CN102851496A - Treatment method of high-indium high-iron zinc concentrate - Google Patents
Treatment method of high-indium high-iron zinc concentrate Download PDFInfo
- Publication number
- CN102851496A CN102851496A CN2012103773958A CN201210377395A CN102851496A CN 102851496 A CN102851496 A CN 102851496A CN 2012103773958 A CN2012103773958 A CN 2012103773958A CN 201210377395 A CN201210377395 A CN 201210377395A CN 102851496 A CN102851496 A CN 102851496A
- Authority
- CN
- China
- Prior art keywords
- indium
- zinc
- iron
- pressure
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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 relates to a treatment method of high-indium high-iron zinc concentrate, which comprises the following steps: carrying out two-section acidic reflux oxygen pressure leaching, including low-oxygen-pressure leaching and high-oxygen-pressure leaching, on zinc concentrate which contains 0.07-0.25% of indium In, 14-25% of iron and 40-50% of zinc; directly extracting indium from the low-oxygen-pressure leaching solution; precipitating iron from the solution after indium extraction by an oxygen pressure hematite process, thereby producing hematite slag containing 55-65% of iron; neutralizing the solution after iron precipitation with zinc oxide; carrying out zinc dust purification electrolysis on the neutralized solution to produce electric zinc; returning the neutralized slag to the low-oxygen-pressure leaching; and separating sulfur concentrate and flotation tailings from the high-oxygen-pressure leaching slag by a flotation process, recovering sulfur from the sulfur, and sending the flotation tailings into a fuming furnace to carry out reduction volatilization treatment. The invention can effectively separate iron, zinc and indium in the zinc concentrate, enhance the smelting recovery rate of zinc and indium, recycle iron in the zinc concentrate as a resource, and fundamentally avoid producing low-concentration sulfur dioxide, thereby effectively protecting the environment.
Description
Technical field
The present invention relates to a kind of non-ferrous metal metallurgy method, particularly a kind for the treatment of process that contains indium In0.07%～0.25%, iron content 14%～25%, contains zinc 40～50% zinc ore concentrates.
Background technology
At present, processing the treatment process that the zinc ore concentrate contain indium In0.07%～0.25%, iron content 14%～25% zinc, to contain zinc 40～50% extracts the zinc indium is: Fluidized Bed Roast of Zinc Concentrates desulfurization-zinc baking sand hot acid leaches--and the siderotil method sink iron indium-middle supernatant solution purification electrodeposition and is produced electric zinc-iron vitriol slag reduction volatilization recovery zinc indium.The method is called for short " heat acid leaching-ferro-alum method sink iron " technique, in the method, the higher leaching yield of zinc acquisition, iron and indium coprecipitation are enriched in the iron vitriol slag; By carrying out the reduction volatilization processing to containing the indium iron vitriol slag in rotary kiln, obtained the flue dust of enrichment zinc indium again, be called for short rich indium flue dust, rich indium flue dust extracts indium by the conventional indium-extracting process of processes such as " leaching-extraction-back extractions-displacement-electrolysis " again.The main drawback of the method is: (1) iron vitriol slag quantity of slag is large, carries out need to consuming a large amount of cokes when reduction volatilization is processed at rotary kiln, and production cost is high; (2) smelting recovery of indium is low, and on average containing indium in the revolution kiln slag of output is 0.03%, causes the indium that accounts for raw material zinc ore concentrate indium metal total amount about 10% to reclaim; (3) contain a large amount of sulfate radicals in the iron vitriol slag, in rotary kiln reduction volatilization process, decomposite a large amount of sulfur dioxide gas, after the reduction volatilization flue gas need to absorb processing, could qualified discharge.
In order to address the above problem, many metallargists have carried out a large amount of explorations and test.Chinese patent CN200510031335.0 has proposed to adopt conventional neutral leaching method that major part is reclaimed easily, the zinc that exists with the zinc oxide form is dissolved in the solution, separate with unmanageable zinc ferrite, then neutral leaching residue being carried out the high temperature reduction volatilization processes, make again zinc, indium separates with iron, from the volatilization flue dust, reclaim zinc and indium at last, in this technique, 92% zinc and 70% indium have obtained efficient recovery, but adopt the high temperature reduction volatilization to process neutral leaching residue, the quantity of slag is very large, and slag contains zinc up to more than 25%, the production cost of high temperature reduction volatilization is very high, and the smelting recovery of indium is low, thereby does not finally realize processing containing indium In0.07%～0.25%, the industrial applications of iron content 14%～25% zinc ore concentrate.
