CN106148690B - A kind of germanium silicon separation method - Google Patents
A kind of germanium silicon separation method Download PDFInfo
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- CN106148690B CN106148690B CN201510163645.1A CN201510163645A CN106148690B CN 106148690 B CN106148690 B CN 106148690B CN 201510163645 A CN201510163645 A CN 201510163645A CN 106148690 B CN106148690 B CN 106148690B
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Abstract
The present invention relates to germanium silicon separation technology fields in germanic silicon raw material, especially a kind of germanium silicon separation method, under certain temperature environment and liquid-solid ratio is limited by the ball milling of germanic silicon materials and using sodium hydroxide solution, so that the germanium and silicon in germanic silicon materials are leached, and then destroy package of the silicon dioxide lattice to germanium, again by electrolysis electrolytic separation germanium silicon leachate, so that the separation rate of germanium silicon reaches more than 90%.
Description
Technical field
The present invention relates to germanium silicon separation technology field in germanic silicon raw material, especially a kind of germanium silicon separation method.
Background technology
Containing Ge high silicon raw materials, generally containing SiO2More than 5%, and there was only ten thousand containing Ge/several to some thousandths of.From high silicon
Ge is extracted in raw material, traditional handicraft is volatilized using fire reduction, H2SO4It leaches, extraction or tannin precipitation Ge, due to high silicon original
Ge majorities in material are by SiO2Package, fire reduction volatilization still have considerable part Ge to enter flue dust with package status.With
H2SO4It leaches, the Ge in the package is not leached, and the leaching rate of recovery of Ge is made to be affected, and more than 50% is reached when serious cannot
It is leached, then someone has studied NH4F extract technologies, in H2SO4NH is added in medium4F could destroy SiO up to more than 40g/L2
Wrapping layer, Si exist in the form of silicofluoric acid, and the Ge being leached generally is recycled using the tannin precipitation method, and tannin sinks liquid after Ge and uses stone
Grey neutralisation processing is containing F-Solution generates CaF2Slag muck is put.NH4F leachings can thoroughly destroy SiO2Ge is wrapped up, but due to NH4F prices
Expensive, consumption is big, and the Ge leached can only use the tannin precipitation method to extract at present, thus production cost is high, and the cost of 1kg germanium is about
It is 2000~2500 yuan.
Also, someone is investigated leaches SiO with 20~40% NaOH solution at 90 DEG C or more2And Ge, then use H2SO4
Or HCl is neutralized to PH8~9.2 and is precipitated SiO2, then by heavy white residue carry out alkali leaching.Again as stated above except silicon, except liquid is adjusted again after silicon
PH value is the heavy Ge of 6.5~6.8,90 DEG C or more hydrolysis, can must contain the Ge concentrate of Ge2~3%.But this method technological process is long,
It is big to consume alkali acid consumption, except silicon simultaneously, Ge losses are big, and there are about more than 30% Ge to enter in desilication slag, and the Ge rate of recovery is low, and filtering is tired
Difficulty, wastewater treatment capacity is big, and production cost is also higher.
Then, this researcher passes through long-term exploration and research, the technique of combining hydrogen oxidation sodium solution leaching process, by germanium
Silicon isolation technics is handled using electrolytic method, so that the rate of recovery of germanium is largely improved, reduces germanic silicon
The loss of raw material germanium removal process reduces the difficulty of germanium silicon separation, reduces germanium silicon separation costs；And using electrolysis point
It is had not been reported in technical literature from germanium silicon technology, and then the germanium silicon isolation technics for germanic silicon raw material provides a kind of new think of
Road.
Invention content
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of germanium silicon separation method, can
Germanium in germanic silicon materials is mostly disengaged from silicon dioxide lattice, destroys package of the silicon dioxide lattice to germanium so that contain
The separation of germanium silicon is reached more than 90% by the germanium and silicon in germanium silicon materials by leaching with sodium hydroxide with electrolysis.
