CN107601511A - A kind of method of the separation and Extraction silicon from white residue - Google Patents
A kind of method of the separation and Extraction silicon from white residue Download PDFInfo
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- CN107601511A CN107601511A CN201710597829.8A CN201710597829A CN107601511A CN 107601511 A CN107601511 A CN 107601511A CN 201710597829 A CN201710597829 A CN 201710597829A CN 107601511 A CN107601511 A CN 107601511A
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- Prior art keywords
- white residue
- silicon
- separation
- extraction
- slag
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 73
- 239000010703 silicon Substances 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000926 separation method Methods 0.000 title claims abstract description 34
- 238000000605 extraction Methods 0.000 title claims abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002893 slag Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 230000006698 induction Effects 0.000 claims abstract description 11
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 8
- 238000009413 insulation Methods 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000011112 process operation Methods 0.000 abstract 1
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000011084 recovery Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- ZDUOUNIIAGIPSD-UHFFFAOYSA-N 1,1,1-tribromoethane Chemical compound CC(Br)(Br)Br ZDUOUNIIAGIPSD-UHFFFAOYSA-N 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
The invention discloses a kind of method of the separation and Extraction silicon from white residue, crucible equipped with white residue is placed in induction furnace, and 5 ~ 10Pa will be evacuated in stove, it is re-filled with argon gas, then start induction furnace and white residue is heated to 1450 ~ 1700 DEG C, it is incubated 0.5 ~ 2h, 20 ~ 25 DEG C are cooled to again, mechanically decoupled method is finally taken to be kept completely separate the silicon after cooling with slag, reach the purpose of the separation and Extraction silicon from white residue, for the extraction rate reached of silicon to more than 95%, this method also has certain removal effect to Fe, Al and Ca in silicon in white residue；Present invention process process operation is simple, and cost is cheap, green cleaning, solves the present situation that the white residue that industrial silicon enterprise faces is difficult to separate and recycled, may be directly applied to industrial silicon production process.
Description
Technical field
The present invention relates to a kind of method of the separation and Extraction silicon from white residue, belong to the technical field of Separation ＆ Purification.
Background technology
Industrial silicon is the industrial products smelted by silica and carbonaceous reducing agent in ore-smelting electric furnace, principal component silicone content
More than 98%.Based on material, industrial silicon is widely used in the industries such as metallurgy, chemical industry, electronics, machinery, and industrial silicon is as life
The original material of production solar energy level silicon is just constantly developed.At present, global industry silicon production capacity reaches 5,900,000 tons/year, yield
3140000 tons, Chinese 4,600,000 tons/year of production capacity, the 78% of global aggregated capacity is accounted for, yield reaches 2,100,000 tons.
White residue is that metallic silicon external refining of two-maing ladle prepares caused a kind of metallurgical slag during industrial silicon, two-mans ladle and refined
Cheng Zhong, about 200 kilograms of industrial silicon white residue can be produced by often refining 2 tons of silicon water, and white residue is all used for paving the way for a long time or conduct
Waste is stored up, and occupies substantial amounts of soil space resource, more than 15% metallic silicon amount, these metallic silicons are usually contained in white residue
Loss is in white residue in the form of field trash, it is difficult to which separation and recovery utilizes, and causes the waste of resource.Therefore, divide from white residue
From and to extract metallic silicon significant.
The most easy method of industrial silicon is extracted from white residue is：By obvious light slag and dark slag in white residue by hand first
Hammer separation, then select principle further to separate in, finally separated using melting.However, the method for separation white residue by hand is used, no
But more and pure industrial silicons is hardly resulted in, and there is also certain waste to resource.
