CN104232890A - Wet metallurgy process for low-grade zinc oxide ores - Google Patents
Wet metallurgy process for low-grade zinc oxide ores Download PDFInfo
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Abstract
The invention relates to a wet metallurgy process for low-grade zinc oxide ores. Two-stage leaching is adopted in the process, the leaching rate of Zn can be up to 92-95%, the leaching of impurities including Cu, Fe, Si and Al is effectively inhibited, and high-quality electrolytic zinc can be produced by using processes of extracting Zn by using P204 and electrodepositing the back extraction liquid of Zn. By using the process, the acid consumption is low, the low-grade zinc oxide ores are low in impurity content, high in Zn concentration and high in yield, and a leachate is easy to treat.
Description
Technical field
The present invention relates to field of metallurgy, be specifically related to a kind of hydrometallurgical processes of low-grade zinc oxide ore.
Background technology
Along with the development of the industries such as car industry, construction industry, air system, computer industry, communications industry, pharmaceutical sector, the purposes for zinc opens more wide prospect.It is predicted, the world consumption annual growth of zinc can remain on about 4% from now on, and for China, the application of much industrial sector zinc is also at the early-stage.People consumes zinc level and also falls far short than world average level, also has more wide zinc deficiency and excess to have to be developed.Consumption that is zinc-plated and die casting aspect zinc from now on increases and will accelerate.Therefore, carry forward vigorously the scientific-technical progress of enterprise, further develop production, active adoption novel process, new technology and new installation improve constantly quality product, reduce costs, to accelerate the development of China's Zn Cr coating.
China achieves some achievements in the treatment process of zinc oxide ore, particularly for low-grade zinc oxide ore, and existing many research.
CN102703694A discloses a kind of method of high ferro, low-grade zinc oxide ore wet processing that argillization degree is large, the steps include: 1, directly leach: zinc oxide ore together drops in reactive tank with zinc electrolytic waste liquid and reacts after fragmentation, ball milling, associating leaching done by leach liquor after reaction terminates, and leached mud gives next step washery slag process; 2, leaching is combined: higher-grade zinc oxide ore and the direct solution afterwards that leaches are carried out Leaching reaction, and neutral solution is for purification, and leached mud sends rotary kiln process back to; 3, washery slag: the slag directly leached and weakly acid soln are put into reactive tank and stirs, after reaction, solution returns direct leaching, the valuable metal such as send dressing-works Separation and Recovery plumbous, silver-colored of the leached mud after washing; 4, rotary kiln reduction volatilization: mixed with coal in rear input kiln by leached mud and react, obtain zinc oxide fumes recovery indium germanium, kiln slag reclaims iron, remaining coal.
CN102730748A discloses a kind of method utilizing middle-low grade zinc oxide ore and zinc oxide, plumbous oxide mineral intergrowth to prepare lead chloride and zinc sulfate, and the method comprises the following steps: (1) is broken by zinc ore, after levigate and ammonium sulfate baking mixed; (2) roasting Clinker digestion, gained filtrate carries out heavy iron, aluminium, puies forward the further separation of lead of cadmia; (3) after heavy iron, aluminium gained solution of zinc sulfate inspissation after for electrolysis; (4) put forward cadmia NaCl solution to leach, after leaching, gained filtrate concentrates, and crystallisation by cooling separates out PbCl2 crystal, and NaCl solution returns leaching operation, realizes recycle.
CN102433569A discloses a kind of method of carrying out electrolysis for ammonia leaching process process high basic gangue type low-grade zinc oxide ore leach liquor.The feature of the method is, the high basic gangue zinc oxide ore ammonia zinc ammonia complex solution of leaching after impurity and purification and anodic dissolution is separated with ionic membrane; Zine ion reduces on negative electrode, thus obtains the high metallic zinc of purity; Anode is only separated out O2 and NH3 decomposition is not occurred, and after electrolysis, catholyte can return for leaching.
CN102242262A discloses a kind of method of weakly alkaline amino acid salts system process low-grade zinc oxide ore, after levigate for complicated low-grade zinc oxide ore, coordinate in weakly alkaline amino acid salts system under certain condition and leach, zinc, lead, cadmium, copper and mickel etc. dissolve and enter leach liquor, and calcium, magnesium, iron and silicon etc. do not dissolve and stays in leached mud; Add CaO or Ca(OH in leach liquor) 2 make zinc with zinc oxide form precipitation reclaimed, the valuable metals such as lead, cadmium, copper and mickel and zinc Enrichment are in tutty; Solution CO2 regulator solution pH after depositing zinc makes leaching agent regenerate to certain value, and the leaching agent after regeneration returns recycle, CaCO3 Returning utilization after calcining of leaching agent regenerative process output.