It is achieved particular by following technical scheme：
A kind of germanium silicon separation method, includes the following steps：
(1) mass fraction after germanic silicon materials ball-milling treatment, will be used to be carried out once for the sodium hydroxide solution of 15-30%
Leaching process 2-3h, and processing is filtered, obtain a filter residue and first-time filtrate；Filter residue uses mass fraction again
Sodium hydroxide solution for 15-30% carries out secondary leaching process, and the leaching process time is 0.5-3h, then is filtered place
Reason, obtains secondary filter residue and secondary filtrate；Secondary filter residue returns to be handled, then return it into germanic silicon materials in rotary kiln, is done
Further processing；Secondary filtrate is returned in a leaching process, and after being mixed with sodium hydroxide solution, germanic silicon materials are carried out
Leaching process；
(2) first-time filtrate is handled：Using first-time filtrate as leachate, and to the leachate under normal temperature environment, using straight
Galvanic electricity solution processing >=10h obtains electrodeposit and electrolytic liquid；After electrodeposit carries out drying and processing, germanium concentrate is obtained；
Electrolytic liquid carries out desiliconization processing with lime powder, obtains white residue and desiliconization liquid；White residue returns to rotary kiln processing, and desiliconization liquid returns
It returns in secondary leaching process after being mixed with sodium hydroxide and a filter residue is handled, you can complete the separation of germanium silicon.
During a described leaching process, the liquid-solid ratio of sodium hydroxide solution and germanic silicon materials is 3-4.
During a described leaching process, treatment temperature is 80-90 DEG C.
The leachate handled with DC electrolysis is that Ge reaches 100~2000mg/L, SiO220~50g/L, NaOH
100~150g/L.
The DC electrolysis, 300~700A/m of current density2, electrolytic bath pressure is 3~4V.
The DC electrolysis, anode are alloy lead containing Ag, and cathode is stainless steel plate.The alloy lead containing Ag
Plate can be polylith；Cathode is stainless steel plate, can be 1 piece, two pieces, three pieces or even polylith.
The time of the DC electrolysis processing is 18-40h.
The liquid-solid ratio of the secondary leaching process is 3-4, and the time of secondary leaching process is 2h, secondary leaching process
Temperature is 80-90 DEG C.
Granularity after the germanic silicon materials ball milling is 70-100 mesh.
The temperature that the electrodeposit carries out drying and processing is 50-80 DEG C.
Compared with prior art, technique effect of the invention is embodied in：
The present invention by the ball millings of germanic silicon materials and using sodium hydroxide solution under certain temperature environment and
Liquid-solid ratio is limited so that germanium and silicon in germanic silicon materials are leached, and then destroy silicon dioxide lattice to germanium
Package, by electrolysis electrolytic separation germanium silicon leachate, so that the separation rate of germanium silicon reaches more than 90%.Also, this
Invention carries out desiliconization processing so that silicon also by carrying out desiliconization processing to electrolytic liquid using calcium oxide powder foot couple electrolytic liquid
After being removed in the form of calcium silicates so that after sodium hydroxide solution obtains regeneration, return at the secondary leaching to a filter residue
Reason so that material liquid is constantly recycled, and reduces the loss of raw material, also reduces the discharge capacity of waste liquid.And it is handling
It is consumed in the process without acid-base neutralization so that a large amount of sodium hydroxide solution is recycled, and reduces the cost detached to germanium silicon.
Furthermore the present invention carries out abjection processing by the calcium silicates obtained to desiliconization processing so that the difficulty of filter process
It reduces, that is, avoids silica and show colloidal form presence and bring filtration difficulty, reduce the difficulty of desiliconization, reduce life
Produce cost and energy consumption.And the loss late of the germanium in desiliconization process is small, and only 0.1%；In conjunction with to a leaching process, two
Phase analysis after secondary leaching process again return to after rotary kiln processing, and then germanium therein is carried out at recycling again
Reason, and then the rate of recovery of germanium is improved, reduce the loss late of germanium.
In entire technique, the raw material used is sodium hydroxide and calcium oxide, and the raw material used is easy to get, and also to hydrogen-oxygen
Change sodium to be recycled, so that the processing cost of entire technique is relatively low, small to the pollution of environment, waste liquid discharging amount is low；
Also, the present invention also carries out fluorination lixiviation process and alkali leaching neutralization precipitation method with germanium silicon partition method of the present invention the experimental study of cost
It is compared, 1kg germanium consumption electric energy of the present invention is 1200~1500KWh, and entire production cost is about 1000~1500 yuan, significantly
Less than fluorination lixiviation process and alkali leaching neutralization precipitation method.
Description of the drawings
Fig. 1 is the process flow chart of germanium silicon separation method of the present invention.
