CN108467942A - A method of Selectively leaching zinc, lead, gallium and germanium from zinc replacement slag - Google Patents
A method of Selectively leaching zinc, lead, gallium and germanium from zinc replacement slag Download PDFInfo
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- CN108467942A CN108467942A CN201810150330.7A CN201810150330A CN108467942A CN 108467942 A CN108467942 A CN 108467942A CN 201810150330 A CN201810150330 A CN 201810150330A CN 108467942 A CN108467942 A CN 108467942A
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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
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
-
- 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
-
- 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
- C22B41/00—Obtaining germanium
-
- 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
-
- 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
Abstract
The present invention relates to a kind of methods of Selectively leaching zinc, lead, gallium and germanium in replacement slag from zinc comprising following steps:S1. by the levigate processing of zinc replacement slag, leaching process is carried out to it using deionized water, after the completion of leaching, is separated by solid-liquid separation to contain zinc lixiviating solution and water logging slag；S2. it uses dilute sulfuric acid to carry out leaching process to water logging slag, after the completion of leaching, is separated by solid-liquid separation to obtain leachate containing gallium and sulfuric acid leaching slag；S3. it uses hydrogen peroxide to carry out leaching process to sulfuric acid leaching slag, pH is adjusted with ammonium hydroxide when leaching, after the completion of leaching, is separated by solid-liquid separation to obtain germanic leachate and hydrogen peroxide leached mud；S4. it uses sodium hydroxide solution to carry out leaching process to hydrogen peroxide leached mud, after the completion of leaching, is separated by solid-liquid separation to obtain leaded leachate and leaching with sodium hydroxide slag.It has the beneficial effect that, realizes the efficient selective separation of zinc, gallium, germanium and lead；It is not introduced into F‑, equipment is corroded smaller；Process is simple, easily operated, and the gallium germanium rate of recovery is higher, advantageously reduces production cost.
Description
Technical field
The invention belongs to non-ferrous metal field of hydrometallurgy, and in particular to one kind from zinc replacement slag Selectively leaching zinc,
The method of lead, gallium and germanium.
Background technology
The gallium and germanium of high level are associated in the zinc sulfide concentrates of Southwestern China area output, using peracid oxygen leaching
When technique handles it, gallium and germanium enter infusion solution, and follow-up infusion solution is purified using zinc replacement, gallium and germanium
Enter in zinc replacement slag.In zinc replacement slag in addition to containing the higher gallium of added value and germanium, also the zinc containing high level and
The valuable metals such as lead.In general, zinc replacement slag has higher comprehensive utilization value.
Currently, accompanying element gallium and germanium are mainly recycled by the way of wet method in zinc concentrate, widely used leaching agent packet
Include sulfuric acid and sodium hydroxide.(the China YouSe Acta Metallurgica Sinica .2016 (04) such as Liu Fupeng:908-18) sulfuric acid is used to be tried as leaching
Agent obtains higher zinc, gallium and germanium leaching rate using sodium nitrate or calcium nitrate as auxiliary agent is leached.
CN201611256803.9, CN201710025733.4 propose to use H2SO4- HF leaches Ga and Ge as reagent is leached, and improves
The rate of recovery of Ga and Ge.Above-mentioned leaching process is although higher leaching efficiency can be obtained, since leaching process is in strong acid item
It is carried out under part, zinc, gallium and germanium enter infusion solution, and the processing of follow-up leachate need to pass through more complicated separation process.
CN201310468825.1 proposes to handle the metallurgical slag containing Ga and Ge in such a way that alkalinity is pressurizeed, under optimum process condition, Ga
Leaching rate with Ge is more than 98%.But required naoh concentration is higher in the above process, and subsequent recovery technical process needs to add
Enter a large amount of sulfuric acid and adjusts infusion solution pH to acidity, to recycle gallium and germanium.Simultaneously leaching process due to alkali concentration it is higher, leachate
Middle lead content is higher, and follow-up leachate, which needs to increase, takes off splicer's sequence.
Invention content
A kind of method that the present invention provides Selectively leaching zinc, lead, gallium and germanium in the replacement slag from zinc, it is intended to overcome such as background
When leaching the metallic elements such as gallium and germanium in the slave zinc replacement slag of technology segment introduction, present in prior art means it is many not
Foot.
