CN109957656A - A kind of zinc hydrometallurgy iron vitriol slag recycling and the technique for recycling dilute scattered noble metal - Google Patents
A kind of zinc hydrometallurgy iron vitriol slag recycling and the technique for recycling dilute scattered noble metal Download PDFInfo
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- CN109957656A CN109957656A CN201910125729.4A CN201910125729A CN109957656A CN 109957656 A CN109957656 A CN 109957656A CN 201910125729 A CN201910125729 A CN 201910125729A CN 109957656 A CN109957656 A CN 109957656A
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- recycling
- vitriol slag
- iron
- iron vitriol
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- 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
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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to refuse reclamation technical fields, more particularly to a kind of zinc hydrometallurgy iron vitriol slag recycling and the technique for recycling dilute scattered noble metal, for solving energy consumption existing in the prior art and at high cost, the low disadvantage of recycling degree, the following steps are included: S1, the sodium hydroxide solution that iron vitriol slag and mass concentration are 5~15% be placed in stirred tank by 3~10:1 of liquid-solid ratio being mixed, the iron containing compounds based on iron hydroxide are converted by iron vitriol slag, filtration washing is divided into filter residue and filtrate；S2, the filtrate in step S1 is returned in step S1 conversion and cycle 2~3 times, the natural cooling after sodium sulfate concentration in filtrate reaches saturation, sodium sulfate crystal is precipitated, it refilters, obtain sodium sulphate product, filtrate is incorporated suitable sodium hydroxide after filtering sodium sulphate, and the concentration of the sodium hydroxide solution in step S1 in stirred tank is made to reach 5~15%.The present invention can be environmental-friendly by the iron vitriol slag high efficient resourcing of zinc hydrometallurgy output.
Description
Technical field
The present invention relates to refuse reclamation technical field more particularly to a kind of zinc hydrometallurgy iron vitriol slag recycling and recycle dilute
The technique for dissipating noble metal.
Background technique
In zinc abstraction industry, there are about 40 for the iron vitriol slag using hot acid leaching, the annual output of precipitating alum and removing iron technique domestic at present
Ten thousand tons.Iron vitriol slag is dangerous solid waste, and the iron vitriol slag of zinc smelting factory man output is mainly stored up at present, and iron vitriol slag is largely stored up for a long time
Environmental protection policy is not met, it is necessary to handle.
The prevailing technology of present alum Slag treatment not yet determines that main cause is that alum Slag treatment is at high cost.There is zinc abstraction at present
Producer selects pyrogenic attack, and there are three types of pyrogenic attack main techniques, is respectively as follows: bottom convertor+side-blown converter+fuming furnace and handles, is side-blown
Furnace+fuming furnace, Ausmelt furnace+fuming furnace treatment process.
And pyrogenic attack technique be primarily present it is following: autothermal reaction cannot occur for complex process, material, and smelting temperature is high
Energy consumption is high；Contain SO in flue gas2Concentration is low to be unable to relieving haperacidity, needs to handle, therefore processing difficulty is big；Sodium cannot recycle, and enter
In smelting slag；Iron resource degree is not high, in iron vitriol slag iron be changed into clinker can only as production cement raw material.To sum up institute
It states, pyrogenic attack iron vitriol slag is all energy consumption and at high cost, and recycling degree is low.
Summary of the invention
The purpose of the present invention is to solve energy consumption existing in the prior art and at high cost, recycling degree is low to be lacked
Point, and a kind of zinc hydrometallurgy iron vitriol slag recycling proposed and the technique for recycling dilute scattered noble metal.
The technical solution adopted in the present invention is as follows:
A kind of zinc hydrometallurgy iron vitriol slag recycling and the technique for recycling dilute scattered noble metal, comprising the following steps:
S1, the sodium hydroxide solution that iron vitriol slag and mass concentration are 5~15% is placed in stirred tank by 3~10:1 of liquid-solid ratio and is mixed
Stirring is closed, converts the iron containing compounds based on iron hydroxide for iron vitriol slag, filtration washing is divided into filter residue and filtrate；
S2, the filtrate in step S1 is returned in step S1 conversion and cycle 2~3 times, reaches full to sodium sulfate concentration in filtrate
With rear, natural cooling, sodium sulfate crystal is precipitated, refilters, obtains sodium sulphate product, filter filtrate after sodium sulphate and is incorporated appropriate
Sodium hydroxide, so that the mass concentration of the sodium hydroxide solution in step S1 in stirred tank is reached 5~15%；
S3, the filter residue in step S1 is mixed with the ammonium chloride solution of 3~6mol/L by 3~8:1 of liquid-solid ratio, is incorporated suitable fluorine
Changing hydrogen ammonium is completely dissolved the silicon matter in filter residue, and adding salt acid for adjusting pH value is 1~3, is then mixed, produces after solid-liquor separation
Raw ammonium chloride leached mud and ammonium chloride leachate；
S4, the ammonium chloride leached mud washing in step S3 is obtained into iron oxide red through drying, calcining, ball milling；
S5, when the indium in the ammonium chloride leachate in step S3 is enriched to 500mg/L or more, sheet lead or rolled tin displacement chlorine are first used
Change the silver in ammonium leachate, add metal medium and replace respectively and obtain argentalium alloy and indium slag, the ammonium chloride after displacement soaks
Liquid is returned in step S3 and is recycled out.