Specific embodiment
It is limited technical scheme of the present invention is further, but is required with specific embodiment below in conjunction with the accompanying drawings
The range of protection is not only limited to made description.
Embodiment 1
As shown in Figure 1, a kind of germanium silicon separation method, includes the following steps：
(1) by after germanic silicon materials ball-milling treatment, mass fraction is used once to be soaked for 27% sodium hydroxide solution
Go out and handle 2.1h, and be filtered processing, obtain a filter residue and first-time filtrate；Filter residue use again mass fraction for
18% sodium hydroxide solution carries out secondary leaching process, and the leaching process time is 2.5h, then is filtered processing, obtains
Secondary filter residue and secondary filtrate；Secondary filter residue returns to be handled, then return it into germanic silicon materials in rotary kiln, is done further
Processing；Secondary filtrate is returned in a leaching process, and after being mixed with sodium hydroxide solution, germanic silicon materials are once leached
Processing；
(2) first-time filtrate is handled：Using first-time filtrate as leachate, and to the leachate under normal temperature environment, using straight
Galvanic electricity solution handles 50h, obtains electrodeposit and electrolytic liquid；After electrodeposit carries out drying and processing, germanium concentrate is obtained；Electricity
Liquid carries out desiliconization processing with lime powder after solution, obtains white residue and desiliconization liquid；White residue returns to rotary kiln processing, and desiliconization liquid returns
A filter residue is handled after being mixed in secondary leaching process with sodium hydroxide, you can complete the separation of germanium silicon.
During a described leaching process, the liquid-solid ratio of sodium hydroxide solution and germanic silicon materials is 3.1.
During a described leaching process, treatment temperature is 88 DEG C.
The leachate handled with DC electrolysis is that Ge reaches 500mg/L, SiO240g/L, NaOH 110g/L.
The DC electrolysis, current density 400A/m2, electrolytic bath pressure is 3.7V.
The DC electrolysis, anode are alloy lead containing Ag, and cathode is stainless steel plate.
The time of the DC electrolysis processing is 33h.
The liquid-solid ratio of the secondary leaching process is 3.3, and the temperature of secondary leaching process is 88 DEG C.
Granularity after the germanic silicon materials ball milling is 90 mesh.
The temperature that the electrodeposit carries out drying and processing is 60 DEG C.
Embodiment 2
As shown in Figure 1, a kind of germanium silicon separation method, includes the following steps：
(1) by after germanic silicon materials ball-milling treatment, mass fraction is used once to be soaked for 25% sodium hydroxide solution
Go out and handle 2.5h, and be filtered processing, obtain a filter residue and first-time filtrate；Filter residue use again mass fraction for
20% sodium hydroxide solution carries out secondary leaching process, and the leaching process time is 2h, then is filtered processing, obtains two
Secondary filter residue and secondary filtrate；Secondary filter residue returns to be handled, then return it into germanic silicon materials in rotary kiln, further to be located
Reason；Secondary filtrate is returned in a leaching process, and after being mixed with sodium hydroxide solution, germanic silicon materials are carried out at primary leaching
Reason；
(2) first-time filtrate is handled：Using first-time filtrate as leachate, and to the leachate under normal temperature environment, using straight
Galvanic electricity solution handles 15h, obtains electrodeposit and electrolytic liquid；After electrodeposit carries out drying and processing, germanium concentrate is obtained；Electricity
Liquid carries out desiliconization processing with lime powder after solution, obtains white residue and desiliconization liquid；White residue returns to rotary kiln processing, and desiliconization liquid returns
A filter residue is handled after being mixed in secondary leaching process with sodium hydroxide, you can complete the separation of germanium silicon.
During a described leaching process, the liquid-solid ratio of sodium hydroxide solution and germanic silicon materials is 3.5.
During a described leaching process, treatment temperature is 85 DEG C.
The leachate handled with DC electrolysis is that Ge reaches 1000mg/L, SiO230g/L, NaOH 130g/L.
The DC electrolysis, current density 500A/m2, electrolytic bath pressure is 3.5V.
The DC electrolysis, anode are alloy lead containing Ag, and cathode is stainless steel plate.
The time of the DC electrolysis processing is 30h.
The liquid-solid ratio of the secondary leaching process is 3.5, and the time of secondary leaching process is 2h, secondary leaching process
Temperature is 85 DEG C.
