CN100552059C - Method for directly leaching indium from indium ore - Google Patents
Method for directly leaching indium from indium ore Download PDFInfo
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- CN100552059C CN100552059C CNB2007102023582A CN200710202358A CN100552059C CN 100552059 C CN100552059 C CN 100552059C CN B2007102023582 A CNB2007102023582 A CN B2007102023582A CN 200710202358 A CN200710202358 A CN 200710202358A CN 100552059 C CN100552059 C CN 100552059C
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- indium
- reactor
- extraction
- sulfuric acid
- leaching
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Links
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 123
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000002386 leaching Methods 0.000 title claims abstract description 29
- 239000012141 concentrate Substances 0.000 claims abstract description 41
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000926 separation method Methods 0.000 claims abstract description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 60
- 238000000605 extraction Methods 0.000 claims description 56
- 238000006243 chemical reaction Methods 0.000 claims description 34
- 239000007787 solid Substances 0.000 claims description 22
- 238000005516 engineering process Methods 0.000 claims description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 10
- 150000002472 indium compounds Chemical class 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 11
- 239000000284 extract Substances 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 description 23
- 229910052500 inorganic mineral Inorganic materials 0.000 description 21
- 239000011707 mineral Substances 0.000 description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical class [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 12
- 229910052725 zinc Inorganic materials 0.000 description 10
- 239000011701 zinc Substances 0.000 description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 9
- 229910000337 indium(III) sulfate Inorganic materials 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000005864 Sulphur Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 6
- 239000003350 kerosene Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 238000004512 die casting Methods 0.000 description 5
- 238000006062 fragmentation reaction Methods 0.000 description 5
- 229910001449 indium ion Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000012074 organic phase Substances 0.000 description 5
- 229910052718 tin Inorganic materials 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000003500 flue dust Substances 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 229910052569 sulfide mineral Inorganic materials 0.000 description 2
- 229910020994 Sn-Zn Inorganic materials 0.000 description 1
- 229910009069 Sn—Zn Inorganic materials 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- XUHJGXBPMAPKDW-UHFFFAOYSA-N [As].[Fe]=S Chemical compound [As].[Fe]=S XUHJGXBPMAPKDW-UHFFFAOYSA-N 0.000 description 1
- YWIWTWXAADSUID-UHFFFAOYSA-N [Fe].[In].[S] Chemical compound [Fe].[In].[S] YWIWTWXAADSUID-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- PLZFHNWCKKPCMI-UHFFFAOYSA-N cadmium copper Chemical compound [Cu].[Cd] PLZFHNWCKKPCMI-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 229910001779 copper mineral Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 150000002471 indium Chemical class 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910001608 iron mineral Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 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
- 238000007670 refining Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000019086 sulfide ion homeostasis Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for directly leaching indium from indium ore, which relates to the technical field of wet metallurgy. The method solves the problem that the prior art can not extract indium from indium sulfide concentrate by direct leaching and has the advantages of simple process, high indium metal recovery rate, easy indium separation and low reagent consumption compared with the prior art.
Description
Technical field
The present invention relates to technical field of wet metallurgy, particularly a kind of processing method of indium being separated indium from indium sulfide concentrate.
Background technology
The alleged indium sulfide concentrate of the present invention is meant and contains indium 1500～4500 gram/tons, iron content 18～35%, and sulfur-bearing 26～38% contains the mineral of other valuable metal element simultaneously.
Indium is considerably less at the content of occurring in nature, and most indium associations are in sulphide oress such as lead glance, zink sulphide, chalcopyrite, pyrite, some association is in tin ore, contain indium mineral deposit polymetallic deposit often, in ore dressing process, the scattered metals indium enrichment in the polymetallic ore can be become indium sulfide concentrate.The mineral of indium have sulphur indium iron ore (FeIn in this indium sulfide concentrate
2S
4), roquesite (CuInS
2), sulphur indium Cu-Sn-Zn ore deposit { (Cu, Zn, Fe) 3 (InSn) S
4And dzhalindite (In (OH)
3) etc.Thereby, this indium sulfide concentrate essence is a kind of complex multi-metal sulphide ore thing that contains multiple metallic element, and its feature is the iron level height, sulphur content height, indium content height, generally containing multiple metallic elements such as copper, zinc, lead, tin, antimony, arsenic, is to extract the important mineral wealth of indium metal.