2004～2006 years, Guangxi Huaxi Group Co., Ltd and Central South University have developed jointly the slag-free zinc hydrometallurgy method, applied for patent of invention by the plan hall teacher of Tang of Central South University, patent of invention number is ZL95110609.0, the basic ideas of slag-free zinc hydrometallurgy method are, the zinc baking sand that obtains behind the fluidizing furnace fluidized bed roasting soaks in carrying out, make 70～80% zinc metal enter middle supernatant liquor, produce electric zinc product, neutral leaching residue carries out hot acid and leaches, and makes the dissolving of zinc indium enter solution, and solution adds iron powder or zinc sulfide concentrates reduction, after indium was carried in reducing solution process P204 extraction, the remaining liquid of extraction was produced the coprecipitated starch of ferrite.In this technique, zinc indium leaching yield is high, and leach liquor is reduced, iron in the solution is existed with bivalent form, adopt directly the reduction leach liquor is extracted the recovery indium, effectively shortened the indium-extracting process flow process, the smelting recovery of indium is very high, reaches more than 90%.In this technique, do not adopt oxygen to press the heavy iron technology of hematite process, but the iron in the solution and zinc are carried out co-precipitation, the coprecipitated starch of output ferrite, this patent of invention Special attention will be given to " without the scum " in the technical process, namely in the whole technical process, output scum no longer, but the iron in the raw material has been transferred in the coprecipitated starch of ferrite, iron gets utilization.The method is owing to a large amount of carbon ammonium of consumption, and a large amount of ammoniumsulphate soln of process discharging, and therefore final to apply industrial.
2007～2008 years, Guangxi Huaxi Group Co., Ltd and Beijing Mine and Metallurgy General Inst have developed jointly " the heavy indium of low acid solution reduction-oxygen is pressed the heavy iron of hematite process " and have extracted zinc indium technique, the basic ideas of this technique are, the Zn system trunk Production Flow Chart that keeps as far as possible guest Hua Xi to smelt company limited changes less, adopt the high temperature reduction technology that the low supernatant solution that contains indium is reduced, make the ferric iron in the solution be reduced to ferrous iron, then carry out that heavy indium is replaced in pre-neutralization again and from heavy indium slag the heavy indium that extracts, solution carries out returning neutral the leaching after oxygen is pressed the heavy iron of hematite process behind the heavy indium.In this technique, owing to directly reclaim indium from indium slag, indium has the higher rate of recovery, can reach more than 90%, owing to adopted the comparatively advanced heavy iron of hematite process, the balance of acid has obtained effective control in the flow process again.This technique has been finished pilot-plant test, and smelts one of alternative process of company limited's technological transformation as guest Hua Xi.This technique is not applied for the invention technical patent, and the main purpose of pilot-plant test is except the technical feasibility of checking technical process, has also verified the suitability of domestic titanium material autoclave.
Summary of the invention
The treatment process that the purpose of this invention is to provide a kind of high indium high-iron zinc sulfide concentrate; for containing indium In0.07%～0.25%, iron content 14%～25%, containing zinc 40～50% zinc ore concentrates; iron in the effective separation zinc ore concentrate, zinc, indium; improve zinc, indium smelting recovery; and the rhombohedral iron ore slag that iron in the zinc ore concentrate is converted into contain Fe55～65% recycling in addition; avoid simultaneously the output of low-concentration sulfur dioxide from root, effectively protected environment.
The present invention achieves the above object by the following technical programs: a kind for the treatment of process of high indium high-iron zinc sulfide concentrate, Fig. 1 is seen in technical process, raw material is for containing indium In0.07%～0.25%, iron content 14%～25%, containing zinc 40～50% zinc ore concentrates, carry out according to the following steps: percentage ratio of the present invention is by industry general knowledge, when not specifying, refer to weight percentage, extraction with strip compare the finger percent by volume;
(1) low oxygen pressure leaches: with the high oxygen pressure infusion solution that contains acid 60～100g/L of described zinc ore concentrate and step (2) output, in autoclave pressure in 130～140 ℃, stagnation pressure 0.27～0.36MPa, oxygen partial pressure 0.05～0.10MPa leached 3～5 hours, leached eventually acid 20～30g/L, Fe
3+≤ 3g/L, after the extract process solid-liquid separation, output low oxygen pressure infusion solution and low oxygen pressure leached mud;
(2) high oxygen pressure leaches: with low oxygen pressure leached mud, the electrolysis waste solution that contains acid 135～165g/L and the additional industrial vitriol oil, in autoclave pressure, leached 3～5 hours in 170～175 ℃, stagnation pressure 0.89～1.00MPa, oxygen partial pressure 0.2MPa, leach whole acid≤100g/L, extract is through after the solid-liquid separation, output high oxygen pressure infusion solution and high oxygen pressure leached mud, high oxygen pressure infusion solution return step (1) low oxygen pressure leaching process;
