
Test；A, a flotation: after the sample poured in flotation cell is sized mixing, is sufficiently stirred for, add the sulfur of the 300g/t as vulcanizing agent
Stir 8min after changing sodium, add as stirring 8min after the kerosene of the 200g/t of supplementary catching agent, be subsequently adding as collecting
Stir 4min after penta xanthate of the 400g/t of agent, be eventually adding as stirring 2min, flotation after the terpineol of the 60g/t of foaming agent
5min obtains a flotation concentrate and a flotation tailing；B, secondary flotation: continuously add as sulfur in a flotation tailing
Stir 8min after the sodium sulfide of the 150g/t of agent, then add stirring 4min after penta xanthate of 200g/t, be subsequently adding as rising
Stir 2min, flotation 5min after the terpineol of the 30g/t of infusion and obtain secondary flotation concentrate and secondary flotation mine tailing, secondary flotation
Concentrate is by the flotation operation returning float test next time；C, tertiary flotation: in secondary flotation mine tailing, continuously add work
For stirring 8min after the sodium sulfide of the 100g/t of vulcanizing agent, then stir 4min, flotation 4min after adding penta xanthate of 100g/t and obtain
To tertiary flotation concentrate and flotation tailing, tertiary flotation concentrate is by the secondary flotation operation returning float test next time；D, four
Secondary flotation: pouring in another flotation device selected through row by a flotation concentrate, first selected operation is added as inhibitor
The sodium hexameta phosphate of 200g/t, after stirring 3min, flotation 4min, it is thus achieved that flotation concentrate and four flotation tailings, by four flotation
Mine tailing returns in a flotation operation of float test next time.After above-mentioned floatation process performs seven times, test is obtained every time
Flotation concentrate and the quality of flotation tailing and grade be basically unchanged, will stable after concentrate and tailings sample analysis.
Flotation results shows: in flotation concentrate, copper grade is 26.47%, and the productivity of concentrate is 20.18%, and copper recovery is high
Reach 97.80%；In flotation tailing, copper content is only 0.15%, and flotation tailing meets the composition of such magnesium chromium firebrick production to be wanted
Ask.
Claims (10)
1. the method for metallic copper in copper metallurgy waste refractory materials is reclaimed in a flotation, it is characterised in that copper metallurgy is discarded fire proofed wood
After material crushing raw ore, carry out wet ball-milling, obtain ore pulp；Using kerosene as supplementary catching agent, xanthate is as collecting agent, terpineol
As foaming agent, sodium hexameta phosphate, as inhibitor, carries out FLOTATION SEPARATION to described ore pulp, obtains flotation concentrate and flotation tail
Ore deposit.
The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in flotation the most according to claim 1, it is characterised in that institute
The FLOTATION SEPARATION stated includes one roughing, scans for twice and primary cleaning.
The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in flotation the most according to claim 2, it is characterised in that thick
During choosing, kerosene is 100-400g/t relative to the addition of raw ore, and xanthate is 400-600g/t relative to the addition of raw ore, pine
Oleyl alcohol is 30-80g/t relative to the addition of raw ore.
4. reclaiming the method for metallic copper in copper metallurgy waste refractory materials according to the flotation described in Claims 2 or 3, its feature exists
In, during once purging selection, xanthate is 200-300g/t relative to the addition of raw ore, and terpineol is 30 relative to the addition of raw ore
～60g/t.
The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in flotation the most according to claim 4, it is characterised in that two
Secondary scan during, xanthate is 100-200g/t relative to the addition of raw ore.
6. reclaiming the method for copper metal in copper metallurgy waste refractory materials according to the flotation described in Claims 2 or 3, its feature exists
In, during primary cleaning, sodium hexameta phosphate is 200-400g/t relative to the addition of raw ore.
The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in flotation the most according to claim 1, it is characterised in that institute
Stating copper metallurgy waste refractory materials raw ore is metal attack waste refractory materials, and copper metallurgy waste refractory materials crushing raw ore is little to particle diameter
In 3mm.
The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in flotation the most according to claim 1 and 2, and its feature exists
In, by wet ball-milling, the particle diameter of 70%～90% granule is less than 0.074mm.
