CN101125311B - Vulcanizing-flotation combing method for treating zinc kiln slag - Google Patents
Vulcanizing-flotation combing method for treating zinc kiln slag Download PDFInfo
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- CN101125311B CN101125311B CN2007100662219A CN200710066221A CN101125311B CN 101125311 B CN101125311 B CN 101125311B CN 2007100662219 A CN2007100662219 A CN 2007100662219A CN 200710066221 A CN200710066221 A CN 200710066221A CN 101125311 B CN101125311 B CN 101125311B
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- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 52
- 239000011701 zinc Substances 0.000 title claims abstract description 52
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000005188 flotation Methods 0.000 title claims description 32
- 239000002893 slag Substances 0.000 title claims description 24
- 239000012141 concentrate Substances 0.000 claims abstract description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052742 iron Inorganic materials 0.000 claims abstract description 16
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 36
- WIKSRXFQIZQFEH-UHFFFAOYSA-N [Cu].[Pb] Chemical compound [Cu].[Pb] WIKSRXFQIZQFEH-UHFFFAOYSA-N 0.000 claims description 15
- 238000004073 vulcanization Methods 0.000 claims description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 150000001412 amines Chemical class 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- 229910001656 zinc mineral Inorganic materials 0.000 claims description 10
- 239000005864 Sulphur Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- 229910052745 lead Inorganic materials 0.000 claims description 5
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- 238000005987 sulfurization reaction Methods 0.000 claims description 5
- 238000001238 wet grinding Methods 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 239000012190 activator Substances 0.000 claims description 2
- 238000009837 dry grinding Methods 0.000 claims description 2
- 239000004088 foaming agent Substances 0.000 claims description 2
- 239000003112 inhibitor Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 abstract description 10
- 239000010949 copper Substances 0.000 abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 7
- 239000011707 mineral Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 239000011593 sulfur Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract 1
- 150000003568 thioethers Chemical class 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
The present invention relates to a method of sulphuration-floatation combining processing zinc kiln dreg. Making the material zinc kiln dreg grinded in a dry manner to the texture -0.074 mm, which covers 30 to 50 wt percent, and adding the simple substance sulfur of 3 to 5 wt percent, and microwave heating and sulphuration for 5 to 8 minutes under 250 DEG C to 500 DEG C, and then holding wet type grinding, and the pulp concentration is 50 to 60 percent, and when the texture is grinded to -0.074 covering 60 to 75wt percent, and then holding the floatation art. Complexly recovering copper and lead mixed concentrate, the zinc concentrate and the iron concentrate from the zinc kiln dreg. The invention adopts the manner of combining the low temperature sulphuration and floatation art, which changes the mineral surface activity; and the floatation property of the sulfide is good, and the adding amount of the sulfides is few, and the invention has small energy consumption with little environmental pollution.
Description
One, technical field
The present invention relates to a kind of method of vulcanizing-flotation Combined Treatment zinc kiln slag, a kind ofly specifically carry out vulcanizing treatment with microwave, adopt the valuable metal element in the mode separation of Zinc kiln slag of flotation then, obtain the method for copper-lead bulk concentrate, zinc concentrate and iron ore concentrate.Belong to choosing-smelting Combined Treatment technical field.
Two, technical background
The residue that zinc kiln slag is zine-smelting plant's zinc hydrometallurgy leached mud after rotary kiln evaporation is handled belongs to the secondary smelting slag, and it contains valuable metal elements such as a certain amount of iron and part zinc, copper, silver, has bigger recovery value.But because its thing phase composition is extremely complicated, cause the valuable metal element in the zinc kiln slag to be difficult to reclaim, cause the waste of resource.Known in the past zinc kiln slag treatment technology shows; Be to adopt more than 1200 ℃ temperature to carry out the processing of thermal process route mostly, in case add vulcanizing agent or chlorinating agent, the problem of inevitably bringing sulfide or chloride environmental pollution into; Zinc kiln slag is to belong to a kind of oxide ore, oxide ore directly carries out the known document of FLOTATION SEPARATION and (opens deep, Qiu Yueqin, Tang Yun etc. STUDY ON MINERAL TECHNOLOGY OF ZINC OXIDE. the journal .2000 of Guizhou University of Technology, 29 (6): 49～53) show that the lead-zinc thing has the characteristics of difficult choosing.
