CN106868304A - A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum - Google Patents

A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum Download PDF

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Publication number
CN106868304A
CN106868304A CN201611224595.4A CN201611224595A CN106868304A CN 106868304 A CN106868304 A CN 106868304A CN 201611224595 A CN201611224595 A CN 201611224595A CN 106868304 A CN106868304 A CN 106868304A
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China
Prior art keywords
scum
zinc
iron
impurity content
autoclave
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Inventor
张向阳
倪恒发
张新庄
杨腾蛟
张文科
孔金换
张阳
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YUGUANG ZINC INDUSTRY Co Ltd HENAN
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YUGUANG ZINC INDUSTRY Co Ltd HENAN
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • C22B19/20Obtaining zinc otherwise than by distilling
    • C22B19/26Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Paper (AREA)

Abstract

The present invention relates to a kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum, using the solubility of the zinc sulfate principle that solubility with temperature is raised and reduced more than 60 DEG C, in oxydrolysis iron removal mixing scum is obtained using low temperature conditions, reduce the crystallization of zinc in iron removal, the content of zinc in scum is consequently reduced, limitation of the existing method for removing iron to the concentration of zinc ion in iron content solution of zinc sulfate is overcome;Will mixing scum with it is neutral or after sizing mixing containing acid producing waste water it is continuous, be quantitatively adding in autoclave, siderotil, ferric subsulfate, goethite react and are converted into iron oxide at high temperature, the soluble sulphate reacted in the soluble sulphate and former mixing scum for producing is dissolved in the water, obtain the low oxidation scum of impurity content, iron oxide cinder grade is correspondingly improved, while produce waste water being recycled.