The material of indium sulfide concentrate is formed complicated, main metallic element indium, iron, it is various that variation of valence is deposited in the occurrence status of sulphur and tax, disperse trickle, in same ore body, usually there are multiple indium mineral and iron mineral, the indium overwhelming majority in the concentrate exists with the form of sulfide, simultaneously with the sulfide mineral of iron, the sulfide mineral of copper, there is relevant complex relationship in the sulfide of arsenic etc., in addition, also can form indium hydroxyl stone etc., the pozzuolite copper mineral, mineral such as arsenic iron sulfur mineral, thereby, indium sulfide concentrate is to compose with multiple valence state sulfide to deposit, the association of mixing mutually, and disseminated grain size is thinner, there is the argillization state, the granularity thickness is extremely inhomogeneous, and microfine is quartzy and clay content is very high, and the existence of indium presents complicacy, variation, characteristics such as changeableization.Thereby the separation of these class mineral and enrichment are quite difficult and complicated.Therefore, most indium is to reclaim from the byproduct of productions such as zinc, lead, tin.As in zinc pyrometallurgical smelting process, from the dust of nodulizing coke oven and lead the crude zinc rectification and purification process and hard zinc, extract indium; When zinc hydrometallurgy, from the volatile matter (flue dust) of waelz process or fuming process and copper cadmium filter residue, extract indium; Smelt in the production at lead, product of refined lead (containing copper dross slag, oxide compound) and the processing back different products that obtain (for example flue dust of cupric dross reverberatory furnace melting and slag) thereof extract indium; In the refining of the calcining retailoring of concentrate or concentrate preroasting and thick tin, be to extract indium from flue dust and exhausted ionogen.
At present, the smelting of indium mainly is to reclaim from the byproduct that lead, zinc, tin are smelted, the indium of western countries 90% is to reclaim from the byproduct of plumbous zinc production, contains recovery method that the indium intermediate material extracts indium and mainly contains the oxidative slagging method and reclaim indium, electrolysis concentration method and reclaim indium, ion exchange method and reclaim that indium, sulfurization roasting method reclaim indium, hot acid leaches a siderotil method and reclaims indium from above-mentioned.In aforesaid method, for the indium metal in the indium sulfide material complicated and changeable being separated and extracting, on the principles of chemistry, must make the sulfide that can not be dissolved in the indium in acid, alkali and the water, be converted into soluble oxide compound or salt.At present, also there are not special technology and technology directly indium sulfide concentrate to be handled separately.Reason is that indium compound can not dissolve with the method that simple acidleach goes out in the indium sulfide concentrate, and adopt the technology of roasting and technology will make indium dispersion and the long complexity of flow process strategic point, indium mineral behavior complexity in the indium sulfide concentrate still more, this has just fundamentally limited employing routine techniques and technology this kind indium concentrate has been reclaimed separately and utilized, thereby, the deficiency that aforesaid method exists is the technical matters complexity, metal recovery rate is low, valuable metal disperses, reagent consumption is big, be difficult to overcome the complicacy of mineral, make the extraction and the separation difficulty of indium in the mineral, big for environment pollution.
Summary of the invention
The method of direct leaching indium in the indium provided by the present invention ore deposit is to solve the problem that still can't directly leach high indium vulcanised ore concentrate, and realizes that technical matters is simple, indium metal rate of recovery height, and indium is easily separated, the purpose that reagent consumption is little.
In order to address the above problem, the method for direct leaching indium comprises the following steps: in this indium ore deposit
(1), dissolving indium compound: will pulverize, levigate indium sulfide concentrate joins in the reactor with sulfuric acid concentration is that the aqueous sulfuric acid of 100～300 grams per liters mixes, aerating oxygen and to control the still internal pressure be 1.0MPa～6.0MPa in reactor, 100 ℃～300 ℃ of heating and control still interior reaction temperatures, allow sulfuric acid, oxygen and indium sulfide concentrate in reaction kettle for reaction, indium is leached in leach liquor with the form of easily dissolving compound;
(2), the material with reactor carries out liquid-solid separation, the acquisition leach liquor;
(3), adopt extracting-back extraction-replacing process technology extraction separation to obtain indium to above-mentioned leach liquor.