(3) indium is carried in the extraction of low oxygen pressure leach liquor: it is that the extraction agent that 20%P204+80% kerosene is made into extracts the extraction indium that the low oxygen pressure infusion solution adopts volume ratio, extraction temperature is 10～40 ℃, compare A/O=20:1～50:1, extraction progression is 3 grades, obtains negative indium organic phase and the remaining liquid of indium extraction; Negative indium organic phase is stripped by 3 grades of concentration of hydrochloric acid 4.5～5.5mol, O/A=10:1～30:1, back extraction progression, then replaces at ambient temperature 3～7 days with zinc ingot metal, obtains the sponge indium, the thick indium of the group's of pressure founding anode, 5～8 days smart indiums of output of thick indium electrolysis;
(4) oxygen is pressed the heavy iron of rhombohedral iron ore: the remaining liquid of indium extraction carried out the heavy iron of hematite process 4～6 hours in 170～175 ℃, stagnation pressure 0.89～1.00MPa, oxygen partial pressure 0.2MPa in autoclave pressure, solution Fe≤3g/L behind the heavy iron, heavy iron after product is through after the solid-liquid separation, solution behind output rhombohedral iron ore slag and the heavy iron, the rhombohedral iron ore slag utilizes as iron resources;
(5) neutralization: behind heavy iron, add oxide powder and zinc in the liquid and neutralize, neutral temperature be 60～80 ℃, in and 1～2 hour time, terminal point pH=4.0～5.5, neutralized reaction product is through after the solid-liquid separation, output neutral solution and in and slag, neutral solution is produced electric zinc through conventional zinc powder cleansing soln electrolysis process, in and slag return low oxygen pressure and leach;
(6) high oxygen pressure leaching residue flotation: employing is sent out the high oxygen pressure leached mud without the medicament method for floating and is isolated the sulphur concentrate that contains S 〉=75% and contain S≤20% flotation tailings, retrieving sulphur concentrate sulphur;
(7) the flotation tailings volatilization is processed: flotation tailings carries out the high temperature reduction volatilization to be processed, valuable metal tin, lead, antimony, silver and the zinc that is not leached on a small quantity, indium volatilization enter in the flue dust, by the processing to flue dust, reclaim wherein zinc, indium, tin, lead, antimony, silver, high temperature furnace slag is sold to cement industry as raw material.
Advantage of the present invention is:
(1), method is with strong points.Employing the present invention makes iron in the zinc ore concentrate, zinc, indium three's separation reasonable, orderly, efficient, has guaranteed that not only zinc, indium have the higher rate of recovery, and the zinc total yield is 96%, and the indium total yield is 93%.
(2), process optimization.With oxygen press to leach, directly extraction carry indium, oxygen press heavy three the zinc hydrometallurgy modern techniquies of iron of hematite process carried out effective integrated with optimize, technical process is succinct, has realized the high efficiente callback of indium and zinc, has also solved solution equilibria and the acid balance problem in the flow process.
(3), energy-conserving and environment-protective.Adopt oxygen to press leaching-out technique and oxygen to press the heavy iron technology of rhombohedral iron ore to substitute respectively fluidized bed roasting technology and rotary kiln reduction volatilization technology, more efficient realization iron zinc separates, and has also avoided the output of low-concentration sulfur dioxide from root.
Embodiment
By the following examples technical scheme of the present invention is described further.
Embodiment 1
The treatment process of high indium high-iron zinc sulfide concentrate of the present invention comprises the steps:
1, will contain indium In0.07%, iron content 14%, contain 70 kilograms of the zinc ore concentrates of zinc 48%, 3 kilograms of dry neutralization slags that contain zinc 32%, add and to contain sour 60g/L, contain zinc 98.7g/L, iron content 7.5 grams per liters, contain the high oxygen pressure leach liquor 390L of indium 0.073g/L, be 130～134 ℃ at extraction temperature, leach under stagnation pressure 0.30MPa, the oxygen partial pressure 0.05MPa condition, in 500L lining titanium autoclave pressure, leached 3 hours, extract is through after the solid-liquid separation, obtain low oxygen pressure infusion solution 374L, leach liquor contains zinc 131.8g/L, contains sour 20g/L, Fe
3+1.7g/L, Fe
Always10.8g/L, indium 0.116g/L, 82 kilograms of output hygrometric state low oxygen pressure leached muds.
2, with 82 kilograms of hygrometric state low oxygen pressure leached muds, 380L contains sour 165g/L, contains electrolysis waste solution and the 2L vitriol oil of zinc 50g/L, under the condition of 170～175 ℃ of extraction temperatures, leaching stagnation pressure 0.90MPa, oxygen partial pressure 0.2MPa, in 500L lining titanium autoclave pressure in leaching 3 hours, extract is through after the solid-liquid separation, obtain high oxygen pressure leach liquor 390L, leach liquor contains zinc 98.7g/L, contains sour 60g/L, Fe7.5g/L, contains indium 0.073g/L, 43 kilograms of output hygrometric state high oxygen pressure leached muds, water rate 31%, dried slag contain zinc 5.2%, contain indium 0.008%.