Three, summary of the invention
The present invention provides a kind of method of vulcanizing-flotation Combined Treatment zinc kiln slag, adopt broken mill, microwave vulcanization and floatation process, comprehensive copper-lead bulk concentrate, zinc concentrate and the iron ore concentrate of reclaiming from zinc kiln slag, the mode that the present invention adopts cryogenic vulcanization and floatation process to combine, reach and reduced energy consumption and the sulphide flotation performance is good, the vulcanizing agent addition is few, reduced environmental pollution and changed the purpose of mineral surfaces activity.
Fig. 1 is seen in patent technological process of the present invention, and the invention step is as follows:
1) the raw material zinc kiln slag is carried out dry milling to the account for 30～50wt% of granularity, add the elemental sulfur of 3-5wt%, fully behind the mixing, obtain sulphur matter mixture for-0.074mm;
2) sulphur matter mixture is carried out the heating using microwave sulfuration, vulcanization process condition is: microwave vulcanization 5-8min, microwave power are 400～850W, and curing temperature is 250～500 ℃;
3) product after the microwave vulcanization is carried out wet grinding, the ore pulp concentration expressed in percentage by weight is 50-60%, and granularity is milled to-and 0.074mm accounts for 60～75wt%;
4) mixture behind the wet grinding is carried out flotation, the flotation concrete steps are as follows: at first carry out the bulk flotation of copper-lead, add and adjust agent sodium metasilicate 90～110g/t, mix 2～8min, inhibitor carboxymethyl cellulose (CMC) 45～55g/t mixes 2～8min, collecting agent hydroximic acid 700～900g/t, mix 2～8min, foaming agent 2
#Oil 30～45g/t behind mixing 1～5min, roughly selects 5min, adds hydroximic acid 150～250g/t again, mixes 2～3min, adds 2
#Oil 30～45g/t mixes 2～3min, scans 4min, finishes the bulk flotation of copper-lead, obtains copper-lead bulk concentrate and mine tailing; In second step, mine tailing carries out the flotation of zinc mineral, adds activator vulcanized sodium 1300～1500g/t, mixes 2～3min, adds collecting agent mixed amine (RNH
2) 450～550g/t, mix 2～3min, roughly select 5min, add vulcanized sodium 400～500g/t again, mix 2～3min, add mixed amine 200～300g/t, mix 2～3min, scan 4min, finish the flotation of zinc mineral, obtain zinc concentrate and iron ore concentrate.
Compare advantage and good effect that the present invention has with known technology:
1) the microwave vulcanization zinc kiln slag is to carry out under cryogenic conditions, and temperature is 250～500 ℃, can reduce additive elemental sulfur (S) volatilization contaminated environment;
2) have the reducing atmosphere of microwave vulcanization zinc kiln slag: because zinc kiln slag contains a certain amount of reducing agent carbon, and carbon is preferential and system in the oxygen combination, stoped additive S and oxygen combination, further prevent elemental sulfur (S) contaminated environment;
3) additive sulfur (S) has improved the activity of zinc kiln slag mineral surfaces under the effect of microwave, makes that the more original oxide ore of mineral after the sulfuration is easy to FLOTATION SEPARATION.And (chemical formula is CuFeS to additive sulfur (S) than pyrite
2) 0.5 sulphur (S) is provided more;
4) adopted cryogenic vulcanization-flotation selecting smelting combination mode to handle zinc kiln slag, obtain copper-lead bulk concentrate, zinc concentrate and iron ore concentrate.Known technology was compared in the past, process reform of the present invention mineral surfaces activity and reduced energy consumption, have the good and energy-saving significance of flotation performance.
Four, description of drawings
Fig. 1 is the process chart of vulcanizing-flotation Combined Treatment zinc kiln slag.