In the step of above-mentioned acidleach dissolving indium compound, processing condition generally can be elected as in the reactor: the pressure in the reactor is 1.2MPa ~ 1.3MPa, and the temperature in the reactor is 201 ℃～300 ℃.
It is P that above-mentioned extraction process can adopt extraction agent
204, and be solvent cut P with kerosene
204Concentration is 30% as extraction system, and carries out 4 grades of indium sulfates in the extraction leach liquor at normal temperatures; It is that concentration is the normal aqueous hydrochloric acid of 6-7 that above-mentioned stripping process can adopt the back extraction medium, and carries out 4 grades of reextraction, contains indium at 50～100g/L in the control anti-stripping agent; Above-mentioned replacing process can adopt pure aluminum plate and anti-stripping agent reaction to displace indium.
Under the condition of the step of above-mentioned acidleach dissolving indium compound, destroy the sulfide structure with oxygen and sulfuric acid, allow sulfide generation oxidation and solubilizing reaction, generate indium sulfate and be dissolved in the acid, obtain indium sulfate solution, the oxidized generting element sulphur of sulphur, the sulfide partial oxidation of iron generates ferric sulfate and enters solution, part generates ironic hydroxide or sulfuric acid siderotil precipitation enters leached mud, and other gangue composition does not then change and is retained in the leached mud.The chemical reaction of its generation is:
FeIn
2S
4+2H
2SO
4+1/2O
2→Fe
2(SO
4)
3+2H
2O+In
2(SO
4)
3+S (1)
CuInS
2+2H
2SO
4+1/2O
2→CuSO
4+2H
2O+In
2(SO
4)
3+S (2)
(Cu，Zn，Fe)
3(InSn)S
4+2H
2SO
4+1/2O
2→
CuSO
4+Fe
2(SO
4)
3+CuSO
4+2H
2O+In
2(SO
4)
3+S (3)
Fe
2(SO
4)
3+3H
2O→Fe(HO)
3↓+3H
2SO
4 (4)
Fe
2(SO
4)
3+3H
2O→Fe(HO)
3↓+3H
2SO
4 (5)
Owing to adopted technique scheme, the present invention compared with prior art has following beneficial effect:
1, solved the directly difficult problem of leaching extraction indium from indium sulfide concentrate.Since acidleach go out with oxidising process be under pressurized state, the oxidising process temperature is brought up to 100～300 ℃, water is as liquid medium, under the vitriolic effect, elements such as indium in the complicated mineral composition in the indium sulfide concentrate are carried out oxidation and chemical reaction, generate easily molten compound, complicated technology and method in the indium removal process become adding depress in the direct oxidation leaching process, make complicated mineral composition change the process of easily dissolving compound into, the smelting metallization processes is simplified, flow process is short, realizes indium sulfide concentrate, complicated indium ore deposit is oxidized to the process of the indium compound of Yi Rong.
In the pressurization direct oxidation acidleach process, because oxygen is under pressurized conditions, press (1) (2) (3) (4) the formula generation oxidizing reaction in the such scheme, and the complicated indium mineral composition in the indium sulfide concentrate is converted into indium sulfate by (1) (2) and (3) formula, complicated indium mineral oxidation conversion is for easily dissolving compound, after maturation process such as extraction, back extraction, separation by displacement are handled, the just qualified thick indium of output; And the oxidized generting element sulphur of the sulphur in the indium sulfide concentrate enters leached mud, and the sulfide of iron partly generates ferric sulfate and enters solution, and another part generates ironic hydroxide or sulfuric acid siderotil precipitation enters leached mud.Therefore, it is a kind of clearer production technology of intensified transformation that indium sulfide concentrate pressurization direct oxidation acidleach transforms, and its main process is not subjected to the variation of mineral composition and restricts.
2, because saved operation such as roasting, thereby this technical matters is simple.
3, the indium metal leaching yield is 88～96%, and the indium metal leaching yield is 55～60% in the common process, thereby this technology metal recovery rate height.
4, owing to adopted the pressure leaching, indium mineral in the mineral are participated in chemical reaction directly, and in the routine techniques technology owing to adopt sinter process, the more stable compound of the oxidized generation of indium mineral in the mineral, thereby the mineral of this technology indium in aqueous sulfuric acid are easily separated than the indium compound in the common process.