3, will contain zinc 131.8g/L, contain sour 20g/L, Fe
3+1.7g/L, Fe
Always10.8g/, L contains the low oxygen pressure leach liquor 374L of indium 0.116g/L, adopting volume ratio is that 20%P204+80% kerosene is made into extraction agent, extract at mixed settler extractor and to carry indium, extraction temperature is 25 ℃, compare A/O=20:1, extraction progression is 3 grades, obtains containing the indium-raffinate that indium is 0.0016g/L; Negative indium organic phase is stripped at mixed settler extractor and is carried indium, and the concentration of hydrochloric acid 4.5M that back extraction is used compares O/A=10:1,3 grades of back extraction progression; The chlorination of hydrochloric acid solution of indium that back extraction obtains was replaced 6 days at ambient temperature with zinc ingot metal, obtained the sponge indium, pressed group, founding to become thick indium anode, thick indium electrolysis 7 days, and the smart indium of output meets 99.995% smart indium of YS/T257-2009 standard.
4, will contain zinc 131.8g/L, contain sour 20g/L, Fe
3+1.7g/L, Fe
Always10.8g/L the remaining liquid 374L of indium extraction, under 170～175 ℃, the condition of stagnation pressure 0.90MPa, oxygen partial pressure 0.2MPa, in 500L lining titanium autoclave pressure, carried out the heavy iron of hematite process 4 hours, heavy iron after product is through after the solid-liquid separation, solution 367L behind the heavy iron contains Fe
Always1.4g/L, contain sour 40g/L, 7.73 kilograms of output hygrometric state rhombohedral iron ore slags, moisture 26%, 5.72 kilograms of dry state rhombohedral iron ore slags, contain zinc 6.8% at rhombohedral iron ore slag iron content 59%.
5, adding 14 kilograms of oxide powder and zincs that contain zinc 76% among the liquid 367L behind heavy iron neutralizes, neutral temperature be 60～80 ℃, in and 1.5 hours time, terminal point pH=5.0, neutralized reaction product is through after the solid-liquid separation, in output neutral solution 365L and the hygrometric state and 4.6 kilograms of slags, in the hygrometric state and slag moisture 34%, in and slag contain zinc 32%, return low oxygen pressure and leach processing, neutral solution 365L produces electric zinc through conventional zinc powder cleansing soln electrolysis process;
6, employing is carried out flotation separation without the medicament method for floating with 43 kilograms of hygrometric state high oxygen pressure leached muds, 31 kilograms in output hygrometric state sulphur concentrate, and water rate 32%, the sulphur concentrate contains S88.1%, retrieving sulphur concentrate sulphur; 13 kilograms of flotation tailings hygrometric states, water rate 36% contains S17.8%.
7, flotation tailings enters fuming furnace and carries out high temperature reduction volatilization and process, valuable metal zinc, indium, tin, lead, antimony volatilization enter in the flue dust, by the processing to flue dust, reclaim wherein zinc, indium, tin, lead, antimony, the fuming slag is sold to cement industry as raw material.
Embodiment 2
Another example of the treatment process of high indium high-iron zinc sulfide concentrate of the present invention comprises the steps:
1, contain indium In0.15%, iron content 18%, contain 4.2 tons of the zinc ore concentrates of zinc 49%, 200 kilograms of dry neutralization slags that contain zinc 23%, add and to contain sour 87g/L, contain zinc 90.1g/L, iron content 7.9 grams per liters, contain 23.4 cubic metres of the high oxygen pressure leach liquors of indium 0.149g/L, under 133～138 ℃ of extraction temperatures, leaching stagnation pressure 0.32MPa, the oxygen partial pressure 0.08MPa condition, in 30 cubic metres lining titanium autoclave pressure, leached 4 hours, extract is through after the solid-liquid separation, obtain 22.1 cubic metres of low oxygen pressure infusion solutions, infusion solution contains zinc 134.1g/L, contains sour 23g/L, Fe
3+1.3g/L, Fe
Always12.9g/L, contain indium 0.251g/L, 4.25 tons of output hygrometric state low oxygen pressure leached muds.
2, with 4.25 tons of hygrometric state low oxygen pressure leached muds, 23.0 cubic meter contains sour 163g/L, electrolysis waste solution and 0.2 cubic metre of vitriol oil of containing zinc 48g/L, 173～177 ℃ of extraction temperatures, leach stagnation pressure 0.95MPa, under the condition of oxygen partial pressure 0.2MPa, in the lining titanium autoclave pressure of 30 cubic metres of volumes in leaching 3.5 hours, extract is through after the solid-liquid separation, obtain 23.4 cubic metres of high oxygen pressure leach liquors, leach liquor contains zinc 90.1g/L, contain sour 87g/L, Fe7.9g/L, contain indium 0.149g/L, 2.94 tons of output hygrometric state high oxygen pressure leached muds, water ratio 31%, dried slag contains zinc 4.8%, contain indium 0.012%.