The technical solution that the present invention solves above-mentioned technical problem is as follows：One kind from zinc replacement slag Selectively leaching zinc, lead,
The method of gallium and germanium comprising following steps:
S1. Leaching Zinc：By the levigate processing of zinc replacement slag, then under agitation, it is soaked using deionized water
Go out processing, after the completion of leaching, is separated by solid-liquid separation to contain zinc lixiviating solution and water logging slag；
S2. gallium is leached：Under agitation, leaching process is carried out to the water logging slag that S1 is obtained using dilute sulfuric acid, leached
Cheng Hou is separated by solid-liquid separation to obtain leachate containing gallium and sulfuric acid leaching slag；
S3. germanium is leached：Under agitation, sulfuric acid leaching slag is obtained to S2 using hydrogen peroxide and carries out leaching process, leached
When with the pH of ammonium hydroxide adjusting control infusion solution be 5.0~8.0, after the completion of leaching, be separated by solid-liquid separation to obtain germanic leachate and dioxygen
Water logging is slagged tap；
S4. lead is leached：Under agitation, the hydrogen peroxide leached mud that S3 is obtained is leached using sodium hydroxide solution
Processing, after the completion of leaching, is separated by solid-liquid separation to obtain leaded leachate and leaching with sodium hydroxide slag.
The chemical reaction that each step of the above method provided by the invention occurs is as follows.
The main chemical reactions equation that water Leaching Zinc occurs is as follows：
ZnSO4=Zn2++SO4 2- (1)
The main chemical reactions equation that sulfuric acid leaching gallium occurs is as follows：
2Ga+3H2SO4=Ga2(SO4)3+3H2 (2)
Ga2O3+3H2SO4=3H2O+Ga2(SO4)3 (3)
It is as follows that hydrogen peroxide leaches the primary chemical equation that germanium occurs：
Ge+2H2O2+2NH3=(NH4)2GeO3+H2O (4)
GeO+H2O2+2NH3=(NH4)2GeO3 (5)
GeO2+2NH3+H2O=(NH4)2GeO3 (6)
The main chemical reactions equation that leaching with sodium hydroxide lead occurs is as follows：
PbSO4+ 4NaOH=Na2SO4+Na2Pb(OH)4 (7)
Based on the above technical solution, the present invention can also have following further specific choice.
Specifically, the levigate processing in S1 refer to by zinc replacement slag it is levigate to granularity be 50~100 μm.
Specifically, the liquid-solid ratio of deionized water and zinc replacement slag is 4~10 in S1:1mL/g, extraction time be 0.25~
4h, extraction temperature are 25~40 DEG C.
Specifically, in S2 dilute sulfuric acid a concentration of 0.1~1mol/L.
Specifically, the liquid-solid ratio of dilute sulfuric acid and water logging slag is 4~10 in S2:1mL/g, extraction time are 0.25~4h, leaching
It is 25~80 DEG C to go out temperature.
Specifically, in S3 hydrogen peroxide a concentration of 0.2~2mol/L, a concentration of 0.1~1mol/L of ammonium hydroxide.
Specifically, the liquid-solid ratio of hydrogen peroxide and sulfuric acid leaching slag is 5~10 in S3:1mL/g, extraction time be 0.25~
4h, extraction temperature are 25~80 DEG C.
Specifically, in S4 sodium hydroxide a concentration of 2~5mol/L, the liquid of sodium hydroxide solution and hydrogen peroxide leached mud is solid
Than being 5~10:1mL/g, extraction time are 0.25~4h, and extraction temperature is 25~80 DEG C.
Specifically, it is 100~600rpm that the stirring condition in S1 to S4, which refers to control mixing speed,.Using general when stirring
Stirred tank.
Specifically, the zinc replacement slag, which is oxygen, presses zinc replacement slag caused by acid leaching process zinc lixiviating solution purification process,
Middle Zn and Pb contents are respectively 1.0%~20.0% and 0.5%~5.0%；Ga and Ge contents are respectively 0.1%~0.5% He
0.1%~0.8%.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) it is leached using substep, each step mainly leaches a metal ion species, obtains the leaching rich in the metal ion
Liquid realizes the efficient selective separation of zinc in zinc replacement slag, gallium, germanium and lead；
(2) in leaching process and it is not introduced into F-, equipment corrosion is smaller, and the purification of follow-up leachate is without the de- F- processes of complexity；
(3) leaching process is simple, and easily operated, the gallium germanium rate of recovery is higher, advantageously reduces production cost.