5, in the common process owing to adopt roasting to make sulfide be transformed into oxide compound, the required sulfuric acid amount of sulfuric acid dissolution oxide compound wants many than the required sulfuric acid amount of sulfuric acid dissolution sulfide, sulfide will partly generate vitriol during sulfuric acid dissolution sulfide, thereby this technology sulphate reagent consumption is little.
Embodiment
Example one:
To direct leaching indium in 2.5 tons of indium sulfide concentrates that contain indium 1500 gram/tons, step is as follows:
1, with 2.5 tons moisture 8%, contain indium 1500 gram/ton indium sulfide concentrate fragmentations, add water for ball milling, be milled down to ore pulp and cross 200 mesh sieves and reach more than 85%.
2, according to above-mentioned grind the weight and the water content of ore pulp, the sulfuric acid and the water that add calculated amount, making the sulfuric acid concentration in the aqueous sulfuric acid is 150 grams per liters, solvent and solute weight ratio is at 4: 1, their added in 15 cubic metres the pressure reaction still, with steam heating and with flow aerating oxygen in reactor of 1.4 kg/minute, the control reactor temperature is at 101 ℃ ± 1 ℃, keep still internal pressure 1.0MPa, allow indium sulfide concentrate reaction kettle for reaction leaching 30 minutes, detecting the indium leaching yield is 65%.
3, adopt plate-and-frame filter press, the leach liquor of aforesaid reaction vessel is carried out liquid-solid separation, the solid after liquid-solid separation separates is a leached mud, and the liquid after liquid-solid separation separates is leach liquor.
4, adopt extracting-back extraction-replacing process technology extraction separation to obtain indium to above-mentioned leach liquor.Adopt P
204Be extraction agent, with 200
#Kerosene is under the situation of thinner, is mixed with P
204Concentration is 30% extraction system, at normal temperatures, adopts 4 grades of indium sulfates in the extraction process extraction leach liquor; Employing equivalent concentration is that the aqueous hydrochloric acid of 6-7N is the back extraction medium, to adopting P
204Strip for the organic phase that is rich in indium sulfate of extraction agent, reextraction progression is 4 grades, contains indium at 50～100g/L in the control anti-stripping agent; The horizontal counter-current extraction groove that extraction tank adopts full PVC to make; Adopt the indium ion in the pure aluminum plate displacement anti-stripping agent, obtain the sponge indium, die casting melted ingot then obtains containing the thick indium of indium 98.5%.
Result: 2.188 kilograms of thick indiums that obtain to contain indium 98.5%.
Example two:
To direct leaching indium in 2.5 tons of indium sulfide concentrates that contain indium 4500 gram/tons, step is as follows:
1, moisture 8% with 2.5 tons, contain indium 4500 gram/ton indium sulfide concentrate fragmentations, add water for ball milling, be milled down to ore pulp and cross 200 mesh sieves and reach more than 85%.
2, according to above-mentioned grind the weight and the water content of ore pulp, the sulfuric acid and the water that add calculated amount, making the sulfuric acid concentration in the aqueous sulfuric acid is 200 grams per liters, solvent and solute weight ratio is at 5: 1, their added in 15 cubic metres the pressure reaction still, with steam heating and with flow aerating oxygen in reactor of 2.5 kg/minute, the control reactor temperature is at 300 ℃ ± 1 ℃, keep still internal pressure 6.0MPa, allow indium sulfide concentrate reaction kettle for reaction leaching 60 minutes, detecting the indium leaching yield is 99%.
3, adopt plate-and-frame filter press, the leach liquor of aforesaid reaction vessel is carried out liquid-solid separation, the solid after liquid-solid separation separates is a leached mud, and the liquid after liquid-solid separation separates is leach liquor.
4, adopt extracting-back extraction-replacing process technology extraction separation to obtain indium to above-mentioned leach liquor and adopt P
204Be extraction agent, with 200
#Kerosene is under the situation of thinner, is mixed with P
204Concentration is 30% extraction system, at normal temperatures, adopts 4 grades of indium sulfates in the extraction process extraction leach liquor; Employing equivalent concentration is that the aqueous hydrochloric acid of 6-7N is the back extraction medium, to adopting P
204Strip for the organic phase that is rich in indium sulfate of extraction agent, reextraction progression is 4 grades, contains indium at 50～100g/L in the control anti-stripping agent; The horizontal counter-current extraction groove that extraction tank adopts full PVC to make; Adopt the indium ion in the pure aluminum plate displacement anti-stripping agent, obtain the sponge indium, die casting melted ingot then obtains containing the thick indium of indium 98.5%.
