CN107723467A - A kind of method of high efficiente callback germanium - Google Patents
A kind of method of high efficiente callback germanium Download PDFInfo
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- CN107723467A CN107723467A CN201710851232.1A CN201710851232A CN107723467A CN 107723467 A CN107723467 A CN 107723467A CN 201710851232 A CN201710851232 A CN 201710851232A CN 107723467 A CN107723467 A CN 107723467A
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- germanium
- efficiente callback
- high efficiente
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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
- C22B7/007—Wet processes by acid leaching
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
- C22B41/00—Obtaining germanium
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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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- Geochemistry & Mineralogy (AREA)
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Abstract
The invention belongs to metal recovery field, specifically discloses a kind of method of high efficiente callback germanium.This method comprises the following steps：Germanium slag is crushed, is milled to 130~180 mesh；Microwave acid dipping is done with sulfuric acid solution, is added leaching agent and oxidant while leaching, is controlled whole acid concentration to obtain acid leaching residue and pickle liquor after the completion of acidleach between 70~90g/L；Potassium oxide is added into solution, does to neutralize twice and leaches, by a filter residue and secondary filter residue in 380~480 DEG C of 2.5~4h of roasting temperature, obtain thick germanium dioxide, high-purity germanium dioxide is prepared after chlorinated distillation, rectifying and hydrolyzing process in thick germanium dioxide.The inventive method is easy to operate, technique is simple and flow is short, need to only carry out an acidleach and neutralize twice to leach, the comprehensive recovery of germanium reaches more than 98.6%.
Description
Technical field
The invention belongs to metallurgical technology field, is related to metal recovery, and in particular to a kind of method of high efficiente callback germanium.
Background technology
Germanium is a kind of important semi-conducting material, for manufacturing transistor and various electronic installations.Germanium belongs to dispersed elements,
In nature it is in mainly in dispersity association polymetallic deposit, it is industrial at present mainly from the sulphide ore of lead-zinc core copper
Extract germanium.
In lead zinc-copper smelting process, when germanium is higher in raw material, germanium can be enriched in the materials such as cigarette ash or replacement slag,
When handling these germanic higher materials, the technique of generally use at present, first, being leached germanium by normal pressure or hyperbaric oxygen leaching, evergreen chinquapin
Glue adsorption and enrichment germanium, germanium dioxide is distilled to recover, the germanium in leached mud is recycled to cigarette ash by fuming furnace, leaches recovery again；
The comprehensive recovery of the method germanium is only 90%, while adds fuming process, causes long flow path, production cost height.It is second, normal
Fluoride or nitrate are added when pressure leaches, improves the leaching rate of germanium；The method germanium leaching rate is up to 90~95%, but due to adding
Fluoride or nitrate are added, high have been required to the corrosion resistance of equipment, service life of equipment is short, operating environment rather harsh, difficult
To adapt to environmental requirement.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method of high efficiente callback germanium, and the leaching rate of this method germanium reaches
To more than 98.6%, and simplify the production technology of germanium.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of method of high efficiente callback germanium, this method
Comprise the following steps：
(1) using germanium slag as raw material, germanium slag is crushed, is milled to 130~180 mesh；
(2) the germanium slag that step (1) obtains is done into acidleach with sulfuric acid solution, and introduces microwave reinforced leaching, germanium slag and sulfuric acid
The liquid-solid ratio of solution is 6.5~7.5 ︰ 1, adds leaching agent and oxidant while leaching, controls whole acid concentration in 70~90g/L
Between, acid leaching residue and pickle liquor are obtained after the completion of acidleach；
(3) above-mentioned pickle liquor is heated to 80~85 DEG C, adds the liquid of potassium oxide, the pickle liquor and potassium oxide thereto
Gu ratio is 8.5~9.5 ︰ 1, after stirring 0.5~0.6h, 1.5~2.5h of reaction is stood, a filter residue is filtrated to get and once filters
Liquid；
(4) above-mentioned first-time filtrate is heated to 85~90 DEG C, adds potassium oxide, the first-time filtrate and potassium oxide thereto
Liquid-solid ratio be 9.0~9.5 ︰ 1, after stirring 0.5~0.6h, stand 2.0~2.5h of reaction, be filtrated to get secondary filter residue and secondary
Filtrate；
(5) an above-mentioned filter residue and secondary filter residue are obtained into thick titanium dioxide in 380~480 DEG C of 2.5~4h of roasting temperature
High-purity germanium dioxide is prepared after chlorinated distillation, rectifying and hydrolyzing process in germanium, thick germanium dioxide.