Specific implementation mode
Technical solution provided by the invention is described in further detail below in conjunction with specific embodiment, example is only
For explaining the present invention, it is not intended to limit the scope of the present invention.
The conventional method that method is then well known to those skilled in the art unless otherwise noted is used in following implementation, institute
The drug used is then commercial product unless otherwise noted.
Embodiment 1
Zinc replacement slag is obtained, zinc in zinc replacement slag, lead by certain factory's acidity pressurization zinc dust precipitation containing zinc lixiviating solution, and gallium and germanium contain
Amount is respectively 6.33%, 4.37%, 0.13% and 0.41%.
Selectively leaching zinc, lead, gallium and germanium from above-mentioned zinc replacement slag, are as follows：
S1. Leaching Zinc：By levigate to the whole 100 μm of sieves excessively of zinc replacement slag, take above-mentioned zinc replacement slag 500g that 3000mL is added
In deionized water, it is filtered, washed, dries after leaching 3h under conditions of 25 DEG C of temperature, mixing speed 350rpm, obtain water logging slag
248.5g analyzes zinc in water logging slag, and lead, gallium and Ge content are respectively 1.08%, 8.79%, 0.25% and 0.80%, calculates zinc,
Lead, gallium and germanium leaching rate are respectively 91.52%, 0.031%, 4.42% and 3.02%.
S2. gallium is leached：1500mL 0.2mol/LH are added in above-mentioned 248.5g water loggings slag2SO4In sulfuric acid solution, in temperature
80 DEG C, leach under conditions of mixing speed 400rpm and to be filtered, washed after 4h, dry, obtain sulfuric acid leaching slag 205.6g, analyze sulfuric acid
Zinc in leached mud, lead, gallium and Ge content are respectively 1.20%, 10.59%, 0.02% and 0.95%, calculate zinc, lead, gallium and germanium
Leaching rate is respectively 8.07%, 0.32%, 93.38% and 1.75%.
S3. germanium is leached：Prepare 1500mL 0.25mol/L L H2O2As reagent is leached, 0.25mol/L ammonium hydroxide tune is used
Section pH value of solution is leached to above-mentioned 205.6g sulfuric acid leachings slag is added after 7.0 under conditions of 80 DEG C of temperature, mixing speed 300rpm
It is filtered, washed, dries after 3h, obtain hydrogen peroxide leached mud 185.5g, analyze zinc in hydrogen peroxide leached mud, lead, gallium and Ge content point
Not Wei 1.32%, 11.70%, 0.022% and 0.10%, calculate zinc, lead, gallium and germanium leaching rate are respectively 0.68%, 0.29%,
0.69% and 90.50%.
S4. lead is leached：Above-mentioned 185.5g hydrogen peroxide leached mud is added in 1200mL 4mol/LNaOH solution, in temperature
80 DEG C, leach under conditions of mixing speed 300rpm and to be filtered, washed after 3h, dry to get leaching with sodium hydroxide slag 110.8g, divide
Zinc in liberation of hydrogen sodium oxide molybdena leached mud, lead, gallium and Ge content are respectively 2.20%, 1.05%, 0.036% and 0.16%, calculate zinc,
Lead, gallium and germanium leaching rate are respectively 0.45%, 94.64%, 2.25% and 4.43%.
Embodiment 2
Zinc replacement slag is obtained, zinc in zinc replacement slag, lead by certain factory's acidity pressurization zinc dust precipitation containing zinc lixiviating solution, and gallium and germanium contain
Amount is respectively:7.50%, 4.75%, 0.18% and 0.65%.
Selectively leaching zinc, lead, gallium and germanium from above-mentioned zinc replacement slag, are as follows：
S1. Leaching Zinc：By levigate to the whole 75 μm of sieves excessively of zinc replacement slag, takes above-mentioned zinc replacement slag 400g that 3000mL is added and go
In ionized water, it is filtered, washed, dries after leaching 2h under conditions of 40 DEG C of temperature, mixing speed 300rpm, obtain water logging slag
206.5g analyzes zinc in water logging slag, and lead, gallium and Ge content are respectively 1.20%, 9.19%, 0.33% and 1.23%, calculates zinc,
Lead, gallium and germanium leaching rate are respectively 91.74%, 0.12%, 5.35% and 2.31%.