Result: 10.125 kilograms of thick indiums that obtain to contain indium 98.5%.
Example three:
To direct leaching indium in 2.5 tons of indium sulfide concentrates that contain indium 2500 gram/tons, step is as follows:
1, moisture 8% with 2.5 tons, contain indium 2500 gram/ton indium sulfide concentrate fragmentations, add water for ball milling, be milled down to ore pulp and cross 200 mesh sieves and reach more than 85%.
2, according to above-mentioned grind the weight and the water content of ore pulp, the sulfuric acid and the water that add calculated amount, making the sulfuric acid concentration in the aqueous sulfuric acid is 180 grams per liters, solvent and solute weight ratio is at 6: 1, their added in 15 cubic metres the pressure reaction still, with steam heating and with flow aerating oxygen in reactor of 3.6 kg/minute, the control reactor temperature is at 200 ℃ ± 1 ℃, keep still internal pressure 3.0MPa, allow indium sulfide concentrate reaction kettle for reaction leaching 120 minutes, detecting the indium leaching yield is 97%.
3, adopt plate-and-frame filter press, the leach liquor of aforesaid reaction vessel is carried out liquid-solid separation, the solid after liquid-solid separation separates is a leached mud, and the liquid after liquid-solid separation separates is leach liquor.
4, adopt extracting-back extraction-replacing process technology extraction separation to obtain indium to above-mentioned leach liquor and adopt P
204Be extraction agent, with 200
#Kerosene is under the situation of thinner, is mixed with P
204Concentration is 30% extraction system, at normal temperatures, adopts 4 grades of indium sulfates in the extraction process extraction leach liquor; Employing equivalent concentration is that the aqueous hydrochloric acid of 6-7N is the back extraction medium, to adopting P
204Strip for the organic phase that is rich in indium sulfate of extraction agent, reextraction progression is 4 grades, contains indium at 50～100g/L in the control anti-stripping agent; The horizontal counter-current extraction groove that extraction tank adopts full PVC to make; Adopt the indium ion in the pure aluminum plate displacement anti-stripping agent, obtain the sponge indium, die casting melted ingot then obtains containing the thick indium of indium 98.5%.
Result: 5.625 kilograms of thick indiums that obtain to contain indium 98.5%.
Example four:
To direct leaching indium in 2.5 tons of indium sulfide concentrates that contain indium 3500 gram/tons, step is as follows:
1, moisture 8% with 2.5 tons, contain indium 3500 gram/ton indium sulfide concentrate fragmentations, add water for ball milling, be milled down to ore pulp and cross 200 mesh sieves and reach more than 85%.
2, according to above-mentioned grind the weight and the water content of ore pulp, the sulfuric acid and the water that add calculated amount, making the sulfuric acid concentration in the aqueous sulfuric acid is 170 grams per liters, solvent and solute weight ratio is at 4.5: 1, their added in 15 cubic metres the pressure reaction still, with steam heating and with flow aerating oxygen in reactor of 2.0 kg/minute, the control reactor temperature is at 180 ℃ ± 1 ℃, keep still internal pressure 1.6MPa, allow indium sulfide concentrate reaction kettle for reaction leaching 180 minutes, detecting the indium leaching yield is 95%.
3, adopt plate-and-frame filter press, the leach liquor of aforesaid reaction vessel is carried out liquid-solid separation, the solid after liquid-solid separation separates is a leached mud, and the liquid after liquid-solid separation separates is leach liquor.
4, adopt extracting-back extraction-replacing process technology extraction separation to obtain indium to above-mentioned leach liquor and adopt P
204Be extraction agent, with 200
#Kerosene is under the situation of thinner, is mixed with P
204Concentration is 30% extraction system, at normal temperatures, adopts 4 grades of indium sulfates in the extraction process extraction leach liquor; Employing equivalent concentration is that the aqueous hydrochloric acid of 6-7N is the back extraction medium, to adopting P
204Strip for the organic phase that is rich in indium sulfate of extraction agent, reextraction progression is 4 grades, contains indium at 50～100g/L in the control anti-stripping agent; The horizontal counter-current extraction groove that extraction tank adopts full PVC to make; Adopt the indium ion in the pure aluminum plate displacement anti-stripping agent, obtain the sponge indium, die casting melted ingot then obtains containing the thick indium of indium 98.5%.