CN101734686A discloses the method for a kind of high value-added greening comprehensive utilization middle-low grade zinc oxide ore (being mainly willemite, lapis calaminaris, smithsonite), the method comprises the following steps: (1) is broken by zinc oxide ore, levigate rear and ammoniumsulphate soln mix, roasting after drying and dehydrating (smithsonite need be calcined before batch mixing); (2) product of roasting is water-soluble, uses ferriammonium sulfate method removal of impurities, obtain zinc sulfate refined liquid after filtering; (3) zinc sulfate refined liquid electrodeposition zinc, electrodeposition waste liquid leads to ammonia makes ammonium sulfate recovery; (4) filter residue (mainly the oxide compound of siliceous, iron) prepares silica product with alkaline purification, and residual residue is used as iron-smelting raw material or deep processing becomes high value added product.
CN1632141A discloses a kind of acid-ammonia extraction of high silicon high iron low grade zinc oxide ore zinc, it is characterized in that this method is: (1) ore grinding, obtain breeze → (2) breeze normal temperature acid adding to transform → (3) add alkali or limestone vegetation → (4) ammonification lixiviate → (5) solid-liquor separation → (6) and must operate liquid → (7) containing Zn100-150g/l through multistage lixiviate and send after conventional purification and be electrolyzed to produce zinc ingot metal or produce zinc oxide product.
CN1414121A discloses a kind of method processing low grade zinc oxide ore, adopt alkali leaching-electrodeposition process flow process output metal zinc or hydrolytic precipitation output oxide powder and zinc, be particularly suitable for processing the low grade zinc oxide ore containing Zn < 20%, with the NaOH aqueous solution as leaching ore deposit agent, the zinc in ore is made to enter solution with sodium zincate, plumbous as precipitation using the aqueous solution of Na2S, copper, the contamination precipitation agent such as cadmium, make lead, copper, cadmium, manganese, iron, the impurity element such as calcium and most of silicon remains in slag, realize zinc and magazins' layout, it is low that this technical process has processing temperature, energy consumption is low, simplify clean liquid operation, the advantage that flow process shortens, thus can fully effectively utilize zinc resource leaved for development.
But for low-grade zinc oxide ore, the effect of above-mentioned treatment process is unsatisfactory, mainly because acid consumption is large, impurity is many, zinc concentration is low, leach liquor is difficult to process, therefore low-grade zinc oxide ore is never well utilized.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is the hydrometallurgical processes providing a kind of low-grade zinc oxide ore.Described technique adopts two sections of leachings, and the leaching yield of Zn can reach 92% ~ 95%, and the leaching of impurity Cu, Fe, Si, Al is effectively suppressed, and the technique of leach liquor P204 extracting zinc, zinc strip liquor electrodeposition can production high-quality electricity zinc.Technique acid consumption is low, impurity is few, zinc concentration is high, leach liquor is easy to process, and income is high.Technique acid consumption is low, impurity is few, zinc concentration is high, leach liquor is easy to process, and income is high.
The technical solution used in the present invention is:
A hydrometallurgical processes for low-grade zinc oxide ore, described zinc oxide ore containing zinc grade 5-20% be comprise the following steps:
Zinc oxide ore first passes through fragmentation and ore grinding;
Ore pulp delivers to meutral innersion;
After the dense filtration of ore pulp after leaching, leached mud carries out second segment leaching, i.e. acidic leaching; Some limestone powders can be added after leaching terminates pH value is adjusted to 2 refilter; After slurry filtration, acid leaching solution returns meutral innersion, can discharge after leached mud washing;
Meutral innersion liquid sends into extraction process; Raffinate part returns leaching, and part is as leached mud wash water, and wash water can return leaching;
Can more than 90g/L be reached containing Zn in zinc strip liquor, before power transmission is amassed, first will carry out oily water separation reclaim the organism carried secretly in solution, then with remaining micro-content organism in activity charcoal powder absorption removing solution to eliminate the impact of organism on Zinc electrolysis; Electrodeposition waste liquid returns reextraction section, and part delivers to leaching operation;
Its major technique condition is as follows:
(1) broken, ore grinding
Crumbling method: two sections of open circuits; Particle size after cracking: <20mm; Grinding particle size :-0.074mm accounts for 40-50%; Deliver to the pulp density of leaching vat: 50-60%
(2) meutral innersion
Extraction temperature: 30-40 DEG C; Extraction time: 1 hour; Gu liquid/than: 3-4/1; Leach endpoint pH: 5.2-5.4;
(3) acidic leaching
Extraction temperature: 80-85 DEG C; Extraction time: 1 hour; Gu liquid/than: 2-3/1; Endpoint pH: 1-1.5;
(4) extract
Material liquid component: Zn25-30g/L, pH5.2-5.5; Organic phase concentration: 30-50%(v/v) P204+260# kerosene;
Progression: 10 grades; Wherein, extraction section 3 grades, washing section 3 grades, stripping section 2 grades, washes Fe section 1 grade, washes Cl
-section 1 grade;
Compare (O/A): extraction section 2-3/1, washing section 8-10/1, stripping section 2-4/1, wash Fe section internal recycle, wash Cl
-section internal recycle;
Washings: 10-20g/L sulfuric acid;
Strip liquor: waste electrolyte is containing Zn30-50g/L, sulfur acid 130-140g/L;
(5) Zinc electrolysis
Current density: 300-500A/m2; Same pole span: 80mm; Bath voltage: about 3.3V; Anode: Pb-Ag-Ca-Sr; Negative electrode Al plate; Electrolyte temperature: 35-40 DEG C; The new liquid of electrolysis: Zn>90g/L; Electrolysis waste solution is containing Zn30-50g/L, sulfur acid 130-140g/L.