Five, concrete embodiment
Example one
Raw material zinc kiln slag main chemical compositions weight percentage is TFe 31.36wt%, Zn 4.57wt%, Cu0.77wt%, Pb 0.48wt%, C 15wt%, ore grinding accounts for 30～50wt% to-0.074mm, the sulphur that adds 5wt% fully behind the mixing, carries out heating using microwave sulfuration 5min, heating using microwave power is 400～850W, and curing temperature is 300 ± 50 ℃; Product after the microwave vulcanization carries out ore grinding in wet ball mill, pulp density is 60%, and granularity is milled to-and 0.074mm accounts for 60～75wt%; The ore grinding afterproduct carries out flotation, adds sodium metasilicate 100g/t, mixes 5min, adds CMC50g/t, mixes 5min, adds hydroximic acid 800g/t, mixes 5min; Add 2
#Oil 36g/t mixes 3min and roughly selects 5min afterwards, adds hydroximic acid 200g/t again, mixes 2min, 2
#Oil 38g/t carries out scanning of copper-lead mixture after mixing 2min, obtains copper-lead bulk concentrate and mine tailing after scanning 4min; Flotation tailing is carried out the flotation of zinc mineral, add vulcanized sodium 1400g/t, mix 3min, add mixed amine 500g/t, mix 2min and roughly select 5min afterwards, add vulcanized sodium 450g/t again, mix 2min, add mixed amine 250g/t, mix 2min and carry out scanning of zinc mineral, scan 4min and obtain zinc concentrate and iron ore concentrate afterwards.Copper, plumbous bulk concentrate cupric 1.84wt%, plumbous 1.29wt%, copper, the plumbous rate of recovery are respectively 30.15wt%, 33.9wt%; Zinc concentrate contains zinc 8.67wt%, and the rate of recovery of zinc is 60.19wt%; The TFe content of iron ore concentrate is 60.3wt%, and the rate of recovery of iron is 88.5%.
Example two
Raw material zinc kiln slag main chemical compositions weight percentage is TFe 32.82wt%, Zn 5.29wt%, Cu 0.91wt%, Pb 0.6wt%, C 18wt%, ore grinding accounts for 30～50wt% to-0.074mm, the sulphur that adds 4wt% behind the mixing, carries out heating using microwave sulfuration 8min, heating using microwave power is 400～850W, and curing temperature is 450 ℃ ± 50 ℃; Product after the microwave vulcanization carries out ore grinding in wet ball mill, pulp density is 50%, and granularity is milled to-and 0.074mm accounts for 60～75wt%; The ore grinding afterproduct carries out flotation, adds sodium metasilicate 110g/t, mixes 8min, adds CMC55g/t, mixes 8min, adds hydroximic acid 900g/t, mixes 8min, adds 2
#Oil 45g/t mixes 5min, adds hydroximic acid 250g/t again, 2 after roughly selecting 5min
#Oil 45g/t mixes 2min, carries out scanning of copper-lead mixed mineral, obtains copper-lead bulk concentrate and mine tailing after scanning 4min; Mine tailing carries out the flotation of zinc mineral, adds vulcanized sodium 1500g/t, mixes 3min, mixed amine 550g/t, mix 3min, add vulcanized sodium 500g/t again after roughly selecting 5min, mix 2min, add mixed amine 300g/t, mix 3min, scan behind the 4min zinc concentrate and iron ore concentrate.Copper-lead bulk concentrate cupric 1.94wt%, leaded 1.54wt%, copper, the plumbous rate of recovery are respectively 28.78wt%, 30.65wt%; Zinc concentrate contains zinc 10.52wt%, and the rate of recovery of zinc is 70.2wt%, and the TFe content of iron ore concentrate is 61.4wt%, and the rate of recovery of iron is 90.5%.
Example three
Raw material zinc kiln slag main chemical compositions weight percentage is TFe 33.55wt%, Zn 6.46wt%, Cu1.1wt%, Pb0.82wt%, C 22wt%, carry out ore grinding and account for 30～50wt% to-0.074mm, the sulphur that adds 5wt% fully behind the mixing, carries out microwave vulcanization 5min, heating using microwave power is 400～850W, and curing temperature is 400 ℃ ± 50 ℃; Product after the microwave vulcanization carries out ore grinding in wet ball mill, pulp density is 60%, and granularity is milled to-and 0.074mm accounts for 60～75wt% ore grinding afterproduct and carries out flotation, adds sodium metasilicate 90g/t, mix 2min, add CMC45g/t, mix 2min, add hydroximic acid 700g/t, mix 3min, add 2
#Oil 30g/t mixes the bulk flotation that 1.5min carries out copper, lead afterwards, roughly selects 5min, adds hydroximic acid 150g/t again, mixes 2min; Add 2
#Oil 30g/t carries out scanning of copper-lead mixture after mixing 2min, obtains copper-lead bulk concentrate and mine tailing after scanning 4min; Mine tailing carries out the flotation of zinc mineral, add vulcanized sodium 1300g/t, mix 2min, add mixed amine 450g/t, mix the flotation that 2min carries out zinc mineral afterwards, add vulcanized sodium 400g/t again after roughly selecting 5min, mix 2min, add mixed amine 200g/t, carry out scanning of zinc mineral behind the mixing 2min, scan 4min, obtain zinc concentrate and iron ore concentrate.Copper-lead bulk concentrate cupric 2.14wt%, plumbous 1.7wt%, then copper, the plumbous rate of recovery are respectively 16.31wt%, 19.65wt%; Zinc concentrate contains zinc 7.92wt%, and the rate of recovery of zinc is 58.5wt%, and the TFe content of iron ore concentrate is 57.3wt%, and the rate of recovery of iron is 97.5%.