Preferably, it is 60~80 DEG C that mixing, which keeps temperature, in the S1, in stirred tank, and being stirred to react the time is 1~2h.
Preferably, in the S3, after adjusting pH value, 1~2h is stirred to react at a temperature of condition is 50~90 DEG C.
Preferably, in the S4, drying temperature is 100~150 DEG C, and calcination temperature is 700~900 DEG C.
Preferably, in the S5, metal medium is the one of which of lead, zinc or aluminium.
The present invention passes through wet process-pyrogenic process process integration for the valuable element recycling in iron vitriol slag.By the master in iron vitriol slag
Elemental iron, sulphur, sodium is wanted to be separately converted to iron oxide red and sodium sulphate；Noble metal and dissipated metal silver, indium in alum slag obtain
Preferable enriching and recovering.Wet process-pyrogenic process process integration processing iron vitriol slag and energy consumption is lower, it can be achieved that iron vitriol slag high efficient resourcing,
Cost is low with respect to pyrogenic attack iron vitriol slag, industrial hazard solid waste is converted to valuable resource, and production process pollution is small, environmental protection
Health solves the problems, such as that largely stockpiling does not meet environmental protection policy to iron vitriol slag for a long time instantly.Design layout of the present invention is reasonable, and operation is steady
It is fixed, can be and environmental-friendly effectively by the iron vitriol slag high efficient resourcing of zinc hydrometallurgy output, it is worthy to be popularized.
Detailed description of the invention
Fig. 1 be temperature be at 750 DEG C calcined oxide iron oxide red SEM figure；
Fig. 2 be temperature be at 850 DEG C calcined oxide iron oxide red SEM figure.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment one
Referring to Fig.1, a kind of zinc hydrometallurgy iron vitriol slag recycling proposed by the present invention and the technique of dilute scattered noble metal is recycled, including with
Lower step:
S1, the sodium hydroxide solution that iron vitriol slag and mass concentration are 12% is placed in stirred tank by liquid-solid ratio 3:1, mixing is kept
Temperature 60 C is stirred to react 1.5h, converts the iron containing compounds based on iron hydroxide for iron vitriol slag, filtration washing is divided into filter
Slag and filtrate；
S2, the filtrate in step S1 is returned in step S1 conversion and cycle 2 times, reaches saturation to sodium sulfate concentration in filtrate
Afterwards, natural cooling is precipitated sodium sulfate crystal, refilters, obtains sodium sulphate product, filters filtrate after sodium sulphate and is incorporated suitable
Sodium hydroxide makes the mass concentration of the sodium hydroxide solution in step S1 in stirred tank reach 12%；
S3, the filter residue in step S1 is mixed with the ammonium chloride solution of 6mol/L by liquid-solid ratio 3:1, is incorporated suitable ammonium acid fluoride
It is completely dissolved the silicon matter in filter residue, adding salt acid for adjusting pH value is 1.5, is then stirred to react at a temperature of condition is 60 DEG C
1.5h generates ammonium chloride leached mud and ammonium chloride leachate after solid-liquor separation；
S4, the ammonium chloride leached mud washing in step S3 is obtained through dry, 750 DEG C of temperature lower calcinations, ball millings at a temperature of 105 DEG C
Iron oxide red；
S5, when the indium in the ammonium chloride leachate in step S3 is enriched to 520mg/L, first with sheet lead displacement ammonium chloride leachate
In silver, displacement obtains argentalium alloy, and one of displacement for adding metallic zinc or aluminium obtains indium slag, the chlorination after displacement
Ammonium leachate is returned in step S3 and is recycled.