Result: 7.628 kilograms of thick indiums that obtain to contain indium 98.5%.
Example five:
To direct leaching indium in 2.5 tons of indium sulfide concentrates that contain indium 2000 gram/tons, step is as follows:
1, moisture 8% with 2.5 tons, contain indium 2000 gram/ton indium sulfide concentrate fragmentations, add water for ball milling, be milled down to ore pulp and cross 200 mesh sieves and reach more than 85%.
2, according to above-mentioned grind the weight and the water content of ore pulp, the sulfuric acid and the water that add calculated amount, making the sulfuric acid concentration in the aqueous sulfuric acid is 160 grams per liters, solvent and solute weight ratio is at 5: 1, their added in 15 cubic metres the pressure reaction still, with steam heating and with flow aerating oxygen in reactor of 1.8 kg/minute, the control reactor temperature is at 150 ℃ ± 1 ℃, keep still internal pressure 1.2MPa, allow indium sulfide concentrate reaction kettle for reaction leaching 240 minutes, detecting the indium leaching yield is 95%.
3, adopt plate-and-frame filter press, the leach liquor of aforesaid reaction vessel is carried out liquid-solid separation, the solid after liquid-solid separation separates is a leached mud, and the liquid after liquid-solid separation separates is leach liquor.
4, adopt extracting-back extraction-replacing process technology extraction separation to obtain indium to above-mentioned leach liquor and adopt P
204Be extraction agent, with 200
#Kerosene is under the situation of thinner, is mixed with P
204Concentration is 30% extraction system, at normal temperatures, adopts 4 grades of indium sulfates in the extraction process extraction leach liquor; Adopting equivalent concentration is that the normal aqueous hydrochloric acid of 6-7N is the back extraction medium, to adopting P
204Strip for the organic phase that is rich in indium sulfate of extraction agent, reextraction progression is 4 grades, contains indium at 50～100g/L in the control anti-stripping agent; The horizontal counter-current extraction groove that extraction tank adopts full PVC to make; Adopt the indium ion in the pure aluminum plate displacement anti-stripping agent, obtain the sponge indium, die casting melted ingot then obtains containing the thick indium of indium 98.5%.
Result: 4.50 kilograms of thick indiums that obtain to contain indium 98.5%.
Claims (2)
1. the direct method of leaching indium in the indium ore deposit the steps include:
(1), dissolving indium compound: will pulverize, levigate indium sulfide concentrate joins in the reactor with sulfuric acid concentration is that the aqueous sulfuric acid of 100～300 grams per liters mixes, solvent and solute weight ratio is 4: 1,4.5: 1,5: 1,6: 1, aerating oxygen and to control the still internal pressure be 1.0MPa～6.0MPa in reactor, 100 ℃～300 ℃ of heating and control still interior reaction temperatures, allow sulfuric acid, oxygen and indium sulfide concentrate in reaction kettle for reaction, the reaction leaching time is 30 minutes～240 minutes, and indium is leached in leach liquor with the form of easily dissolving compound;
(2), the material with reactor carries out liquid-solid separation, the acquisition leach liquor;
(3), adopt extracting-back extraction-replacing process technology extraction separation to obtain indium to above-mentioned leach liquor.
2. the method for direct leaching indium in the indium according to claim 1 ore deposit is characterized in that: in the step of described acidleach dissolving indium compound, the pressure in the reactor is 1.2MPa～1.3MPa, and the temperature in the reactor is 150 ℃～250 ℃.
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| CN103602815B (en) * | 2013-11-06 | 2015-12-09 | 四川长虹电器股份有限公司 | The method of recovery indium from waste liquid crystal display |
| CN104357661B (en) * | 2014-10-30 | 2017-05-31 | 云南铜业股份有限公司 | A kind of Recovering Copper from lead copper matte, the method for indium |
| CN105886797A (en) * | 2015-01-25 | 2016-08-24 | 昆明冶金高等专科学校 | Method for preparing sponge indium from polymetallic sulfide material |
| CN105907978B (en) * | 2016-04-20 | 2018-06-29 | 武汉长海高新技术有限公司 | A kind of method of recovery indium in flue dust containing indium |
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