S2. gallium is leached：Above-mentioned 206.5g water loggings slag is added in 2000mL 0.15mol/L sulfuric acid solutions, in temperature 70
DEG C, leach under conditions of mixing speed 350rpm and to be filtered, washed after 4h, dry, obtain sulfuric acid leaching slag 164.5g, analysis sulfuric acid leaching
It slags tap middle zinc, lead, gallium and Ge content are respectively 1.45%, 11.50%, 0.015% and 1.50%, calculate zinc, lead, gallium and germanium leaching
Extracting rate is respectively 3.74%, 0.32%, 96.38% and 2.85%.
S3. germanium is leached：Prepare 1500mL 0.15mol/L H2O2As reagent is leached, is adjusted and soaked using 0.5mol/L ammonium hydroxide
Go out pH value of solution to above-mentioned 164.5g sulfuric acid leachings slag is added after 8.0, is leached under conditions of 80 DEG C of temperature, mixing speed 400rpm
It is filtered, washed, dries after 4h, obtain hydrogen peroxide leached mud 148.6g, analyze zinc in hydrogen peroxide leached mud, lead, gallium and Ge content point
Not Wei 1.60%, 12.70%, 0.017% and 0.13%, calculate zinc, lead, gallium and germanium leaching rate are respectively 0.32%, 0.24%,
0.63% and 92.17%.
S4. lead is leached：Above-mentioned 148.6g hydrogen peroxide leached mud is added in 1000mL 4mol/LNaOH solution, in temperature
80 DEG C, leach under conditions of mixing speed 400rpm and to be filtered, washed after 2h, dry to get leaching with sodium hydroxide slag 88.3g, divide
Zinc in liberation of hydrogen sodium oxide molybdena leached mud, lead, gallium and Ge content are respectively 2.68%, 1.35%, 0.027% and 0.21%, calculate zinc,
Lead, gallium and germanium leaching rate are respectively 0.47%, 93.68%, 2.77% and 4.01%.
It should be noted that after each step filtering of Examples 1 and 2 obtained filtrate be rich in certain corresponding metal from
The solution of son, corresponding filtrate obtain corresponding metal ion through purified treatment in the prior art is recyclable.Such as mistake in S1
The leachate rich in zinc, lead are obtained after filter, then the content very little in the leachate such as gallium and germanium passes through dezincify purification of leaching liquor
Technique carries out purified treatment, and purification technique can be zinc replacement commonly used in the prior art, chemical precipitation method etc..It is soaked in S4
Go out the leaching with sodium hydroxide slag after lead because the metal element content of high added value is relatively low, can be handled directly as waste.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method of Selectively leaching zinc, lead, gallium and germanium in replacement slag from zinc, which is characterized in that include the following steps:
S1. Leaching Zinc：By the levigate processing of zinc replacement slag, then under agitation, it is carried out at leaching using deionized water
Reason after the completion of leaching, is separated by solid-liquid separation to contain zinc lixiviating solution and water logging slag；
S2. gallium is leached：Under agitation, leaching process is carried out to the water logging slag that S1 is obtained using dilute sulfuric acid, after the completion of leaching,
It is separated by solid-liquid separation to obtain leachate containing gallium and sulfuric acid leaching slag；
S3. germanium is leached：Under agitation, sulfuric acid leaching slag is obtained to S2 using hydrogen peroxide and carries out leaching process, when leaching with
The pH of ammonium hydroxide adjusting control infusion solution is 5.0~8.0, after the completion of leaching, is separated by solid-liquid separation to obtain germanic leachate and dioxygen water logging
It slags tap；
S4. lead is leached：Under agitation, the hydrogen peroxide leached mud that S3 is obtained is carried out at leaching using sodium hydroxide solution
Reason, after the completion of leaching, is separated by solid-liquid separation to obtain leaded leachate and leaching with sodium hydroxide slag.
2. the method for Selectively leaching zinc, lead, gallium and germanium, feature in a kind of replacement slag from zinc according to claim 1
Be, the levigate processing in S1 refer to by zinc replacement slag it is levigate to granularity be 50~100 μm.