9. reclaiming the method for metallic copper in copper metallurgy waste refractory materials according to the flotation described in Claims 2 or 3, its feature exists
In, in rougher process, it is initially charged kerosene 100-400g/t and stirs 8min, add xanthate stirring 2-6min, be eventually adding Oleum Pini
Alcohol stirring 1-3min, flotation 4-8min；
During once purging selection, it is initially charged xanthate stirring 2-6min, adds terpineol stirring 1-3min, flotation 4-8min；
During secondary is scanned, add xanthate stirring 2-6min, flotation 3-6min；
During primary cleaning, add Polymeric sodium metaphosphate. stirring 2-4min, flotation 3-6min.
The method of metallic copper in copper metallurgy waste refractory materials is reclaimed in flotation the most according to claim 1, it is characterised in that
Described copper metallurgy waste refractory materials is that magnesium chromium firebrick is discarded in copper metallurgy；One roughing, scan for twice during, before FLOTATION SEPARATION
Using sulfiding reagent to carry out prevulcanization, described sulfiding reagent is selected from Na2One in S or NaHS.
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Cited By (7)
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| CN107350085A (en) * | 2017-06-21 | 2017-11-17 | 云南省地质矿产勘查开发局中心实验室（国土资源部昆明矿产资源监督检测中心） | Preparation and application of copper oxide ore flotation composite collecting agent |
| CN107716088A (en) * | 2017-09-29 | 2018-02-23 | 中南大学 | A kind of method for handling discarded magchrome refractory |
| CN109482335A (en) * | 2018-11-28 | 2019-03-19 | 中南大学 | A kind of method of copper and tin in FLOTATION SEPARATION discarded circuit board |
| CN110157918A (en) * | 2019-06-28 | 2019-08-23 | 金川集团股份有限公司 | A kind of method of the useless magnesite-chrome brick recycling high-grade rare precious metal of kaldo converter |
| CN113333436A (en) * | 2021-05-21 | 2021-09-03 | 中国矿业大学 | All-component comprehensive utilization method of coal gasification fine slag |
| CN113477404A (en) * | 2021-07-06 | 2021-10-08 | 中南大学 | Method for efficiently recovering copper-nickel metal from nickel smelting slag |
| CN114586645A (en) * | 2022-03-29 | 2022-06-07 | 昆明理工大学 | Method for preparing nutrient soil from coal gangue solid waste |
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Cited By (9)
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| CN107350085A (en) * | 2017-06-21 | 2017-11-17 | 云南省地质矿产勘查开发局中心实验室（国土资源部昆明矿产资源监督检测中心） | Preparation and application of copper oxide ore flotation composite collecting agent |
| CN107716088A (en) * | 2017-09-29 | 2018-02-23 | 中南大学 | A kind of method for handling discarded magchrome refractory |
| CN109482335A (en) * | 2018-11-28 | 2019-03-19 | 中南大学 | A kind of method of copper and tin in FLOTATION SEPARATION discarded circuit board |
| CN110157918A (en) * | 2019-06-28 | 2019-08-23 | 金川集团股份有限公司 | A kind of method of the useless magnesite-chrome brick recycling high-grade rare precious metal of kaldo converter |
| CN110157918B (en) * | 2019-06-28 | 2021-01-05 | 金川集团股份有限公司 | Method for recycling high-grade rare and precious metals from waste magnesia-chrome bricks of Kaldo converter |
| CN113333436A (en) * | 2021-05-21 | 2021-09-03 | 中国矿业大学 | All-component comprehensive utilization method of coal gasification fine slag |
| CN113477404A (en) * | 2021-07-06 | 2021-10-08 | 中南大学 | Method for efficiently recovering copper-nickel metal from nickel smelting slag |
| CN114586645A (en) * | 2022-03-29 | 2022-06-07 | 昆明理工大学 | Method for preparing nutrient soil from coal gangue solid waste |
| CN114586645B (en) * | 2022-03-29 | 2023-09-15 | 昆明理工大学 | Method for preparing nutrient soil from gangue solid waste |
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Application publication date: 20161207 |