3, will contain zinc 134.1g/L, contain sour 21g/L, Fe
3+1.37g/L, Fe
Always12.9g/L, contain 23.0 cubic metres of the low oxygen pressure leach liquors of indium 0.251g/L, adopting volume ratio is that 20%P204+80% kerosene is made into extraction agent, extract at mixed settler extractor and to carry indium, extraction temperature is 27 ℃, compare A/O=20:1, extraction progression is 3 grades, and obtaining the remaining liquid of indium extraction, to contain indium be 0.0023g/L; Negative indium organic phase is stripped at mixed settler extractor and is carried indium, and reextraction concentration of hydrochloric acid 4.8M compares O/A=15:1,3 grades of back extraction progression; The chlorination of hydrochloric acid solution of indium that reextraction obtains was replaced 6 days at ambient temperature with zinc ingot metal, and obtain the sponge indium and press the thick indium of group's founding anode, thick indium electrolysis 6 days, the smart indium of output meets 99.995% of YS/T257-2009 standard.
4, will contain zinc 134.1g/L, contain sour 23g/L, Fe
3+1.37g/L, Fe
Always12.9g/L 23.0 cubic metres of remaining liquid of indium extraction, under 173～178 ℃, the condition of stagnation pressure 0.95MPa, oxygen partial pressure 0.2MPa, in 30 cubic metres lining titanium autoclave pressure, carried out the heavy iron of hematite process 4.5 hours, heavy iron after product is through after the solid-liquid separation, solution is 22.1 cubic metres behind the heavy iron, contains Fe
Always1.54g/L, contain sour 41g/L, 0.598 ton of output hygrometric state rhombohedral iron ore slag, water rate 25%, 0.448 ton of dry state rhombohedral iron ore slag, contains zinc 6.9% at rhombohedral iron ore slag iron content 58%.
5, behind heavy iron in 22.1 cubic metres of the liquid, adding 0.95 ton of oxide powder and zinc containing zinc 74% neutralizes, neutral temperature be 65～75 ℃, in and 1.5 hours time, terminal point pH=5.0, neutralized reaction product is through after the solid-liquid separation, in 22.0 cubic metres of output neutral solutions and the hygrometric state and 495 kilograms of slags, in the hygrometric state and slag moisture 34%, the dry neutralization slag contains zinc 23%, returns low oxygen pressure and leaches and process, 22.0 cubic metres of zinc powders through routine of neutral solution purify, electrolysis of solutions explained hereafter electricity zinc.
6, employing is carried out flotation separation without the medicament method for floating with 2.94 tons of hygrometric state high oxygen pressure leached muds, 1.92 tons in output hygrometric state sulphur concentrate, and water rate 32%, the sulphur concentrate contains S85.7%, retrieving sulphur concentrate sulphur; 1.11 tons of flotation tailings hygrometric states, water rate 35% contains S19.6%.
7, flotation tailings enters fuming furnace and carries out high temperature reduction volatilization and process, valuable metal zinc, indium, tin, lead, antimony volatilization enter in the flue dust, by the processing to flue dust, reclaim wherein zinc, indium, tin, lead, antimony, the fuming slag is sold to cement industry as raw material.
Embodiment 3
The another example of the treatment process of high indium high-iron zinc sulfide concentrate of the present invention comprises the steps:
1, will contain indium In0.25%, iron content 25%, contain 4.0 tons of the zinc ore concentrates of zinc 50%, 200 kilograms of dry neutralization slags that contain zinc 30%, add and to contain sour 100g/L, contain zinc 87.5g/L, iron content 10.4 grams per liters, contain 24.6 cubic metres of the high oxygen pressure leach liquors of indium 0.221g/L, under 135～140 ℃ of extraction temperatures, leaching stagnation pressure 0.35MPa, the oxygen partial pressure 0.10MPa condition, in 30 cubic metres lining titanium autoclave pressure, leached 4.5 hours, extract is through after the solid-liquid separation, obtain 23.2 cubic metres of low oxygen pressure leach liquors, leach liquor contains zinc 124.6g/L, contains sour 29.6g/L, Fe
3+1.9g/L, Fe
Always16.8g/L, contain indium 0.383g/L, 4.07 tons of output hygrometric state low oxygen pressure leached muds.
2, with 4.07 tons of hygrometric state low oxygen pressure leached muds, 24.1 cubic meter contains sour 161g/L, electrolysis waste solution and 0.3 cubic metre of vitriol oil of containing zinc 45g/L, 175～180 ℃ of extraction temperatures, leach stagnation pressure 1.00MPa, under the condition of oxygen partial pressure 0.2MPa, in the lining titanium autoclave pressure of 30 cubic metres of volumes in leaching 4.5 hours, extract is through after the solid-liquid separation, obtain 24.6 cubic metres of high oxygen pressure leach liquors, leach liquor contains zinc 87.5g/L, contain sour 100g/L, Fe10.4g/L, contain indium 0.221g/L, 2.87 tons of output hygrometric state high oxygen pressure leached muds, water rate 31%, dried slag contains zinc 4.35%, contain indium 0.019%.