Wherein, in the method for above-mentioned high efficiente callback germanium, the concrete operations condition of ball milling is described in step (1)：Using ball
Grinding machine carries out ball milling, and ball material mass ratio is 30~40:1, abrading-ball be diameter 4mm steel ball, 250~350rpm of drum's speed of rotation.
Wherein, in the method for above-mentioned high efficiente callback germanium, the power of microwave described in step (2) is 500~600W.
Wherein, in the method for above-mentioned high efficiente callback germanium, the temperature of acidleach described in step (2) is 80~85 DEG C, and the time is
0.5~0.8h.
Wherein, in the method for above-mentioned high efficiente callback germanium, leaching agent described in step (2) is potassium oxalate, and its addition is germanium
The 6~8% of slag amount.
Wherein, in the method for above-mentioned high efficiente callback germanium, oxidant described in step (2) is hydrogen peroxide, and its addition is germanium
The 10~13% of slag amount.
Wherein, in the method for above-mentioned high efficiente callback germanium, the concentration of hydrogen peroxide described in step (2) is 24~35%.
Wherein, in the method for above-mentioned high efficiente callback germanium, the rotating speed that is stirred described in step (3) and (4) for 300~
400rpm。
Wherein, in the method for above-mentioned high efficiente callback germanium, secondary filtrate sends to wastewater treatment process described in step (4).
Compared with prior art, the beneficial effects of the invention are as follows：The inventive method is easy to operate, technique is simple and flow
It is short, it need to only carry out an acidleach and neutralize twice to leach, germanium leaching efficiency is high：Microwave leaching and leaching agent are used during acidleach
The mode being combined, the leaching efficiency (account for germanium amount 60% or so) of germanium is greatly improved, save extraction time；Neutralize and leach twice
Shi Zengjia whipping steps, accelerate to neutralize speed and germanium leaching efficiency.The comprehensive recovery of this method germanium reaches more than 98.6%, together
In Shi Liyong and heavy germanium substitutes the heavy germanium of tannin, reduces production cost, the development to germanium industry provides necessary technical support.
Embodiment
The invention provides a kind of method of high efficiente callback germanium, this method comprises the following steps：
(1) using germanium slag as raw material, germanium slag is crushed, is milled to 130~180 mesh；
(2) the germanium slag that step (1) obtains is done into acidleach with sulfuric acid solution, and introduces microwave reinforced leaching, the power of microwave
For 500~600W, the liquid-solid ratio of germanium slag and sulfuric acid solution is 6.5~7.5 ︰ 1, and acidleach temperature is 80~85 DEG C, the time is 0.5~
0.8h, leaching agent-potassium oxalate and oxidant-hydrogen peroxide are added while leaching, controls whole acid concentration between 70~90g/L,
Acid leaching residue and pickle liquor are obtained after the completion of acidleach；During acidleach by the way of microwave leaching and leaching agent are combined, greatly improve
The leaching efficiency (account for germanium amount 60% or so) of germanium, save extraction time；
(3) above-mentioned pickle liquor is heated to 80~85 DEG C, adds the liquid of potassium oxide, the pickle liquor and potassium oxide thereto
Gu ratio is 8.5~9.5 ︰ 1, after stirring 0.5~0.6h, 1.5~2.5h of reaction is stood, a filter residue is filtrated to get and once filters
Liquid；
(4) above-mentioned first-time filtrate is heated to 85~90 DEG C, adds potassium oxide, the first-time filtrate and potassium oxide thereto
Liquid-solid ratio be 9.0~9.5 ︰ 1, after stirring 0.5~0.6h, stand 2.0~2.5h of reaction, be filtrated to get secondary filter residue and secondary
Filtrate；Neutralizing twice increases whipping step when leaching, accelerate to neutralize speed and germanium leaching efficiency；
(5) an above-mentioned filter residue and secondary filter residue are obtained into thick titanium dioxide in 380~480 DEG C of 2.5~4h of roasting temperature
High-purity germanium dioxide is prepared after chlorinated distillation, rectifying and hydrolyzing process in germanium, thick germanium dioxide.
Wherein, in the method for above-mentioned high efficiente callback germanium, the concrete operations condition of ball milling is described in step (1)：Using ball
Grinding machine carries out ball milling, and ball material mass ratio is 30~40:1, abrading-ball be diameter 4mm steel ball, 250~350rpm of drum's speed of rotation.
Wherein, in the method for above-mentioned high efficiente callback germanium, the addition of potassium oxalate described in step (2) is the 6 of germanium slag amount
~8%；The addition of the hydrogen peroxide is the 10~13% of germanium slag amount.