Sheep reality et al.（The patent No. 201611131058.5）A kind of tribromoethane solution for white residue separation is disclosed to return
Receipts system, including residue module and silicon module, are characterized in repeatedly being fractionated, good separating effect, efficiency high.Tan Yi et al.（Patent
Numbers 201310244836.1）The slag former for being easy to white residue to separate during a kind of polycrystalline silicon medium melting and its application method, energy are provided
White residue separating effect is enough improved, the viscosity of slag, improves the rate of recovery, reduce cost when reducing the separation of slag silicon.Qu Ren waits people quietly and existed《Cloud
It is southern metallurgical》On delivered the entitled technique of industrial silicon " from white residue extract " (2012,41 (3):Paper 83-85), is carried
A kind of method for handling industrial silicon white residue has been supplied, it is molten using main frequency furnace, supplying by processes such as picking, machine choosing, dispensing, meltings
Agent, refines elemental silicon from industrial silicon waste, and product reaches industrial silicon precision.Although some researchers separate to white residue and carried out
Attempt, but be all extremely difficult to preferable effect.
The content of the invention
It is an object of the invention to propose a kind of method for white residue separation and Extraction silicon, recovery of this method to industrial silicon
Effect is fairly obvious, and the extraction rate reached of industrial silicon solves the shape that silicon is difficult to separate and utilized in white residue well to more than 95%
Condition, cost of the present invention is cheap, green cleaning, for from white residue separation and Extraction silicon provide a new approach.
Technical scheme is as follows：The crucible equipped with white residue is placed in induction furnace first, while will be taken out in stove true
Sky is filled with argon gas to 5 ~ 10Pa；Then start induction furnace and white residue is heated to 1450 ~ 1700 DEG C, and be incubated 0.5 ~ 2h；It will protect
White residue after temperature is cooled to 20 ~ 25 DEG C；Finally take mechanically decoupled method to be kept completely separate the silicon after cooling with slag, that is, reach
The purpose of separation and Extraction silicon from white residue.
The method of present invention separation and Extraction silicon from white residue, concrete operations are as follows：
（1）Crucible equipped with white residue is placed in induction furnace, while 5 ~ 10Pa will be evacuated in stove, and is filled with argon gas；
（2）Start induction furnace and white residue is heated to 1450 ~ 1700 DEG C, and be incubated 0.5 ~ 2h；Wherein induction furnace power frequency is 2.5
~ 3.0kHz, power are 4 ~ 6kW；
（3）White residue after insulation is cooled to 20 ~ 25 DEG C；Wherein rate of temperature fall is 20 ~ 50 DEG C/min；
（4）Take mechanically decoupled method to be kept completely separate the silicon after cooling with slag, that is, reach the separation and Extraction silicon from white residue
Purpose；Wherein the slag after cooling is carried out with silicon using wire cutting machine mechanically decoupled.
Beneficial effects of the present invention：
（1）The inventive method is practical, production cost is low without add any reagent into white residue.
（2）The inventive method can be completed to separate the purpose of white residue, operation in induction furnace by heating-insulation-cooling
With the equal very simple of equipment.
（3）The effect of the inventive method white residue separation is fairly obvious, the extraction rate reached of silicon to more than 95%, impurity member in silicon
Plain Al, Fe, Ca also have certain removal effect.
Operation is simple for the inventive method, and cost is cheap, green, for from white residue separation and Extraction silicon provide one
The new effective way of kind, practicality is stronger, has broad application prospects.
Embodiment
The present invention is further illustrated by the examples that follow, but should be noted that the scope of the present invention not by these embodiments
Limitation.
Embodiment 1：The method of separation and Extraction silicon, concrete operations are as follows from white residue：
（1）Using Fe, Al, Ca content be respectively 0.187%, 0.121% and 0.083% industrial silicon white residue as raw material, weigh 80g silicon
Slag loads graphite crucible, and crucible is placed in intermediate frequency furnace, while 10Pa will be evacuated in stove, then is filled with argon to vacuum chamber
Gas is until 1 atmospheric pressure；
（2）The power frequency of regulation intermediate frequency furnace is 2.5kHz, power 4.6kW, starts intermediate frequency furnace and is heated, use is red
Outer temperature measurer carries out temperature survey；
（3）After in-furnace temperature reaches 1450 DEG C, insulation 30min is carried out to melting white residue, power is turned down after insulation, made warm in stove
Degree is cooled to 20 DEG C with 35 DEG C/min speed；
（4）It is mechanically decoupled to the white residue progress after cooling using wire cutting machine, with Fe, Al, Ca in silicon after the measure separation of XRF methods
The content of metal impurities is respectively 0.114%, 0.092% and 0.079%；The recovery rate that silicon in white residue is calculated according to silicon gauge is
96.6%。
Embodiment 2：The method of separation and Extraction silicon, concrete operations are as follows from white residue：
（1）Using Fe, Al, Ca content be respectively 0.187%, 0.121% and 0.083% industrial silicon white residue as raw material, weigh 100g silicon
Slag loads graphite crucible, and crucible is placed in intermediate frequency furnace, while 5Pa will be evacuated in stove, then is filled with argon to vacuum chamber
Gas is until 1 atmospheric pressure；
（2）The power frequency of regulation intermediate frequency furnace is 2.8kHz, power 5kW, starts intermediate frequency furnace and is heated, use is infrared
Temperature measurer carries out temperature survey；
（3）After in-furnace temperature reaches 1500 DEG C, insulation 2h is carried out to melting white residue, power is turned down after insulation, makes in-furnace temperature
25 DEG C are cooled to 20 DEG C/min speed；
（4）Machine cuts separation is carried out to the white residue after cooling using wire cutting machine, with Fe in silicon after the measure separation of XRF methods,
The content of Al, Ca metal impurities is respectively 0.102%, 0.104% and 0.064%；The recovery rate of silicon in white residue is calculated according to silicon gauge
For 95.6%.
Embodiment 3：The method of separation and Extraction silicon, concrete operations are as follows from white residue：
（1）Using Fe, Al, Ca content be respectively 0.187%, 0.121% and 0.083% industrial silicon white residue as raw material, weigh 80g silicon
Slag loads graphite crucible, and crucible is placed in intermediate frequency furnace, while 5Pa will be evacuated in stove, then is filled with argon to vacuum chamber
Gas is until 1 atmospheric pressure；
（2）The power frequency of regulation intermediate frequency furnace is 3.0kHz, power 6kW, starts intermediate frequency furnace and is heated, use is infrared
Temperature measurer carries out temperature survey；
（3）After in-furnace temperature reaches 1700 DEG C, insulation 1h is carried out to melting white residue, power is turned down after insulation, makes in-furnace temperature
23 DEG C are cooled to 50 DEG C/min speed；
（4）Machine cuts separation is carried out to the white residue after cooling using wire cutting machine, with Fe in silicon after the measure separation of XRF methods,
The content of Al, Ca metal impurities is respectively 0.165%, 0.118% and 0.073%；The recovery rate of silicon in white residue is calculated according to silicon gauge
For 95.0%.
Embodiment 4：The method of separation and Extraction silicon, concrete operations are as follows from white residue：
（1）Using Fe, Al, Ca content be respectively 0.187%, 0.121% and 0.083% industrial silicon white residue as raw material, weigh 80g silicon
Slag loads graphite crucible, and crucible is placed in intermediate frequency furnace, while 8Pa will be evacuated in stove, then is filled with argon to vacuum chamber
Gas is until 1 atmospheric pressure；
（2）The power frequency of regulation intermediate frequency furnace is 2.7kHz, power 5.5kW, starts intermediate frequency furnace and is heated, use is red
Outer temperature measurer carries out temperature survey；
（3）After in-furnace temperature reaches 1650 DEG C, insulation 1.5h is carried out to melting white residue, power is turned down after insulation, made warm in stove
Degree is cooled to 25 DEG C with 30 DEG C/min speed；
（4）Machine cuts separation is carried out to the white residue after cooling using wire cutting machine, with Fe in silicon after the measure separation of XRF methods,
The content of Al, Ca metal impurities is respectively 0.152%, 0.0957% and 0.066%；The extraction of silicon in white residue is calculated according to silicon gauge
Rate is 96.2%.
Claims (4)
- A kind of 1. method of the separation and Extraction silicon from white residue, it is characterised in that carry out as follows：（1）Crucible equipped with white residue is placed in induction furnace, and 5 ~ 10Pa will be evacuated in stove, is re-filled with argon gas；（2）Start induction furnace and white residue is heated to 1450 ~ 1700 DEG C, and be incubated 0.5 ~ 2h；（3）White residue after insulation is cooled to 20 DEG C ~ 25 DEG C；（4）Take mechanically decoupled method to be kept completely separate the silicon after cooling with slag, that is, reach the separation and Extraction silicon from white residue Purpose.
- 2. the method for the separation and Extraction silicon according to claim 1 from white residue, it is characterised in that：Step（2）Middle induction furnace Power frequency is 2.5 ~ 3.0kHz, and power is 4 ~ 6kW.
- 3. the method for the separation and Extraction silicon according to claim 1 from white residue, it is characterised in that：Step（3）Middle cooling speed Rate is 20 ~ 50 DEG C/min.
- 4. the method for the separation and Extraction silicon according to claim 1 from white residue, it is characterised in that：Step（4）It is middle to use line Cutting machine carries out mechanically decoupled to the slag after cooling with silicon.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710597829.8A CN107601511A (en) | 2017-07-21 | 2017-07-21 | A kind of method of the separation and Extraction silicon from white residue |
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| CN201710597829.8A CN107601511A (en) | 2017-07-21 | 2017-07-21 | A kind of method of the separation and Extraction silicon from white residue |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675306A (en) * | 2018-05-30 | 2018-10-19 | 云南永昌硅业股份有限公司 | A kind of method of silicon metal in high efficiente callback white residue |
| CN111232987A (en) * | 2020-04-10 | 2020-06-05 | 昆明理工大学 | Method for efficiently recovering elemental silicon in industrial silicon slag |
| CN112179803A (en) * | 2020-09-29 | 2021-01-05 | 昆明理工大学 | Quantitative analysis method for content of elemental silicon in industrial silicon slag |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302012A (en) * | 2007-05-08 | 2008-11-12 | 黄东 | Purification process of photovoltaic silicon for solar cell |
| CN101948112A (en) * | 2010-09-16 | 2011-01-19 | 陈应天 | The method of a kind of divided silicon and surplus slag |
-
2017
- 2017-07-21 CN CN201710597829.8A patent/CN107601511A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302012A (en) * | 2007-05-08 | 2008-11-12 | 黄东 | Purification process of photovoltaic silicon for solar cell |
| CN101948112A (en) * | 2010-09-16 | 2011-01-19 | 陈应天 | The method of a kind of divided silicon and surplus slag |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675306A (en) * | 2018-05-30 | 2018-10-19 | 云南永昌硅业股份有限公司 | A kind of method of silicon metal in high efficiente callback white residue |
| CN108675306B (en) * | 2018-05-30 | 2021-11-16 | 云南永昌硅业股份有限公司 | Method for efficiently recovering silicon metal in silicon slag |
| CN111232987A (en) * | 2020-04-10 | 2020-06-05 | 昆明理工大学 | Method for efficiently recovering elemental silicon in industrial silicon slag |
| CN112179803A (en) * | 2020-09-29 | 2021-01-05 | 昆明理工大学 | Quantitative analysis method for content of elemental silicon in industrial silicon slag |
| CN112179803B (en) * | 2020-09-29 | 2022-03-01 | 昆明理工大学 | Quantitative analysis method for content of elemental silicon in industrial silicon slag |
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Application publication date: 20180119 |