3. the method for Selectively leaching zinc, lead, gallium and germanium, feature in a kind of replacement slag from zinc according to claim 1
It is, the liquid-solid ratio of deionized water and zinc replacement slag is 4~10 in S1:1mL/g, extraction time are 0.25~4h, extraction temperature
It is 25~40 DEG C.
It is dilute in S2 4. the method for Selectively leaching zinc, lead, gallium and germanium in a kind of replacement slag from zinc according to claim 1
A concentration of 0.1~1mol/L of sulfuric acid.
5. the method for Selectively leaching zinc, lead, gallium and germanium, feature in a kind of replacement slag from zinc according to claim 4
It is, the liquid-solid ratio of dilute sulfuric acid and water logging slag is 4~10 in S2:1mL/g, extraction time are 0.25~4h, extraction temperature 25
~80 DEG C.
6. the method for Selectively leaching zinc, lead, gallium and germanium, feature in a kind of replacement slag from zinc according to claim 1
It is, a concentration of 0.2~2mol/L of hydrogen peroxide, a concentration of 0.1~1mol/L of ammonium hydroxide in S3.
7. the method for Selectively leaching zinc, lead, gallium and germanium, feature in a kind of replacement slag from zinc according to claim 6
It is, the liquid-solid ratio of hydrogen peroxide and sulfuric acid leaching slag is 5~10 in S3:1mL/g, extraction time are 0.25~4h, extraction temperature
It is 25~80 DEG C.
8. the method for Selectively leaching zinc, lead, gallium and germanium, feature in a kind of replacement slag from zinc according to claim 1
It is, a concentration of 2~5mol/L of sodium hydroxide in S4, the liquid-solid ratio of sodium hydroxide solution and hydrogen peroxide leached mud is 5~10:
1mL/g, extraction time are 0.25~4h, and extraction temperature is 25~80 DEG C.
9. according to the side of Selectively leaching zinc, lead, gallium and germanium in a kind of replacement slag from zinc of claim 1 to 8 any one of them
Method, which is characterized in that the stirring condition in S1 to S4 refers to that control mixing speed is 100~600rpm.
10. according to the side of Selectively leaching zinc, lead, gallium and germanium in a kind of replacement slag from zinc of claim 1 to 8 any one of them
Method, which is characterized in that the zinc replacement slag is zinc replacement slag caused by oxygen pressure acid leaching process zinc lixiviating solution purification process, wherein
Zn and Pb contents are respectively 1.0%~20.0% and 0.5%~5.0%；Ga and Ge contents are respectively 0.1%~0.5% He
0.1%~0.8%.
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Cited By (6)
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| CN109182787A (en) * | 2018-11-01 | 2019-01-11 | 中南大学 | A method of improving germanium, gallium leaching rate in germanic, gallium material |
| CN111440955A (en) * | 2020-05-15 | 2020-07-24 | 广东先导稀材股份有限公司 | Method for extracting gallium from gallium-containing smelting slag |
| CN112646983A (en) * | 2020-10-29 | 2021-04-13 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | Method for directly leaching gallium-germanium slag replaced by zinc powder |
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| CN115261626A (en) * | 2022-07-29 | 2022-11-01 | 广东先导稀材股份有限公司 | Method for recovering gallium from gallium-zinc-containing material under normal pressure |
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| CN109182787A (en) * | 2018-11-01 | 2019-01-11 | 中南大学 | A method of improving germanium, gallium leaching rate in germanic, gallium material |
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| CN112646983A (en) * | 2020-10-29 | 2021-04-13 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | Method for directly leaching gallium-germanium slag replaced by zinc powder |
| CN114318017A (en) * | 2021-12-28 | 2022-04-12 | 广东省科学院资源利用与稀土开发研究所 | Method for deep leaching of zinc, copper, gallium and germanium from zinc replacement slag |
| CN115261626A (en) * | 2022-07-29 | 2022-11-01 | 广东先导稀材股份有限公司 | Method for recovering gallium from gallium-zinc-containing material under normal pressure |
| CN115386732A (en) * | 2022-09-06 | 2022-11-25 | 昆明冶金研究院有限公司 | Method for efficiently recycling zinc, germanium and indium in zinc oxide smoke dust |
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