Wherein, in the method for above-mentioned high efficiente callback germanium, the concentration of hydrogen peroxide described in step (2) is 24~35%.
Wherein, in the method for above-mentioned high efficiente callback germanium, the rotating speed that is stirred described in step (3) and (4) for 300~
400rpm。
Wherein, in the method for above-mentioned high efficiente callback germanium, secondary filtrate sends to wastewater treatment process described in step (4).
The present invention is made further explanation and description below in conjunction with specific embodiment, but and is not so limited the present invention
Protection domain.
Embodiment 1
The method of high efficiente callback germanium, this method comprise the following steps：
(1) using germanium slag as raw material, germanium slag is crushed, ball milling is carried out using ball mill, ball material mass ratio is 32 ︰ 1, and abrading-ball is
Diameter 4mm steel ball, drum's speed of rotation 300rpm, it is milled to 130 mesh；
(2) the germanium slag that step (1) obtains is done into acidleach with sulfuric acid solution, and introduces microwave reinforced leaching, the power of microwave
For 500W, the liquid-solid ratio of germanium slag and sulfuric acid solution is 7.5 ︰ 1, and acidleach temperature is 85 DEG C, time 0.7h, is added while leaching
(hydrogen peroxide concentration 28%, it adds for leaching agent-potassium oxalate (oxalic acid potassium application rate is the 6% of germanium slag amount) and oxidant-hydrogen peroxide
Enter amount for germanium slag amount 12%), control whole acid concentration to obtain acid leaching residue and pickle liquor after the completion of 80g/L, acidleach；Through inspection
Survey, the content of germanium accounts for the 64.3% of germanium total amount in pickle liquor；
(3) above-mentioned pickle liquor is heated to 85 DEG C, adds the liquid-solid ratio of potassium oxide, the pickle liquor and potassium oxide thereto
After stirring 0.5h for 9.0 ︰ Isosorbide-5-Nitrae 00rpm rotating speeds, reaction 2h is stood, is filtrated to get a filter residue and first-time filtrate；
(4) above-mentioned first-time filtrate is heated to 90 DEG C, adds the liquid of potassium oxide, the first-time filtrate and potassium oxide thereto
Gu after stirring 0.5h for 9.5 ︰ Isosorbide-5-Nitrae 00rpm rotating speeds, reaction 2.5h is stood, is filtrated to get secondary filter residue and secondary filtrate, it is secondary
Filtrate sends to wastewater treatment process；
(5) by an above-mentioned filter residue and secondary filter residue in 420 DEG C of roasting temperature 3.0h, thick germanium dioxide is obtained, thick two
High-purity germanium dioxide is prepared after chlorinated distillation, rectifying and hydrolyzing process in germanium oxide.The comprehensive leaching of germanium in the present embodiment
Rate is 98.9%.
Embodiment 2
The method of high efficiente callback germanium, this method comprise the following steps：
(1) using germanium slag as raw material, germanium slag is crushed, ball milling is carried out using ball mill, ball material mass ratio is 40 ︰ 1, and abrading-ball is
Diameter 4mm steel ball, drum's speed of rotation 350rpm, it is milled to 160 mesh；
(2) the germanium slag that step (1) obtains is done into acidleach with sulfuric acid solution, and introduces microwave reinforced leaching, the power of microwave
For 550W, the liquid-solid ratio of germanium slag and sulfuric acid solution is 7.0 ︰ 1, and acidleach temperature is 80 DEG C, time 0.8h, is added while leaching
(hydrogen peroxide concentration 30%, it adds for leaching agent-potassium oxalate (oxalic acid potassium application rate is the 7% of germanium slag amount) and oxidant-hydrogen peroxide
Enter amount for germanium slag amount 11%), control whole acid concentration to obtain acid leaching residue and pickle liquor after the completion of 90g/L, acidleach；Through inspection
Survey, the content of germanium accounts for the 65.9% of germanium total amount in pickle liquor；
(3) above-mentioned pickle liquor is heated to 80 DEG C, adds the liquid-solid ratio of potassium oxide, the pickle liquor and potassium oxide thereto
For 9.5 ︰ 1, after 360rpm rotating speeds stir 0.6h, reaction 2.5h is stood, is filtrated to get a filter residue and first-time filtrate；
(4) above-mentioned first-time filtrate is heated to 85 DEG C, adds the liquid of potassium oxide, the first-time filtrate and potassium oxide thereto
Gu ratio is 9.5 ︰ 1, after 360rpm rotating speeds stirring 0.6h, reaction 2.5h is stood, is filtrated to get secondary filter residue and secondary filtrate；
(5) by an above-mentioned filter residue and secondary filter residue in 480 DEG C of roasting temperature 2.5h, thick germanium dioxide is obtained, thick two
High-purity germanium dioxide is prepared after chlorinated distillation, rectifying and hydrolyzing process in germanium oxide.The comprehensive leaching of germanium in the present embodiment
Rate is 99.2%.