Below lower detailed description is carried out to the present invention:
Zinc oxide ore first passes through fragmentation and ore grinding, and this ore deposit belongs to easy ore grinding, and grinding particle size reaches 0.074mm and accounts for 40-50%.Ore pulp delivers to meutral innersion, this ore is easy to leach, but it is favourable for improving extraction temperature to the leaching suppressing SiO2, extraction time is 1 hour, endpoint pH controls at 5.2-5.4, Fe and SiO2 under these conditions in leach liquor can remain on lower concentration, and this operation for extraction process is favourable.After the dense filtration of ore pulp after leaching, leached mud carries out second segment leaching, i.e. acidic leaching, extraction temperature 80-85 DEG C, and 1 hour time, endpoint pH controls at 1-1.5.Some limestone powders can be added after leaching terminates pH value is adjusted to 2 refilter, the content of Fe in acid leaching solution can be reduced so on the one hand, also can improve filtration velocity on the other hand.After slurry filtration, acid leaching solution returns meutral innersion, can discharge after leached mud washing.
Meutral innersion liquid sends into extraction process, and extraction agent is certain density P204, and thinner is 260# kerosene.Extraction process adopt 3 grades of extractions, 3 grades of washings, 2 grades of back extractions, 1 grade wash Fe, wash Cl for 1 grade
-, totally 10 grades.Extraction agent can not saponification in advance, can save saponification alkali like this, greatly reduce production cost.Raffinate part returns leaching, and part is as leached mud wash water, and wash water can return leaching, and neutralisation also can be adopted to reclaim.
Can more than 90g/L be reached containing Zn in zinc strip liquor, before power transmission is amassed, first will carry out oily water separation reclaim the organism carried secretly in solution, then with remaining micro-content organism in activity charcoal powder absorption removing solution to eliminate the impact of organism on Zinc electrolysis.Zinc electrolysis anode adopts Pb-Ag-Ca-Sr quad alloy, and negative electrode is A1 plate, and current density controls at 300-500A/m
2, electrodeposition waste liquid returns reextraction section, and part is delivered to leaching operation and opened a way to make the impurity in electrolytic solution.
Its major technique condition is as follows:
(1) broken, ore grinding
Crumbling method: two sections of open circuits; Particle size after cracking: <20mm; Grinding particle size :-0.074mm accounts for 40-50%; Deliver to the pulp density of leaching vat: 50-60%
(2) meutral innersion
Extraction temperature: 30-40 DEG C; Extraction time: 1 hour; Gu liquid/than: 3-4/1; Leach endpoint pH: 5.2-5.4;
(3) acidic leaching
Extraction temperature: 80-85 DEG C; Extraction time: 1 hour; Gu liquid/than: 2-3/1; Endpoint pH: 1-1.5;
(4) extract
Material liquid component: Zn25-30g/L, pH5.2-5.5; Organic phase concentration: 30-50%(v/v) P204+260# kerosene;
Progression: 10 grades; Wherein, extraction section 3 grades, washing section 3 grades, stripping section 2 grades, washes Fe section 1 grade, washes Cl
-section 1 grade;
Compare (O/A): extraction section 2-3/1, washing section 8-10/1, stripping section 2-4/1, wash Fe section internal recycle, wash Cl
-section internal recycle;
Washings: 10-20g/L sulfuric acid;
Strip liquor: waste electrolyte is containing Zn30-50g/L, sulfur acid 130-140g/L;
(5) Zinc electrolysis
Current density: 300-500A/m2; Same pole span: 80mm; Bath voltage: about 3.3V; Anode: Pb-Ag-Ca-Sr; Negative electrode Al plate; Electrolyte temperature: 35-40 DEG C; The new liquid of electrolysis: Zn>90g/L; Electrolysis waste solution is containing Zn30-50g/L, sulfur acid 130-140g/L.