Granularity after the germanic silicon materials ball milling is 80 mesh.
The temperature that the electrodeposit carries out drying and processing is 60 DEG C.
Embodiment 3
As shown in Figure 1, a kind of germanium silicon separation method, includes the following steps：
(1) by after germanic silicon materials ball-milling treatment, mass fraction is used once to be soaked for 30% sodium hydroxide solution
Go out and handle 3h, and be filtered processing, obtain a filter residue and first-time filtrate；Filter residue use again mass fraction for
30% sodium hydroxide solution carries out secondary leaching process, and the leaching process time is 3h, then is filtered processing, obtains two
Secondary filter residue and secondary filtrate；Secondary filter residue returns to be handled, then return it into germanic silicon materials in rotary kiln, further to be located
Reason；Secondary filtrate is returned in a leaching process, and after being mixed with sodium hydroxide solution, germanic silicon materials are carried out at primary leaching
Reason；
(2) first-time filtrate is handled：Using first-time filtrate as leachate, and to the leachate under normal temperature environment, using straight
Galvanic electricity solution handles 13h, obtains electrodeposit and electrolytic liquid；After electrodeposit carries out drying and processing, germanium concentrate is obtained；Electricity
Liquid carries out desiliconization processing with lime powder after solution, obtains white residue and desiliconization liquid；White residue returns to rotary kiln processing, and desiliconization liquid returns
A filter residue is handled after being mixed in secondary leaching process with sodium hydroxide, you can complete the separation of germanium silicon.
During a described leaching process, the liquid-solid ratio of sodium hydroxide solution and germanic silicon materials is 4.
During a described leaching process, treatment temperature is 90 DEG C.
The leachate handled with DC electrolysis is that Ge reaches 2000mg/L, SiO250g/L, NaOH 150g/L.
The DC electrolysis, current density 700A/m2, electrolytic bath pressure is 4V.
The DC electrolysis, anode are alloy lead containing Ag, and cathode is stainless steel plate.
The time of the DC electrolysis processing is 40h.
The liquid-solid ratio of the secondary leaching process is 4, and the temperature of secondary leaching process is 90 DEG C.
Granularity after the germanic silicon materials ball milling is 100 mesh.
The temperature that the electrodeposit carries out drying and processing is 80 DEG C.
Embodiment 4
As shown in Figure 1, a kind of germanium silicon separation method, includes the following steps：
(1) by after germanic silicon materials ball-milling treatment, mass fraction is used once to be soaked for 15% sodium hydroxide solution
Go out and handle 2h, and be filtered processing, obtain a filter residue and first-time filtrate；Filter residue use again mass fraction for
15% sodium hydroxide solution carries out secondary leaching process, and the leaching process time is 0.5h, then is filtered processing, obtains
Secondary filter residue and secondary filtrate；Secondary filter residue returns to be handled, then return it into germanic silicon materials in rotary kiln, is done further
Processing；Secondary filtrate is returned in a leaching process, and after being mixed with sodium hydroxide solution, germanic silicon materials are once leached
Processing；
(2) first-time filtrate is handled：Using first-time filtrate as leachate, and to the leachate under normal temperature environment, using straight
Galvanic electricity solution handles 10h, obtains electrodeposit and electrolytic liquid；After electrodeposit carries out drying and processing, germanium concentrate is obtained；Electricity
Liquid carries out desiliconization processing with lime powder after solution, obtains white residue and desiliconization liquid；White residue returns to rotary kiln processing, and desiliconization liquid returns
A filter residue is handled after being mixed in secondary leaching process with sodium hydroxide, you can complete the separation of germanium silicon.
During a described leaching process, the liquid-solid ratio of sodium hydroxide solution and germanic silicon materials is 3.
During a described leaching process, treatment temperature is 80 DEG C.
The leachate handled with DC electrolysis is that Ge reaches 100mg/L, SiO220g/L, NaOH 100g/L.
The DC electrolysis, current density 300A/m2, electrolytic bath pressure is 3V.
The DC electrolysis, anode are alloy lead containing Ag, and cathode is stainless steel plate.
The time of the DC electrolysis processing is 18h.
The liquid-solid ratio of the secondary leaching process is 3, and the temperature of secondary leaching process is 80 DEG C.
Granularity after the germanic silicon materials ball milling is 70 mesh.
The temperature that the electrodeposit carries out drying and processing is 50 DEG C.
Embodiment 5
As shown in Figure 1, a kind of germanium silicon separation method, with 30% NaOH at 80~90 DEG C to the original containing Ge, Si, Pb
Material leaches 3 hours, obtains alkali leaching liquor containing Ge353.6mg/L, SiO2Then 18.2g/L, Pb510.2mg/L use current density
370A/m2, slot pressure 4V makees anode with one block of stereotype containing Ag, and two pieces of stainless steel plates make cathode, at normal temperatures, are electrolysed 32 hours, electric
Liquid contains Ge26.3mg/L, SiO after solution218.1g/L, Pb0mg/L, Ge electrodeposit rate 94.8%, SiO20.5%, electrodeposition precipitation
Object contains Ge1.56%.
Embodiment 6
As shown in Figure 1, alkali immersion liquid is obtained containing Ge312mg/L, SiO by the germanium silicon separation method of example 5218.4g/L Pb4g/
L, with current density 700A/m2, slot pressure 3.8V is electrolysed 40 hours, obtains electrolytic liquid containing Ge13.2mg/L, SiO218.2g/L,
Pb69mg/L, Ge electrolyzing rate 96.8%, SiO21.1%, Pb98.3%, the earth of positive pole (electrodeposition sediment) is containing Ge2.83%.
Embodiment 7
As shown in Figure 1, a kind of germanium silicon separation method, is leached at 80~90 DEG C containing Ge3300g/t with 15% NaOH,
Pb2.2%, SiO217.5% raw material obtains leachate containing Ge419mg/L, SiO221.3g/L, NaOH66.1g/L, with two pieces
Stereotype containing Ag makees anode, and 3 pieces of stainless steel plates make cathode, current density 685A/m2, slot pressure 4V, room temperature be electrolysed 18 hours, must be electrolysed
Liquid contains Ge36.6mg/L, SiO afterwards2The electrolyzing rate 93.1% of 21g/L, NaOH77.8g/L, Ge, SiO221.7%, electrolytic deposition
Object contains Ge3.86%.
Embodiment 8
As shown in Figure 1, by the germanium silicon separation method of example 7, to be leached with 20% NaOH, alkali immersion liquid contains Ge401mg/L,
SiO225.2g/L NaOH143.1g/L.With one piece of anode, two pieces of cathodes, current density 730A/m2, slot pressure 3.8V, electrolysis 30
Hour, electrolytic liquid contains Ge23.1mg/L, SiO2The electrolyzing rate 95.4% of 20.95%, NaOH96.8/L, Ge, SiO2
16.9%.Electrodeposition deposit contains Ge3.25%.
Embodiment 9
As shown in Figure 1, the electrolytic liquid shown in example 8 carries out desiliconization by 1.5 extraordinarily CaO of stoichiometric amount and handles
NaOH regenerated liquids contain SiO2646.1mg/L, NaOH126.9g/L take off SiO2Efficiency 96.9%, containing Ge21.6mg/L, Ge rates of deposition
6.5%, NaOH regeneration rate 30.1% is carried out sodium hydroxide leaching, must leached with the regenerated liquid to being contained Ge, Si raw materials example 8 Suo Shi
Liquid contains Ge401mg/L, SiO2 25.2g/L。
Embodiment 10
As shown in Figure 1, a kind of germanium silicon separation method, carries out according to the germanium silicon separation method shown in embodiment 8, soak for the first time
The NaOH gone out is returned for second of NaOH leachate, and second of NaOH leached removes SiO for liquid after electrolysis Ge2, regenerated NaOH,
First time leachate contains Ge470mg/L, SiO230.5g/L, second of leachate contain Ge143mg/L, SiO29.59g/L first
Secondary leachate is for being electrolysed, and condition carries out as shown in example 8.Electrolytic liquid contains Ge54.72mg/L, SiO234.4g/L.Ge's
Electrolyzing rate 91.3%, SiO213.1%.
It is important to point out that, above example is only limitted to be further limited technical scheme of the present invention herein,
The improvement of non-protruding essential characteristics and non-significant progress that those skilled in the art make on this basis, belongs to this hair
Bright protection category.
Claims (10)
1. a kind of germanium silicon separation method, which is characterized in that include the following steps：
(1) by after germanic silicon materials ball-milling treatment, mass fraction is used once to be leached for the sodium hydroxide solution of 15-30%
2-3h is handled, and is filtered processing, obtains a filter residue and first-time filtrate；Filter residue use again mass fraction for
The sodium hydroxide solution of 15-30% carries out secondary leaching process, and the leaching process time is 0.5-3h, then is filtered place
Reason, obtains secondary filter residue and secondary filtrate；Secondary filter residue returns to be handled, then return it into germanic silicon materials in rotary kiln, is done
Further processing；After being mixed in leaching process of secondary filtrate return with sodium hydroxide solution, germanic silicon materials are carried out
Leaching process；
(2) first-time filtrate is handled：Using first-time filtrate as leachate, and to the leachate under normal temperature environment, using direct current
Solution processing >=10h obtains electrodeposit and electrolytic liquid；After electrodeposit carries out drying and processing, germanium concentrate is obtained；Electrolysis
Liquid carries out desiliconization processing with lime powder afterwards, obtains white residue and desiliconization liquid；White residue returns to rotary kiln processing, and desiliconization liquid returns to two
A filter residue is handled after being mixed in secondary leaching process with sodium hydroxide, you can complete the separation of germanium silicon.
2. germanium silicon separation method as described in claim 1, which is characterized in that during a described leaching process, sodium hydroxide
The liquid-solid ratio of solution and germanic silicon materials is 3-4.
3. germanium silicon separation method as described in claim 1, which is characterized in that during a described leaching process, treatment temperature
It is 80-90 DEG C.
4. germanium silicon separation method as described in claim 1, which is characterized in that it is described with DC electrolysis handle leachate be
Ge reaches 100~2000mg/L, SiO2100~150g/L of 20~50g/L, NaOH.
5. germanium silicon separation method as described in claim 1, which is characterized in that the DC electrolysis, current density 300~
700A/m2, electrolytic bath pressure is 3~4V.
6. germanium silicon separation method as described in claim 1, which is characterized in that the DC electrolysis, anode are to be closed containing Ag
Golden stereotype, cathode are stainless steel plate.
7. germanium silicon separation method as described in claim 1, which is characterized in that the time of the DC electrolysis processing is 18-
40h。
8. germanium silicon separation method as described in claim 1, which is characterized in that the liquid-solid ratio of the secondary leaching process is 3-
4, the time of secondary leaching process is 2h, and the temperature of secondary leaching process is 80-90 DEG C.
9. germanium silicon separation method as described in claim 1, which is characterized in that the granularity after the germanic silicon materials ball milling
For 70-100 mesh.
10. germanium silicon separation method as described in claim 1, which is characterized in that the electrodeposit carries out drying and processing
Temperature be 50-80 DEG C.
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| CN109182787B (en) * | 2018-11-01 | 2020-07-31 | 中南大学 | Method for improving leaching rate of germanium and gallium in material containing germanium and gallium |
| CN110386606A (en) * | 2019-08-02 | 2019-10-29 | 西安凯立新材料股份有限公司 | A method of recycling SiGe from germanic optical fiber waste material |
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| RU2337164C1 (en) * | 2007-03-06 | 2008-10-27 | Леонид Михайлович Черемисинов | Method of processing zinc and germanium containing solid phase polymetallic mineral material |
| CN101418373A (en) * | 2008-09-16 | 2009-04-29 | 云南临沧鑫圆锗业股份有限公司 | Method for extracting germanium from chlorinated distillation slag |
| CN101591023A (en) * | 2008-05-26 | 2009-12-02 | 同方环境股份有限公司 | A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power |
| CN103614576A (en) * | 2013-11-27 | 2014-03-05 | 谈发堂 | Method for recycling germanium from germanium-containing glass |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2337164C1 (en) * | 2007-03-06 | 2008-10-27 | Леонид Михайлович Черемисинов | Method of processing zinc and germanium containing solid phase polymetallic mineral material |
| CN101591023A (en) * | 2008-05-26 | 2009-12-02 | 同方环境股份有限公司 | A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power |
| CN101418373A (en) * | 2008-09-16 | 2009-04-29 | 云南临沧鑫圆锗业股份有限公司 | Method for extracting germanium from chlorinated distillation slag |
| CN103614576A (en) * | 2013-11-27 | 2014-03-05 | 谈发堂 | Method for recycling germanium from germanium-containing glass |
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