Description

A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum
Technical field
Zinc hydrometallurgy is reduced the invention belongs to zinc hydrometallurgy impurity removing technology field, more particularly to a kind of combination using high/low temperature The method of impurity content in oxidation scum.
Background technology
Hematite process is except the main method of iron, hematite precipitation process from zinc hydrometallurgy iron content solution of zinc sulfate except iron In can form siderotil(Autunezite, sodium jarosite, hydration siderotil etc.), ferric subsulfate, the impurity such as goethite, simultaneously because sulphur The solubility of sour zinc solubility with temperature more than 60 DEG C is raised and reduced, under the reaction condition of existing method for removing iron(Temperature Degree is at 180 DEG C or so)Zinc sulfate solubility is less than 110g/L, and substantial amounts of zinc sulfate crystallization is mixed into scum, causes produced oxidation Zn, K, Na, S content are high in scum, and the later use to iron oxide is unfavorable.
The method of conventional reduction impurity content includes at present:(1)Impurity is decomposed by high-temperature calcination and remove, but should There is high energy consumption, low-concentration sulfur dioxide in method;(2)It is lowered into the iron content solution of zinc sulfate of iron removal system The concentration of middle zinc ion, it is to avoid zinc sulfate crystallization at high temperature, but the method limitation is larger, because of the iron content of zinc hydrometallurgy output It is higher than 110g/L that solution of zinc sulfate is most of containing zinc, need to be taken measures(Adjusting process is diluted with water)Strict control iron content sulfuric acid The concentration of zinc ion in zinc solution, high cost, difficulty is big, and because K, Na content are high in iron content solution of zinc sulfate solution, iron K, Na in alum are difficult to enter solution, and K, Na content are high in causing oxidation scum.
The content of the invention
It is an object of the invention to solve prior art zinc hydrometallurgy hematite process except the oxidation scum impurity that iron is produced contains Amount it is high and it is existing reduce the undesirable problem of impurity content in oxidation scum, and providing a kind of reduces zinc hydrometallurgy oxidation scum The method of impurity content, using the solubility of the zinc sulfate principle that solubility with temperature is raised and reduced more than 60 DEG C, in oxygen Obtain mixing scum using low temperature conditions in change hydrolysis iron removal, reduce the crystallization of zinc in iron removal, subtract accordingly Lack the content of zinc in scum, overcome limitation of the existing method for removing iron to the concentration of zinc ion in iron content solution of zinc sulfate;Will Mixing scum with it is neutral or after being sized mixing containing acid producing waste water it is continuous, be quantitatively adding in autoclave, siderotil, alkali formula sulfuric acid at high temperature Iron, goethite react and are converted into iron oxide, react the soluble sulphur in the soluble sulphate and former mixing scum for producing Hydrochlorate is dissolved in the water, and obtains the low oxidation scum of impurity content, has been correspondingly improved iron oxide cinder grade, while producing waste water Recycled.
The technical solution adopted in the present invention is:
A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum, comprises the following steps:
Step 1), will contain in ferrous solution of zinc sulfate and it is rear add except carrying out low-temperature oxidation hydrolysis in iron autoclave except iron, Temperature control forms the mixture of iron oxide and goethite at 120-150 DEG C, by mixture cooling, is filtrated to get mixing scum With nonferrous solution of zinc sulfate;
Step 2), by step 1)In the mixing scum that obtains and water add surge tank to be made into the ore pulp that mass ratio is 5-20%, be used in combination It is steam heated to 80-95 DEG C;
Step 3), by step 2)In the ore pulp that obtains is continuous, be quantitatively adding removal of impurities autoclave in carry out removal of impurities, be passed through compressed air Or nitrogen, temperature control discharges autoclave at 180-230 DEG C after the completion of reaction;
Step 4), be separated by filtration, by step 3)Filtration system is sent into after the ore pulp cooling of middle discharge autoclave to be separated by filtration, Obtain impure low oxidation scum, filtrate return system.
Further improve, step 1) in containing zinc ion concentration in ferrous solution of zinc sulfate be 140-180g/L.
Further improve, step 1) in low-temperature oxidation hydrolysis iron removal in, partial pressure of oxygen is 0.1-0.3MPa, time 1- 3h。
Further improve, step 2) in used water of sizing mixing for neutral or containing acid producing waste water.
Further improve, step 3) in dedoping step, it is higher than the corresponding saturated vapour pressure of reaction temperature to keep kettle pressure 0.1-0.3MPa, reaction time 0.5-3h.
The beneficial effects of the present invention are:
1., using the solubility of the zinc sulfate principle that solubility with temperature is raised and reduced more than 60 DEG C, iron is removed in oxydrolysis During obtain mixing scum using low temperature conditions, the crystallization of zinc in iron removal is reduced, in consequently reducing scum The content of zinc, overcomes limitation of the existing method for removing iron to the concentration of zinc ion in iron content solution of zinc sulfate;
2. by scum with it is neutral or after sizing mixing containing acid producing waste water it is continuous, be quantitatively adding in autoclave, siderotil, alkali formula at high temperature Ferric sulfate, goethite react and are converted into iron oxide, solvable in the soluble sulphate of reaction generation and former mixing scum Property sulfate be dissolved in the water, reduce oxidation scum in impurity content, be correspondingly improved the purpose of iron oxide cinder grade, together When production waste water recycled;
3. energy consumption is low, do not produce sulfur dioxide compared with conventional direct high-temperature calcination method.
The method of impurity content is with miscellaneous in reduction scum in a kind of reduction zinc hydrometallurgy oxidation scum that the present invention is provided The content of matter, overcomes limitation of the existing method for removing iron to the concentration of zinc ion in iron content solution of zinc sulfate, improves iron oxide Cinder grade, and environmental protection advantage.
Brief description of the drawings
The technological process of the method for impurity content is shown in a kind of reduction zinc hydrometallurgy oxidation scum that Fig. 1 is provided for the present invention It is intended to.
Specific embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1:A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum, comprises the following steps:
Step 1), by 15g/L containing ferrous iron, in the solution of zinc sulfate containing zinc 180g/L and it is rear add it is low except being carried out in iron autoclave Warm oxydrolysis removes iron, and 120 DEG C of reaction temperature, partial pressure of oxygen 0.1MPa, time 1h form the mixture of iron oxide and goethite, A small amount of solvable sulfate containing the impurity such as a small amount of ferric subsulfate, siderotil and entrainment in mixture, by mixture cooling, filters To mixing scum and nonferrous solution of zinc sulfate;
Step 2), by step 1)In the mixing scum that obtains add surge tank to be made into the ore pulp of mass ratio 5% with water, and use steam 85 DEG C are heated to, water used can be realized useless using neutrality or containing acid producing waste water, in the present embodiment using cooling tower sewer Water circulation use;
Step 3), by step 2)In the ore pulp that obtains is continuous, be quantitatively adding removal of impurities autoclave in carry out removal of impurities, reaction temperature 180 DEG C, time 3h is passed through compressed air, and it is higher than the corresponding saturated vapour pressure of reaction temperature to keep kettle pressure(1.0MPa)0.3MPa, instead Autoclave is discharged after the completion of answering, autunezite, sodium jarosite, hydration siderotil, ferric subsulfate, goethite occur such as during being somebody's turn to do Lower reaction is converted into iron oxide, and chemical principle is as follows:
Soluble sulphate dissolving in the soluble sulphate generated in above-mentioned reaction and former mixing scum enters in water;
Step 4), be separated by filtration, by step 3)The ore pulp cooling feeding filtration system of middle discharge autoclave is separated by filtration, and is obtained It is to oxidation scum composition:Containing zinc 0.49%, sulphur 0.45%, potassium 0.006%, sodium 0.005%, iron 64%, filtrate returns to zinc hydrometallurgy system System, recycles.
Embodiment 2:A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum, comprises the following steps;
Step 1), by 20g/L containing ferrous iron, in the solution of zinc sulfate containing zinc 140g/L and it is rear add it is low except being carried out in iron autoclave Warm oxydrolysis removes iron, and 150 DEG C of reaction temperature, partial pressure of oxygen 0.2MPa, time 3h form the mixture of iron oxide and goethite, A small amount of solvable sulfate containing the impurity such as a small amount of ferric subsulfate, siderotil and entrainment in mixture, by mixture cooling, filters To mixing scum and nonferrous solution of zinc sulfate;
Step 2), by step 1)In electrolytic zinc in the mixing scum that obtains and Zinc Hydrometallurgy Process scald groove water and add surge tank It is made into the ore pulp of mass ratio 10%, and with being steam heated to 90 DEG C;Water used can be using neutrality or containing acid producing waste water, in this reality Apply in example and groove water is scalded using the electrolytic zinc in Zinc Hydrometallurgy Process, realize cycling utilization of wastewater;
Step 3), by step 2)In the ore pulp that obtains is continuous, be quantitatively adding removal of impurities autoclave in carry out removal of impurities, reaction temperature 200 DEG C, time 2h is passed through nitrogen, and it is higher than the corresponding saturated vapour pressure of reaction temperature to keep kettle pressure(1.55MPa)0.2MPa, has reacted Into rear discharge autoclave, autunezite, sodium jarosite, hydration siderotil, ferric subsulfate, goethite react and turn during being somebody's turn to do Iron oxide is turned to, reaction principle is in the same manner as in Example 1, in the soluble sulphate generated in above-mentioned reaction and former mixing scum Soluble sulphate dissolving enter water in;
Step 4), be separated by filtration, by step 3)The ore pulp cooling feeding filtration system of middle discharge autoclave is separated by filtration, and is obtained It is to oxidation scum composition:Containing zinc 0.42%, sulphur 0.47%, potassium 0.005%, sodium 0.004%, iron 63%, filtrate returns to zinc hydrometallurgy system System, recycles.
A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum of embodiment 3, comprises the following steps;
Step 1), by 30g/L containing ferrous iron, in the solution of zinc sulfate containing zinc 160g/L and it is rear add it is low except being carried out in iron autoclave Warm oxydrolysis removes iron, 140 DEG C of reaction temperature, partial pressure of oxygen 0.3MPa, time 1.5h, the mixing of formation iron oxide and goethite Thing, a small amount of solvable sulfate containing the impurity such as a small amount of ferric subsulfate, siderotil and entrainment in mixture, by mixture cooling, mistake Filter obtains mixing scum and nonferrous solution of zinc sulfate;
Step 2), by step 1)In the mixing scum that obtains add surge tank to be made into the lead smelting gas wash water in Zinc Hydrometallurgy Process The ore pulp of mass ratio 20%, and with being steam heated to 95 DEG C;Water used can be using neutrality or containing acid producing waste water, in the present embodiment Lead smelting gas wash water in middle use Zinc Hydrometallurgy Process, realizes cycling utilization of wastewater;
Step 3), by step 2)In the ore pulp that obtains is continuous, be quantitatively adding removal of impurities autoclave in carry out removal of impurities, reaction temperature 230 DEG C, time 0.5h is passed through nitrogen, and it is higher than the corresponding saturated vapour pressure of reaction temperature to keep kettle pressure(About 2.80MPa)0.1MPa, instead Autoclave is discharged after the completion of answering, autunezite, sodium jarosite, hydration siderotil, ferric subsulfate, goethite occur anti-during being somebody's turn to do Iron oxide should be converted into, specific reaction principle is such as embodiment 1, the soluble sulphate generated in above-mentioned reaction and former mixing iron Soluble sulphate dissolving in slag enters in water;
Step 4), be separated by filtration, by step 3)The ore pulp cooling feeding filtration system of middle discharge autoclave is separated by filtration, and is obtained It is to oxidation scum composition:Containing zinc 0.44%, sulphur 0.40%, potassium 0.004%, sodium 0.005%, iron 65%, filtrate returns to zinc hydrometallurgy system System, recycles.
Specific embodiment more than can be seen that a kind of of present invention offer and reduce miscellaneous in zinc hydrometallurgy oxidation scum The method of matter content is hydrolyzed by low-temperature oxidation and removes two operations of iron and removal of impurities, greatly reduces impurity content in iron oxide, phase That answers improves the grade of oxidation scum, at the same produce waste water to recycling, with reduction impurity content conventional at present Method is compared and the zinc ion of iron content solution of zinc sulfate need not be limited, therefore existing smelting process need not be improved, adjusted, together When do not produce sulfur dioxide, energy consumption low.

Claims (5)

1. it is a kind of to reduce the method that zinc hydrometallurgy aoxidizes impurity content in scum, it is characterised in that to comprise the following steps:
Step 1), will contain in ferrous solution of zinc sulfate and it is rear add except carrying out low-temperature oxidation hydrolysis in iron autoclave except iron, Temperature control forms the mixture of iron oxide and goethite at 120-150 DEG C, by mixture cooling, is filtrated to get mixing scum With nonferrous solution of zinc sulfate;
Step 2), by step 1)In the mixing scum that obtains and water add surge tank to be made into the ore pulp that mass ratio is 5-20%, be used in combination It is steam heated to 80-95 DEG C;
Step 3), by step 2)In the ore pulp that obtains is continuous, be quantitatively adding removal of impurities autoclave in carry out removal of impurities, temperature control exists 180-230 DEG C, compressed air or nitrogen are passed through, autoclave is discharged after the completion of reaction;
Step 4), be separated by filtration, by step 3)Filtration system is sent into after the ore pulp cooling of middle discharge autoclave to be separated by filtration, Obtain impure low oxidation scum, filtrate return system.
2. the method that a kind of reduction zinc hydrometallurgy according to claim 1 aoxidizes impurity content in scum, it is characterised in that Step 1) in containing zinc ion concentration in ferrous solution of zinc sulfate be 140-180g/L.
3. the method that a kind of reduction zinc hydrometallurgy according to claim 1 aoxidizes impurity content in scum, it is characterised in that Step 1) in low-temperature oxidation hydrolysis iron removal in, partial pressure of oxygen is 0.1-0.3MPa, time 1-3h.
4. the method that a kind of reduction zinc hydrometallurgy according to claim 1 aoxidizes impurity content in scum, it is characterised in that Step 2) in used water of sizing mixing for neutral or containing acid producing waste water.
5. the method that a kind of reduction zinc hydrometallurgy according to claim 1 aoxidizes impurity content in scum, it is characterised in that Step 3) in dedoping step, the kettle pressure for keeping autoclave is higher than the corresponding saturated vapour pressure 0.1-0.3MPa of reaction temperature, instead 0.5-3h between seasonable.
CN201611224595.4A 2016-12-27 2016-12-27 A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum Pending CN106868304A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107312930A (en) * 2017-07-07 2017-11-03 金川集团股份有限公司 A kind of low nickel matte leaching solution pyrolysis is except the method for iron
CN109607622A (en) * 2019-01-03 2019-04-12 昆明理工大学 A method of iron oxide red product is prepared using the heavy scum of zinc hydrometallurgy hematite process
AU2018319218B2 (en) * 2018-02-01 2020-07-09 Korea Zinc Co., Ltd. Method of recovering iron from zinc sulphate solution
CN111748690A (en) * 2020-07-30 2020-10-09 中南大学 Method for purifying and deironing hydrometallurgy leaching solution based on hydrothermal lattice transformation

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107312930A (en) * 2017-07-07 2017-11-03 金川集团股份有限公司 A kind of low nickel matte leaching solution pyrolysis is except the method for iron
AU2018319218B2 (en) * 2018-02-01 2020-07-09 Korea Zinc Co., Ltd. Method of recovering iron from zinc sulphate solution
US11001507B2 (en) 2018-02-01 2021-05-11 Korea Zinc Co., Ltd. Method of recovering iron from zinc sulphate solution
CN109607622A (en) * 2019-01-03 2019-04-12 昆明理工大学 A method of iron oxide red product is prepared using the heavy scum of zinc hydrometallurgy hematite process
CN111748690A (en) * 2020-07-30 2020-10-09 中南大学 Method for purifying and deironing hydrometallurgy leaching solution based on hydrothermal lattice transformation

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