3, will contain zinc 124.6g/L, contain sour 18.6g/L, Fe
3+1.9g/L, Fe
Always16.8g/L, contain 23.2 cubic metres of the low oxygen pressure leach liquors of indium 0.383g/L, adopting volume ratio is that 20%P204+80% kerosene is made into organism, extract at mixed settler extractor and to carry indium, extraction temperature is 24 ℃, compare A/O=25:1, extraction progression is 3 grades, and obtaining the remaining liquid of indium extraction, to contain indium be 0.0023g/L; Negative indium organic phase is stripped at mixed settler extractor and is carried indium, and reextraction concentration of hydrochloric acid 4.6M compares O/A=20:1,3 grades of back extraction progression; The chlorination of hydrochloric acid solution of indium that reextraction obtains was replaced 6 days at ambient temperature with zinc ingot metal, and obtain the sponge indium and press the thick indium of group's founding anode, thick indium electrolysis 6 days, the smart indium of output meets 99.995% of YS/T257-2009 standard.
4, will contain zinc 124.6g/L, contain sour 19g/L, Fe
3+1.9g/L, Fe
Always16.8g/L 23.2 cubic metres of remaining liquid of indium extraction, under 175～1808 ℃, the condition of stagnation pressure .1.00MPa, oxygen partial pressure 0.2MPa, in 30 cubic metres lining titanium autoclave pressure, carried out the heavy iron of hematite process 4.5 hours, heavy iron after product is through after the solid-liquid separation, solution is 22.3 cubic metres behind the heavy iron, contains Fe
Always1.23g/L, contain sour 46.7g/L, 0.815 ton of output hygrometric state rhombohedral iron ore slag, water rate 25%, 0.611 ton of dry state rhombohedral iron ore slag, contains zinc 5.1% at rhombohedral iron ore slag iron content 60%.
5, behind heavy iron in 22.3 cubic metres of the liquid, adding 0.97 ton of oxide powder and zinc containing zinc 78% neutralizes, neutral temperature be 70～805 ℃, in and 1.5 hours time, terminal point pH=5.0, neutralized reaction product is through after the solid-liquid separation, in 22.0 cubic metres of output neutral solutions and the hygrometric state and 495 kilograms of slags, in the hygrometric state and slag moisture 33%, the dry neutralization slag contains zinc 22%, returns low oxygen pressure and leaches processing, and 22.0 cubic metres of zinc powder cleansing soln electrolysis process through routine of neutral solution are produced electric zinc.
6, employing is carried out flotation separation without the medicament method for floating with 2.87 tons of hygrometric state high oxygen pressure leached muds, 1.88 tons in output hygrometric state sulphur concentrate, and water rate 32%, the sulphur concentrate contains S83.4%, retrieving sulphur concentrate sulphur; 1.06 tons of flotation tailings hygrometric states, water rate 35% contains S18.0%.
7, flotation tailings enters fuming furnace and carries out high temperature reduction volatilization and process, valuable metal zinc, indium, tin, lead, antimony volatilization enter in the flue dust, by the processing to flue dust, reclaim wherein zinc, indium, tin, lead, antimony, the fuming slag is sold to cement industry as raw material.
Claims (1)
1. the treatment process of a high indium high-iron zinc sulfide concentrate is characterized in that, raw material carries out according to the following steps for containing indium In0.07%～0.25%, iron content 14%～25%, containing zinc 40～50% zinc ore concentrates:
(1) low oxygen pressure leaches: with containing of described zinc ore concentrate and step (2) output of sour 60～100g/L high oxygen pressure infusion solution, in autoclave pressure in 130～140 ℃, stagnation pressure 0.27～0.36MPa, oxygen partial pressure 0.05～0.10MPa leached 3～5 hours, leached eventually acid 20～30g/L, Fe
3+≤ 3g/L, after the extract process solid-liquid separation, output low oxygen pressure infusion solution and low oxygen pressure leached mud;
(2) high oxygen pressure leaches: with the low oxygen pressure leached mud, contain acid 135～165g/L electrolysis waste solution and the additional industrial vitriol oil, in autoclave pressure, leached 3～5 hours in 170～175 ℃, stagnation pressure 0.89～1.00MPa, oxygen partial pressure 0.2MPa, leach eventually acid 60～100g/L, extract is through after the solid-liquid separation, output high oxygen pressure infusion solution and high oxygen pressure leached mud, high oxygen pressure infusion solution return the low oxygen pressure leaching process of step (1);