Claims (1)
- One kind the sulfuration one flotation combined processing zinc kiln slag method, it is characterized in that: it is finished according to the following steps,1) the raw material zinc kiln slag is carried out dry milling to the account for 30～50wt% of granularity for-0.074mm, add the elemental sulfur mixing of 3-5wt% after, obtain sulphur matter mixture; Described raw material zinc kiln slag main chemical compositions weight percentage is TFe 31.36%, and Zn 4.57%, and Cu 0.77%, Pb 0.48%, C 15% or TFe32.82%, Zn 5.29%, and Cu 0.91%, Pb 0.6%, C 18% or TFe 33.55%, Zn 6.46%, Cu1.1%, Pb 0.82%, and C 22%;2) sulphur matter mixture is carried out the heating using microwave vulcanizing treatment, the control microwave power is 400～850W, and curing temperature is 250～500 ℃, cure time 5-8min;3) product after the microwave vulcanization is carried out wet grinding, the ore pulp concentration expressed in percentage by weight is 60%, granularity is milled to-0.074mm account for 60～75wt%;4) mixture behind the wet grinding is carried out flotation, at first carry out the bulk flotation of copper-lead, add and adjust agent sodium metasilicate 90～110g/t, mix 2～8min, inhibitor carboxymethyl cellulose (CMC) 45～55g/t mixes 2～8min, collecting agent hydroximic acid 700～900g/t, mix 2～8min, foaming agent 2 #Oil 30～45g/t behind mixing 1～5min, roughly selects 5min, adds hydroximic acid 150～250g/t again, mixes 2～3min, adds 2 #Oil 30～45g/t mixes 2～3min, scans 4min, finishes the bulk flotation of copper-lead, obtains copper-lead bulk concentrate and mine tailing; In second step, mine tailing carries out the flotation of zinc mineral, adds activator vulcanized sodium 1300～1500g/t, mixes 2～3min, adds collecting agent mixed amine (RNH 2) 450～550g/t, mix 2～3min, roughly select 5min, add vulcanized sodium 400～500g/t again, mix 2～3min, add mixed amine 200～300g/t, mix 2～3min, scan 4min, finish the flotation of zinc mineral, obtain zinc concentrate and iron ore concentrate.
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Families Citing this family (10)
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| CN101545038B (en) * | 2009-05-06 | 2010-08-11 | 个旧玉龙再生资源经营有限公司 | Method for producing iron ore concentrate by using poor-tin sulfide ore tailings |
| CN102225369A (en) * | 2011-05-18 | 2011-10-26 | 河南省岩石矿物测试中心 | Beneficiation method for separating copper-lead-zinc multi-metal complex ore embedded with fine particles |
| CN102357425B (en) * | 2011-10-25 | 2013-06-05 | 湖南水口山有色金属集团有限公司 | Method for recovering valuable elements from zinc kiln slag tailings |
| CN102680310A (en) * | 2012-03-20 | 2012-09-19 | 中国人民解放军第二军医大学 | Microwave assisted plasma sample pre-processing method and application in plasma metabonomics analysis |
| CN104741243B (en) * | 2015-04-24 | 2017-03-01 | 中南大学 | Non-ferrous metal ore flotation collector with mercapto-hydroxamic acid group structure and preparation method and application thereof |
| CN104888969B (en) * | 2015-04-24 | 2017-04-19 | 中南大学 | Nonferrous metal ore flotation collecting agent with mercapto-oximido structure and application thereof |
| CN105543494B (en) * | 2016-01-18 | 2017-07-14 | 中南大学 | A kind of method that smelting choosing joint substep reclaims valuable metal in slag |
| CN106179762B (en) * | 2016-07-15 | 2018-07-24 | 昆明理工大学 | A kind of beneficiation method of low-grade shale zinc oxide ore |
| CN107899755B (en) * | 2017-11-13 | 2020-06-05 | 云南迪庆有色金属有限公司 | Synergist for flotation of refractory copper oxide ore |
| CN109806980B (en) * | 2019-01-28 | 2020-12-01 | 西安建筑科技大学 | Method for controlling malachite vulcanization products and application thereof |
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