Described above is the preferred embodiments of the present invention, it is noted that for those skilled in the art, is not being taken off
On the premise of structure of the present invention, various modifications and improvements can be made, these should also be as being considered as protection scope of the present invention,
These are all without the practicality for influenceing the effect of the invention implemented and this patent.
Claims (9)
- A kind of 1. method of high efficiente callback germanium, it is characterised in that this method comprises the following steps：(1) using germanium slag as raw material, germanium slag is crushed, is milled to 130~180 mesh；(2) the germanium slag that step (1) obtains is done into acidleach with sulfuric acid solution, and introduces microwave reinforced leaching, germanium slag and sulfuric acid solution Liquid-solid ratio be 6.5~7.5 ︰ 1, add leaching agent and oxidant while leaching, control whole acid concentration 70~90g/L it Between, acid leaching residue and pickle liquor are obtained after the completion of acidleach；(3) above-mentioned pickle liquor is heated to 80~85 DEG C, adds the liquid-solid ratio of potassium oxide, the pickle liquor and potassium oxide thereto For 8.5~9.5 ︰ 1, after stirring 0.5~0.6h, 1.5~2.5h of reaction is stood, is filtrated to get a filter residue and first-time filtrate；(4) above-mentioned first-time filtrate is heated to 85~90 DEG C, adds the liquid of potassium oxide, the first-time filtrate and potassium oxide thereto Gu ratio is 9.0~9.5 ︰ 1, after stirring 0.5~0.6h, 2.0~2.5h of reaction is stood, is filtrated to get secondary filter residue and secondary filter Liquid；(5) an above-mentioned filter residue and secondary filter residue are obtained into thick germanium dioxide in 380~480 DEG C of 2.5~4h of roasting temperature, High-purity germanium dioxide is prepared after chlorinated distillation, rectifying and hydrolyzing process in thick germanium dioxide.
- 2. the method for high efficiente callback germanium according to claim 1, it is characterised in that ball milling is specific described in step (1) Operating condition is：Ball milling is carried out using ball mill, ball material mass ratio is 30~40:1, abrading-ball be diameter 4mm steel ball, ball mill 250~350rpm of rotating speed.
- 3. the method for high efficiente callback germanium according to claim 1, it is characterised in that the power of microwave described in step (2) For 500~600W.
- 4. the method for high efficiente callback germanium according to claim 3, it is characterised in that the temperature of acidleach described in step (2) For 80~85 DEG C, the time is 0.5~0.8h.
- 5. the method for high efficiente callback germanium according to claim 1, it is characterised in that leaching agent described in step (2) is grass Sour potassium, its addition are the 6~8% of germanium slag amount.
- 6. the method for high efficiente callback germanium according to claim 1, it is characterised in that oxidant is double described in step (2) Oxygen water, its addition are the 10~13% of germanium slag amount.
- 7. the method for high efficiente callback germanium according to claim 6, it is characterised in that hydrogen peroxide is dense described in step (2) Spend for 24~35%.
- 8. the method for high efficiente callback germanium according to claim 1, it is characterised in that stirred described in step (3) and (4) Rotating speed is 300~400rpm.
- 9. the method for high efficiente callback germanium according to claim 1, it is characterised in that state secondary filtrate in step (4) and send to Wastewater treatment process.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110306069A (en) * | 2019-07-09 | 2019-10-08 | 中锗科技有限公司 | A method of the Ti recovery from germanic acid solution, germanic lye |
| CN112250120A (en) * | 2020-12-21 | 2021-01-22 | 矿冶科技集团有限公司 | Method for preparing ternary precursor and lithium carbonate by using waste lithium ion battery black powder and nickel cobalt sulfide ore in synergy mode and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110306069A (en) * | 2019-07-09 | 2019-10-08 | 中锗科技有限公司 | A method of the Ti recovery from germanic acid solution, germanic lye |
| CN112250120A (en) * | 2020-12-21 | 2021-01-22 | 矿冶科技集团有限公司 | Method for preparing ternary precursor and lithium carbonate by using waste lithium ion battery black powder and nickel cobalt sulfide ore in synergy mode and application |
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