(3) indium is carried in the extraction of low oxygen pressure infusion solution: it is that the extraction agent that 20%P204+80% kerosene is made into extracts the extraction indium that the low oxygen pressure infusion solution adopts volume ratio, extraction temperature is 10～40 ℃, compare A/O=20:1～50:1, extraction progression is 3 grades, obtains negative indium organic phase and the remaining liquid of indium extraction; Negative indium organic phase is stripped by 3 grades of concentration of hydrochloric acid 4.5～5.5mol, O/A=10:1～30:1, back extraction progression, then replaces at ambient temperature 3～7 days with zinc ingot metal, obtains the sponge indium, the thick indium of the group's of pressure founding anode, 5～8 days smart indiums of output of thick indium electrolysis;
(4) oxygen is pressed the heavy iron of rhombohedral iron ore: the remaining liquid of indium extraction carried out the heavy iron of hematite process 4～6 hours in 170～175 ℃, stagnation pressure 0.89～1.00MPa, oxygen partial pressure 0.2MPa in autoclave pressure, solution Fe≤3g/L behind the heavy iron, heavy iron after product is through after the solid-liquid separation, solution behind output rhombohedral iron ore slag and the heavy iron, the rhombohedral iron ore slag utilizes as iron resources;
(5) neutralization: behind heavy iron, add oxide powder and zinc in the liquid and neutralize, neutral temperature be 60～80 ℃, in and 1～2 hour time, solution terminal point pH=4.0～5.5, neutralized reaction product is through after the solid-liquid separation, output neutral solution and in and slag, after neutral solution purifies through conventional zinc powder with electrolysis explained hereafter electricity zinc, in and slag return low oxygen pressure and leach;
(6) high oxygen pressure leaching residue flotation: adopt without the medicament method for floating high oxygen pressure leached mud is isolated the sulphur concentrate that contains S 〉=75% and contained S≤20% flotation tailings, retrieving sulphur concentrate sulphur;
(7) the flotation tailings volatilization is processed: flotation tailings carries out the high temperature reduction volatilization to be processed, and reclaims wherein zinc, indium, tin, lead, antimony, silver.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103773958A CN102851496B (en) | 2012-10-08 | 2012-10-08 | Treatment method of high-indium high-iron zinc concentrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103773958A CN102851496B (en) | 2012-10-08 | 2012-10-08 | Treatment method of high-indium high-iron zinc concentrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102851496A true CN102851496A (en) | 2013-01-02 |
| CN102851496B CN102851496B (en) | 2013-12-18 |
Family
ID=47398468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103773958A Active CN102851496B (en) | 2012-10-08 | 2012-10-08 | Treatment method of high-indium high-iron zinc concentrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102851496B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103060559A (en) * | 2013-01-30 | 2013-04-24 | 昆明理工大学 | Microfluid extraction method for extracting and separating In, Fe and Zn |
| CN103173625A (en) * | 2013-04-19 | 2013-06-26 | 长沙矿冶研究院有限责任公司 | Method for efficiently leaching indium from zinc oxide smoke |
| CN103695663A (en) * | 2013-12-13 | 2014-04-02 | 来宾华锡冶炼有限公司 | Smelting method of high-iron multi-metal zinc concentrate |
| CN104148163A (en) * | 2014-07-29 | 2014-11-19 | 广西金山铟锗冶金化工有限公司 | Beneficiation method for processing low grade tin-lead-zinc multi-metal oxidized ores |
| CN105002354A (en) * | 2015-07-28 | 2015-10-28 | 昆明理工大学 | Method for leaching zinc and other valuable metal in zinc sulfide ore through medium-and-low-pressure oxygen enrichment |
| CN106893873A (en) * | 2016-12-28 | 2017-06-27 | 呼伦贝尔驰宏矿业有限公司 | A kind of common association concentrate zinc metallurgy method of zinc sulphide containing indium, silver, arsenic |
| CN108048659A (en) * | 2017-11-22 | 2018-05-18 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | A kind of leaching method of zinc replacement slag |
| CN110872650A (en) * | 2018-08-31 | 2020-03-10 | 呼伦贝尔驰宏矿业有限公司 | Leaching method of zinc concentrate |
| CN111118303A (en) * | 2019-12-05 | 2020-05-08 | 西部矿业股份有限公司 | Method for preparing zinc hypoxide by oxygen pressure leaching of zinc smelting solid waste slag |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664131A (en) * | 2004-12-15 | 2005-09-07 | 云南冶金集团总公司 | Method for extracting indium from high-indium high-iron zinc sulphide concentrates by pressure acid leach and solvent extraction |
| CN101003854A (en) * | 2007-01-22 | 2007-07-25 | 中国科学院过程工程研究所 | New method for soaking out enriched ores of high indium, high iron, and high sulfur zinc |
-
2012
- 2012-10-08 CN CN2012103773958A patent/CN102851496B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664131A (en) * | 2004-12-15 | 2005-09-07 | 云南冶金集团总公司 | Method for extracting indium from high-indium high-iron zinc sulphide concentrates by pressure acid leach and solvent extraction |
| CN101003854A (en) * | 2007-01-22 | 2007-07-25 | 中国科学院过程工程研究所 | New method for soaking out enriched ores of high indium, high iron, and high sulfur zinc |