Embodiment two
Referring to Fig. 2, a kind of zinc hydrometallurgy iron vitriol slag recycling proposed by the present invention and the technique for recycling dilute scattered noble metal, including with
Lower step:
S1, it the sodium hydroxide solution that iron vitriol slag and mass concentration are 5% is placed in stirred tank by liquid-solid ratio 10:1 is mixed,
The iron containing compounds based on iron hydroxide are converted by iron vitriol slag, filtration washing is divided into filter residue and filtrate；
S2, the filtrate in step S1 is returned in step S1 conversion and cycle 3 times, reaches saturation to sodium sulfate concentration in filtrate
Afterwards, natural cooling is precipitated sodium sulfate crystal, refilters, obtains sodium sulphate product, filters filtrate after sodium sulphate and is incorporated suitable
Sodium hydroxide makes the mass concentration of the sodium hydroxide solution in step S1 in stirred tank reach 5%；
S3, the filter residue in step S1 is mixed with the ammonium chloride solution of 6mol/L by liquid-solid ratio 5:1, is incorporated suitable ammonium acid fluoride
It is completely dissolved the silicon matter in filter residue, adding salt acid for adjusting pH value is 2.0, is then stirred to react at a temperature of condition is 70 DEG C
1h generates ammonium chloride leached mud and ammonium chloride leachate after solid-liquor separation；
S4, the ammonium chloride leached mud washing in step S3 is obtained through dry, 850 DEG C of temperature lower calcinations, ball millings at a temperature of 105 DEG C
Iron oxide red；
S5, when the indium in the ammonium chloride leachate in step S3 is enriched to 550mg/L, the one of which of lead, zinc or aluminium is added
The silver in ammonium chloride leachate is replaced, displacement obtains argentalium alloy and indium slag respectively, and the ammonium chloride leachate after displacement returns
It is recycled into step S3.
The red chemical component of calcining iron oxide is analyzed as follows table:
| Project | Zn(%) | Fe(%) | Ca(%) | As(%) | Pb(%) | SiO2(%) | S(%) | Ag(g/t) | In(g/t) |
| 750 DEG C of calcining iron oxide reds | 0.32 | 59.82 | 0.88 | 0.06 | 0.2 | 3.52 | 0.35 | 7.74 | 35 |
| 850 DEG C of calcining iron oxide reds | 0.35 | 60.11 | 0.92 | 0.06 | 0.2 | 3.63 | 0.26 | 7.52 | 29 |
Essential element iron, sulphur, sodium in iron vitriol slag is separately converted to iron oxide red and sodium sulphate by the present invention；Your gold in alum slag
Belong to and dissipated metal silver, indium obtain preferable enriching and recovering.Wet process-pyrogenic process process integration handles iron vitriol slag and energy consumption is lower,
Iron vitriol slag high efficient resourcing can be achieved, cost is low with respect to pyrogenic attack iron vitriol slag, and industrial hazard solid waste is converted to valuable money
Source, and production process pollutes small, environmentally-friendly sanitary, solves the problems, such as that largely stockpiling does not meet environmental protection policy to iron vitriol slag for a long time instantly.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of zinc hydrometallurgy iron vitriol slag recycling and the technique for recycling dilute scattered noble metal, which comprises the following steps:
S1, the sodium hydroxide solution that iron vitriol slag and mass concentration are 5~15% is placed in stirred tank by 3~10:1 of liquid-solid ratio and is mixed
Stirring is closed, converts the iron containing compounds based on iron hydroxide for iron vitriol slag, filtration washing is divided into filter residue and filtrate；
S2, the filtrate in step S1 is returned in step S1 conversion and cycle 2~3 times, reaches full to sodium sulfate concentration in filtrate
With rear, natural cooling, sodium sulfate crystal is precipitated, refilters, obtains sodium sulphate product, filter filtrate after sodium sulphate and is incorporated appropriate
Sodium hydroxide, so that the mass concentration of the sodium hydroxide solution in step S1 in stirred tank is reached 5~15%；
S3, the filter residue in step S1 is mixed with the ammonium chloride solution of 3~6mol/L by 3~8:1 of liquid-solid ratio, is incorporated suitable fluorine
Changing hydrogen ammonium is completely dissolved the silicon matter in filter residue, and adding salt acid for adjusting pH value is 1~3, is then mixed, produces after solid-liquor separation
Raw ammonium chloride leached mud and ammonium chloride leachate；
S4, the ammonium chloride leached mud washing in step S3 is obtained into iron oxide red through drying, calcining, ball milling；
S5, when the indium in the ammonium chloride leachate in step S3 is enriched to 500mg/L or more, sheet lead or rolled tin displacement chlorine are first used
Change the silver in ammonium leachate, add metal medium and replace respectively and obtain argentalium alloy and indium slag, the ammonium chloride after displacement soaks
Liquid is returned in step S3 and is recycled out.
2. a kind of zinc hydrometallurgy iron vitriol slag recycling according to claim 1 and the technique for recycling dilute scattered noble metal, special
Sign is, it is 60~80 DEG C that mixing, which keeps temperature, in the S1, in stirred tank, and being stirred to react the time is 1~2h.
3. a kind of zinc hydrometallurgy iron vitriol slag recycling according to claim 1 and the technique for recycling dilute scattered noble metal, special
Sign is, in the S3, after adjusting pH value, is stirred to react 1~2h at a temperature of condition is 50~90 DEG C.
4. a kind of zinc hydrometallurgy iron vitriol slag recycling according to claim 1 and the technique for recycling dilute scattered noble metal, special
Sign is, in the S4, drying temperature is 100~150 DEG C, and calcination temperature is 700~900 DEG C.
5. a kind of zinc hydrometallurgy iron vitriol slag recycling according to claim 1 and the technique for recycling dilute scattered noble metal, special
Sign is, in the S5, metal medium is the one of which of lead, zinc or aluminium.
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| CN201910125729.4A CN109957656A (en) | 2019-05-21 | 2019-05-21 | A kind of zinc hydrometallurgy iron vitriol slag recycling and the technique for recycling dilute scattered noble metal |
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| CN201910125729.4A CN109957656A (en) | 2019-05-21 | 2019-05-21 | A kind of zinc hydrometallurgy iron vitriol slag recycling and the technique for recycling dilute scattered noble metal |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102443701A (en) * | 2010-10-12 | 2012-05-09 | 中国科学院过程工程研究所 | Clean metallurgic comprehensive utilization method of iron vitriol slags |
| CN103436706A (en) * | 2013-08-14 | 2013-12-11 | 河池市津泰资源再生有限公司 | Method for processing low-grade waste zinc slag to recover zinc, silver, lead and indium |
| CN105039712A (en) * | 2015-08-14 | 2015-11-11 | 陕西理工学院 | Technology for recycling valuable metal from jarosite slag |
| CN105385858A (en) * | 2015-11-03 | 2016-03-09 | 中南大学 | Method for preparing iron oxide red and recycling silver through ferroalumen residues |
| CN106745318A (en) * | 2016-11-28 | 2017-05-31 | 东北大学 | A kind of method of use iron vitriol slag one-step synthesis magnetic ferroferric oxide |
| CN107345274A (en) * | 2017-06-06 | 2017-11-14 | 云南云铜锌业股份有限公司 | It is a kind of that lead, silver, the method for indium are reclaimed from lead smelting gas |
| CN108285312A (en) * | 2018-04-02 | 2018-07-17 | 中钢集团马鞍山矿山研究院有限公司 | A kind of resource utilization method of zinc hydrometallurgy iron vitriol slag and sewage disposal sludge |
-
2019
- 2019-05-21 CN CN201910125729.4A patent/CN109957656A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102443701A (en) * | 2010-10-12 | 2012-05-09 | 中国科学院过程工程研究所 | Clean metallurgic comprehensive utilization method of iron vitriol slags |
| CN103436706A (en) * | 2013-08-14 | 2013-12-11 | 河池市津泰资源再生有限公司 | Method for processing low-grade waste zinc slag to recover zinc, silver, lead and indium |
| CN105039712A (en) * | 2015-08-14 | 2015-11-11 | 陕西理工学院 | Technology for recycling valuable metal from jarosite slag |
| CN105385858A (en) * | 2015-11-03 | 2016-03-09 | 中南大学 | Method for preparing iron oxide red and recycling silver through ferroalumen residues |
| CN106745318A (en) * | 2016-11-28 | 2017-05-31 | 东北大学 | A kind of method of use iron vitriol slag one-step synthesis magnetic ferroferric oxide |
| CN107345274A (en) * | 2017-06-06 | 2017-11-14 | 云南云铜锌业股份有限公司 | It is a kind of that lead, silver, the method for indium are reclaimed from lead smelting gas |
| CN108285312A (en) * | 2018-04-02 | 2018-07-17 | 中钢集团马鞍山矿山研究院有限公司 | A kind of resource utilization method of zinc hydrometallurgy iron vitriol slag and sewage disposal sludge |
Non-Patent Citations (1)
| Title |
|---|
| 陈永明 等: "NaOH分解含铟铁矾渣新工艺", 《中国有色金属学报》 * |
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