The present invention has the following advantages: described technique adopts two sections of leachings, the leaching yield of Zn can reach 92% ~ 95%, the leaching of impurity Cu, Fe, Si, Al is effectively suppressed, and the technique of leach liquor P204 extracting zinc, zinc strip liquor electrodeposition can production high-quality electricity zinc.Technique acid consumption is low, impurity is few, zinc concentration is high, leach liquor is easy to process, and income is high.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment one
A hydrometallurgical processes for low-grade zinc oxide ore, described zinc oxide ore containing zinc grade 5-20% be comprise the following steps:
Zinc oxide ore first passes through fragmentation and ore grinding;
Ore pulp delivers to meutral innersion;
After the dense filtration of ore pulp after leaching, leached mud carries out second segment leaching, i.e. acidic leaching; Some limestone powders can be added after leaching terminates pH value is adjusted to 2 refilter; After slurry filtration, acid leaching solution returns meutral innersion, can discharge after leached mud washing;
Meutral innersion liquid sends into extraction process; Raffinate part returns leaching, and part is as leached mud wash water, and wash water can return leaching;
Can more than 90g/L be reached containing Zn in zinc strip liquor, before power transmission is amassed, first will carry out oily water separation reclaim the organism carried secretly in solution, then with remaining micro-content organism in activity charcoal powder absorption removing solution to eliminate the impact of organism on Zinc electrolysis; Electrodeposition waste liquid returns reextraction section, and part delivers to leaching operation;
Its major technique condition is as follows:
(1) broken, ore grinding
Crumbling method: two sections of open circuits; Particle size after cracking: <20mm; Grinding particle size :-0.074mm accounts for 40-50%; Deliver to the pulp density of leaching vat: 50-60%
(2) meutral innersion
Extraction temperature: 30-40 DEG C; Extraction time: 1 hour; Gu liquid/than: 3-4/1; Leach endpoint pH: 5.2-5.4;
(3) acidic leaching
Extraction temperature: 80-85 DEG C; Extraction time: 1 hour; Gu liquid/than: 2-3/1; Endpoint pH: 1-1.5;
(4) extract
Material liquid component: Zn25-30g/L, pH5.2-5.5; Organic phase concentration: 30-50%(v/v) P204+260# kerosene;
Progression: 10 grades; Wherein, extraction section 3 grades, washing section 3 grades, stripping section 2 grades, washes Fe section 1 grade, washes Cl
-section 1 grade;
Compare (O/A): extraction section 2-3/1, washing section 8-10/1, stripping section 2-4/1, wash Fe section internal recycle, wash Cl
-section internal recycle;
Washings: 10-20g/L sulfuric acid;
Strip liquor: waste electrolyte is containing Zn30-50g/L, sulfur acid 130-140g/L;
(5) Zinc electrolysis
Current density: 300-500A/m2; Same pole span: 80mm; Bath voltage: about 3.3V; Anode: Pb-Ag-Ca-Sr; Negative electrode Al plate; Electrolyte temperature: 35-40 DEG C; The new liquid of electrolysis: Zn>90g/L; Electrolysis waste solution is containing Zn30-50g/L, sulfur acid 130-140g/L.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (6)
1. a hydrometallurgical processes for low-grade zinc oxide ore, described zinc oxide ore containing zinc grade 5-20% be comprise the following steps:
Zinc oxide ore first passes through fragmentation and ore grinding;
Ore pulp delivers to meutral innersion;
After the dense filtration of ore pulp after leaching, leached mud carries out second segment leaching, i.e. acidic leaching; Some limestone powders can be added after leaching terminates pH value is adjusted to 2 refilter; After slurry filtration, acid leaching solution returns meutral innersion, can discharge after leached mud washing;
Meutral innersion liquid sends into extraction process; Raffinate part returns leaching, and part is as leached mud wash water, and wash water can return leaching;
Can more than 90g/L be reached containing Zn in zinc strip liquor, before power transmission is amassed, first will carry out oily water separation reclaim the organism carried secretly in solution, then with remaining micro-content organism in activity charcoal powder absorption removing solution to eliminate the impact of organism on Zinc electrolysis; Electrodeposition waste liquid returns reextraction section, and part delivers to leaching operation.
2. technique according to claim 1: wherein, broken, griding technology is: crumbling method: two sections of open circuits; Particle size after cracking: <20mm; Grinding particle size :-0.074mm accounts for 40-50%; Deliver to the pulp density of leaching vat: 50-60%.
3. technique according to claim 1: wherein, meutral innersion technique is: extraction temperature: 30-40 DEG C; Extraction time: 1 hour; Gu liquid/than: 3-4/1; Leach endpoint pH: 5.2-5.4.
4. technique according to claim 1: wherein, acidic leaching technique is: extraction temperature: 80-85 DEG C; Extraction time: 1 hour; Gu liquid/than: 2-3/1; Endpoint pH: 1-1.5.
5. technique according to claim 1: wherein, extraction process is: material liquid component: Zn25-30g/L, pH5.2-5.5; Organic phase concentration: 30-50%(v/v) P204+260# kerosene;
Progression: 10 grades; Wherein, extraction section 3 grades, washing section 3 grades, stripping section 2 grades, washes Fe section 1 grade, washes Cl
-section 1 grade;
Compare (O/A): extraction section 2-3/1, washing section 8-10/1, stripping section 2-4/1, wash Fe section internal recycle, wash Cl
-section internal recycle;
Washings: 10-20g/L sulfuric acid;
Strip liquor: waste electrolyte is containing Zn30-50g/L, sulfur acid 130-140g/L.
6. technique according to claim 1: wherein, Zinc electrolysis technique is: current density: 300-500A/m2; Same pole span: 80mm; Bath voltage: about 3.3V; Anode: Pb-Ag-Ca-Sr; Negative electrode Al plate; Electrolyte temperature: 35-40 DEG C; The new liquid of electrolysis: Zn>90g/L; Electrolysis waste solution is containing Zn30-50g/L, sulfur acid 130-140g/L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104911630A (en) * | 2015-05-11 | 2015-09-16 | 北京工业大学 | Low bath voltage zinc electrolysis method |
| CN107326197A (en) * | 2017-08-17 | 2017-11-07 | 长兴上拓环境科技有限公司 | A kind of germanic strip liquor alkali recovery process of zinc abstraction |
| CN108554618A (en) * | 2018-04-26 | 2018-09-21 | 昆明理工大学 | A kind of beneficiation method of copper/lead/zinc ore |
| CN108842073A (en) * | 2018-06-01 | 2018-11-20 | 青海华信环保科技有限公司 | A kind of method of alkaline process processing zinc cadmium slag |
| CN112522514A (en) * | 2020-11-17 | 2021-03-19 | 陕西三秦环保科技股份有限公司 | Copper-containing etching solution recycling treatment system and method |
| CN114906871A (en) * | 2022-06-08 | 2022-08-16 | 桂林理工大学 | Method for preparing nano zinc oxide by using secondary zinc oxide |
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2013
- 2013-06-14 CN CN201310239220.5A patent/CN104232890A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104911630A (en) * | 2015-05-11 | 2015-09-16 | 北京工业大学 | Low bath voltage zinc electrolysis method |
| CN107326197A (en) * | 2017-08-17 | 2017-11-07 | 长兴上拓环境科技有限公司 | A kind of germanic strip liquor alkali recovery process of zinc abstraction |
| CN108554618A (en) * | 2018-04-26 | 2018-09-21 | 昆明理工大学 | A kind of beneficiation method of copper/lead/zinc ore |
| CN108842073A (en) * | 2018-06-01 | 2018-11-20 | 青海华信环保科技有限公司 | A kind of method of alkaline process processing zinc cadmium slag |
| CN108842073B (en) * | 2018-06-01 | 2020-11-03 | 青海华信环保科技有限公司 | Method for treating zinc-cadmium slag by alkaline process |
| CN112522514A (en) * | 2020-11-17 | 2021-03-19 | 陕西三秦环保科技股份有限公司 | Copper-containing etching solution recycling treatment system and method |
| CN114906871A (en) * | 2022-06-08 | 2022-08-16 | 桂林理工大学 | Method for preparing nano zinc oxide by using secondary zinc oxide |
| CN114906871B (en) * | 2022-06-08 | 2023-05-26 | 桂林理工大学 | Method for preparing nano zinc oxide by using secondary zinc oxide |
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Application publication date: 20141224 |