Non-Patent Citations (1)
| Title |
|---|
| 夏光祥等: "高铟高铁锌精矿氧压浸出新工艺研究", 《有色金属》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103060559A (en) * | 2013-01-30 | 2013-04-24 | 昆明理工大学 | Microfluid extraction method for extracting and separating In, Fe and Zn |
| CN103173625A (en) * | 2013-04-19 | 2013-06-26 | 长沙矿冶研究院有限责任公司 | Method for efficiently leaching indium from zinc oxide smoke |
| CN103173625B (en) * | 2013-04-19 | 2014-12-10 | 长沙矿冶研究院有限责任公司 | Method for efficiently leaching indium from zinc oxide smoke |
| CN103695663A (en) * | 2013-12-13 | 2014-04-02 | 来宾华锡冶炼有限公司 | Smelting method of high-iron multi-metal zinc concentrate |
| CN104148163A (en) * | 2014-07-29 | 2014-11-19 | 广西金山铟锗冶金化工有限公司 | Beneficiation method for processing low grade tin-lead-zinc multi-metal oxidized ores |
| CN104148163B (en) * | 2014-07-29 | 2016-08-31 | 广西金山铟锗冶金化工有限公司 | A kind of beneficiation method processing low-grade tin-lead-zinc multi-metal oxygen ore deposit |
| CN105002354A (en) * | 2015-07-28 | 2015-10-28 | 昆明理工大学 | Method for leaching zinc and other valuable metal in zinc sulfide ore through medium-and-low-pressure oxygen enrichment |
| CN106893873A (en) * | 2016-12-28 | 2017-06-27 | 呼伦贝尔驰宏矿业有限公司 | A kind of common association concentrate zinc metallurgy method of zinc sulphide containing indium, silver, arsenic |
| CN106893873B (en) * | 2016-12-28 | 2018-11-27 | 呼伦贝尔驰宏矿业有限公司 | A kind of zinc sulphide containing indium, silver, arsenic is total to association concentrate zinc metallurgy method |
| CN108048659A (en) * | 2017-11-22 | 2018-05-18 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | A kind of leaching method of zinc replacement slag |
| CN110872650A (en) * | 2018-08-31 | 2020-03-10 | 呼伦贝尔驰宏矿业有限公司 | Leaching method of zinc concentrate |
| CN111118303A (en) * | 2019-12-05 | 2020-05-08 | 西部矿业股份有限公司 | Method for preparing zinc hypoxide by oxygen pressure leaching of zinc smelting solid waste slag |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102851496B (en) | 2013-12-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102851496B (en) | Treatment method of high-indium high-iron zinc concentrate | |
| CN102312083A (en) | Method for extracting zinc indium and recovering iron from high-iron high indium zinc concentrate | |
| CN107312930B (en) | A kind of method that low nickel matte leaching solution pyrolysis removes iron | |
| CN104531988B (en) | A kind of recovery process of difficult complex multi-metal ore deposit | |
| CN104745810A (en) | Treatment technique of copper-containing high-indium high-iron zinc sulfide concentrate | |
| CN103911512A (en) | Method for removing arsenic and antimony from zinc smelting leaching solution | |
| CN102912147A (en) | Process for recycling lead zinc, silver and iron from tailings after carrying out sulphur flotation on zinc oxygen pressure leaching slag | |
| AU2017402487B2 (en) | Beneficiation method for mixed copper ore with low oxidation rate and high binding rate | |
| CN102978391A (en) | Technology for zinc wet-process clean smelting and resource comprehensive recycling | |
| CN102888515A (en) | Comprehensive utilization method of amarillite slag | |
| CN104726724A (en) | Method for extracting scandium from nickel laterite ores | |
| CN103882236A (en) | Method for processing high-sulfur copper dust and recovering copper by employing a wet process | |
| CN104775030A (en) | Iron removal method in zinc hydrometallurgy process of high-iron zinc sulfide concentrate | |
| CN105177307A (en) | Method for recycling copper-nickel-cobalt from low grade nickel matte through abrasive flotation separation | |
| CN109609768A (en) | A kind of method of comprehensive utilization of low-grade cupric cobalt sulfate slag | |
| CN103484694A (en) | Method for extracting bismuth from copper-bismuth concentrate | |
| CN106957965B (en) | A kind of preparation method of iron oxide product | |
| CN106834698B (en) | A method of the enriching and reclaiming indium from acid solution of the low concentration containing indium | |
| CN103952562A (en) | Comprehensive utilization method of iron vitriol slag | |
| CN103276211B (en) | Method for extracting iron and vanadium from vanadium-titanium magnetite concentrates | |
| CN106906360B (en) | A kind of technique of synthetical recovery cupric cobalt sulfate slag | |
| CN108265177B (en) | A kind of method of zinc hydrometallurgy kiln slag and waste acid comprehensive utilization | |
| CN103882222B (en) | Red soil nickel ore chloride salt baking extracts the method for nickel cobalt | |
| CN106957955A (en) | Handle the method and system of lateritic nickel ore | |
| CN107746961B (en) | A method of recycling antimony from antimony slag |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |