CN106698441A - Treating method for residual liquid and slag slurry produced in polysilicon production - Google Patents
Treating method for residual liquid and slag slurry produced in polysilicon production Download PDFInfo
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Abstract
The invention discloses a treating method for residual liquid and slag slurry produced in polysilicon production, wherein the residual liquid and slag slurry contains silicon and silicon tetrachloride. The method comprises a step of adding a catalyst into the residual liquid and slag slurry so as to allow silicon to react with silicon tetrachloride so as to produce hexachlorodisilane. According to the treating method, through a synthesis reaction for hexachlorodisilane, the content of hexachlorodisilane in the residual liquid and slag slurry is increased, so residual liquid and slag slurry with high added value are obtained, and the economic performance of a hexachlorodisilane recovery process is improved; both solid waste and liquid waste produced in polysilicon production are reasonably converted and recycled, so treating cost for the residual liquid and slag slurry is lowered, and recovery of high-added-value products are realized; bottleneck problems in treating of the residual liquid and slag slurry during polysilicon production are overcome, and products of polysilicon production are diversified; and the discharge amounts of waste gas, waste water and industrial residues during polysilicon production are greatly reduced, and polysilicon production becomes environment-friendlier.
Description
Technical field
The invention belongs to technical field of polysilicon production, and in particular to a kind of production of polysilicon
In raffinate and slurry processing method.
Background technology
With the rapid growth of polysilicon demand, the scale of production of polysilicon factory is also in day
Benefit expands, and the production capacity that Duo Jia polysilicons factory has reached ton is had at present.Polysilicon
The production capacity of production expands, the synthesis of production of polysilicon trichlorosilane, hydrogenation of silicon tetrachloride operation
The raffinate and slurry material of discharge are also more and more in (including heat hydrogenation and cold hydrogenation).
The main composition of these raffinates and slurry material is：The silicon tetrachloride of 40wt%~70wt% and
The list silicon atom such as trichlorosilane component, the hexachloro-silane of 5wt%~20wt% and chlordene two
Many silicon atoms such as double silicon atom components such as siloxanes, the silane of eight chlorine three of 5wt%~10wt%
The solid impurities such as component, the silica flour of 5wt%~30wt% and metal chloride.Because difference is more
The raw material and technological parameter that crystal silicon factory is used are not quite similar, the change of above-mentioned composition
Scope is very big.Treatment at present to raffinate and slurry material is main using the side for drying evaporation
Method reclaims most of silicon tetrachloride therein and trichlorosilane, and remaining component directly enters water-filling
Solution treatment.Silicic acid and hydrogen chloride can be produced during hydrolyzing chlorosilane, therefore uses hydrolysis process
When need substantial amounts of alkali to be neutralized, this not only causes the waste containing silicon material,
Improve the cost for the treatment of.In addition, after raffinate and slurry material are dried evaporation, its
In hexachloro-silane content it is relatively low, it is not reclaimed typically, but directly
Be hydrolyzed treatment, and hexachloro-silane etc. can also produce hydrogen when hydrolyzing, and be obtained after drying
The solid waste that arrives is inflammable in itself, to impact sensitive, the danger of hydrolysis operation is very high.
Hexachloro-silane is widely used, can be used as efficient deoxidier, it can also be used to manufacture
The N-Si film of high-quality, the market price is very high.Raffinate and slurry in production of polysilicon
Hexachloro-silane component in material has high added value, current hexachloro-silane
Recovery technology is used to the direct rectifying of clean filtrate after raffinate and slurry material filtering,
To isolate valuable hexachloro-silane from chlorosilane.But in actual production of polysilicon
Hexachloro-silane constituent content in raffinate and slurry material is very low, and therefrom reclaims out height
The hexachloro-silane of purity needs multistage rectification again, i.e., first chlorosilane is slightly evaporated, so
Dehydrogenation and de- weight are carried out to hexachloro-silane afterwards, equipment investment is larger.Therefore directly use
Economy is not high when filtering, rectifying recovery technology.
The content of the invention
The technical problems to be solved by the invention be directed to present in prior art it is above-mentioned not
Foot, there is provided the processing method of raffinate and slurry in a kind of production of polysilicon, by chlordene
The synthetic reaction of disilane, improves the content of hexachloro-silane in raffinate and slurry.
The technical scheme that solution present invention problem is used is to provide a kind of polysilicon and gives birth to
The processing method of raffinate and slurry in product, includes silicon and four in the raffinate and slurry
Silicon chloride, methods described includes step：A) to adding catalyst in the raffinate and slurry,
So that the silicon and silicon tetrachloride reaction generation hexachloro-silane.
Preferably, the catalyst for being added in the step a) is catalytic amount.
Preferably, the catalyst is the one kind in complex compound, the complex compound of nickel of copper
Or it is several.
Preferably, the catalyst is [Cu (C12H8)2]BF4、{Cu[(Ph)2PCH2
CH2CH2P(Ph)2]2}Cl、{Cu[P(Ph)3]3}Cl、
[(Ph)2PFcP(Ph)2]Ni(PhNCOCH3) in one or more.Wherein, [Cu
(C12H8)2]BF4Molecular structure it is as follows：
{Cu[(Ph)2PCH2CH2CH2P(Ph)2]2Cl molecular structure it is as follows：
{Cu[P(Ph)3]3Cl molecular structure it is as follows：
[(Ph)2PFcP(Ph)2]Ni(PhNCOCH3) molecular structure it is as follows：
Preferably, the content of the silicon tetrachloride in the raffinate and slurry is 40
Wt%~70wt%.
Preferably, the catalyst and the mol ratio of the silicon tetrachloride are 1:
(200~1000).
Preferably, the silicon generates the reaction temperature of hexachloro-silane with silicon tetrachloride reaction
It is 30~250 DEG C to spend, and the reaction time is 4~24 hours.
Preferably, the silicon generates the reaction temperature of hexachloro-silane with silicon tetrachloride reaction
Spend is 100~200 DEG C.
Preferably, the step a) protect gas under carry out, it is described protection gas be nitrogen,
One kind in hydrogen, inert gas, the protection gas is used to keep anhydrous atmosphere.
The processing method of raffinate and slurry in preferably described production of polysilicon is also wrapped
Include step：
B) reacted raffinate and slurry material are filtered, is removed solid therein miscellaneous
Matter；
C) the clean material of raffinate and slurry after filtering is entered into rectifying column, respectively is isolated by
Heavy constituent hexachloro-silane, light component silicon tetrachloride and trichlorosilane；
D) the heavy constituent hexachloro-silane that will be isolated in step c) sequentially enters other two
Individual rectifying column carries out dehydrogenation and de- weight, respectively is isolated by light in heavy constituent hexachloro-silane
Heavy constituent in component, heavy constituent hexachloro-silane, obtains the hexachloro-silane of high-purity.
The processing method of raffinate in production of polysilicon and slurry in the present invention, by six
The synthetic reaction of chlorine disilane, improves the content of hexachloro-silane in raffinate and slurry,
The raffinate and slurry of high added value are obtained, the economy of hexachloro-silane recovery process is improved
Property；Polysilicon is useless while carrying out rational conversion and reclaiming sharp into the solid waste in product, liquid
With, reduce raffinate and slurry processing cost while realize high value added product return
Receive；Raffinate and the bottleneck problem of slurry treatment in production of polysilicon are solved, makes polysilicon
The product diversification of production；The discharge capacity of the three wastes in being produced on polysilicon is significantly reduced,
Make the production more environmental protection of polysilicon.
Brief description of the drawings
Fig. 1 is the processing system of raffinate in the production of polysilicon of the embodiment of the present invention 2 and slurry
System figure.
In figure：1- stirred tank reactors；2- filters；3- topping stills；31- topping stills
Tower top；The tower reactor of 32- topping stills；4- hexachloro-silane lightness-removing columns；41- hexachloro-silanes take off
The tower top of light tower；The tower reactor of 42- hexachloro-silane lightness-removing columns；5- hexachloro-silane weight-removing columns；
The tower top of 51- hexachloro-silane weight-removing columns；The tower reactor of 52- hexachloro-silane weight-removing columns.
Specific embodiment
To make those skilled in the art more fully understand technical scheme, tie below
The drawings and specific embodiments are closed to be described in further detail the present invention.
Embodiment 1
The present embodiment provides the processing method of the raffinate and slurry in a kind of production of polysilicon,
Include silicon and silicon tetrachloride in the raffinate and slurry, methods described includes step：a)
To adding catalyst in the raffinate and slurry so that the silicon is anti-with the silicon tetrachloride
Hexachloro-silane should be generated.
The processing method of raffinate in production of polysilicon and slurry in the present embodiment, passes through
The synthetic reaction of hexachloro-silane, improves the content of hexachloro-silane in raffinate and slurry,
The raffinate and slurry of high added value are obtained, the economy of hexachloro-silane recovery process is improved
Property；Polysilicon is useless while carrying out rational conversion and reclaiming sharp into the solid waste in product, liquid
With, reduce raffinate and slurry processing cost while realize high value added product return
Receive；Raffinate and the bottleneck problem of slurry treatment in production of polysilicon are solved, makes polysilicon
The product diversification of production；The discharge capacity of the three wastes in being produced on polysilicon is significantly reduced,
Make the production more environmental protection of polysilicon.
Embodiment 2
As shown in figure 1, the present embodiment provides raffinate and slurry in a kind of production of polysilicon
Processing method, silicon and silicon tetrachloride are included in the raffinate and slurry, it is specific this
The main composition of raffinate and slurry material in embodiment for 1.7wt% trichlorosilane,
The silicon tetrachloride of 64.9wt%, the hexachloro-silane of 11.0wt%, the silica flour of 12wt%, its
Remaining component is metal chloride, organochlorosilane, high boiling point silicon oil etc..Methods described includes
Step：A) in the case where gas nitrogen is protected, to the raffinate and slag in stirred tank reactor 1
The catalyst of catalytic amount, the mol ratio of the catalyst and the silicon tetrachloride are added in slurry
It is 1:500, the catalyst is the complex compound [Cu (C of copper12H8)2]BF4So that it is described
Silicon at 100 DEG C, reacts 6 hours with the silicon tetrachloride, generates hexachloro-silane, its
In, by the hexachloro-silane in the reacted raffinates of step a) and slurry
Content is 31.2wt%, and the protection gas is used to keep anhydrous atmosphere.Specific polycrystalline
Trichlorosilane synthesis procedure and hydrogenation of silicon tetrachloride operation in silicon production process can all be produced
Raffinate and slurry, all include silicon and silicon tetrachloride, trichlorine hydrogen in these raffinates and slurry
The contained substance phase of raffinate and slurry material in silicon synthesis procedure and hydrogenation of silicon tetrachloride operation
Seemingly, difference is the proportion difference shared by contained substance.By the catalysis of catalyst
Effect causes that the raffinate in production of polysilicon and the silicon in slurry react with the silicon tetrachloride
Generation hexachloro-silane, substantially increases six in the raffinate and slurry in production of polysilicon
The content of chlorine disilane, is easy to the treatment of subsequent process steps.
The processing method of raffinate in production of polysilicon and slurry in the present embodiment, passes through
The synthetic reaction of hexachloro-silane, improves the content of hexachloro-silane in raffinate and slurry,
The raffinate and slurry of high added value are obtained, the economy of hexachloro-silane recovery process is improved
Property；Polysilicon is useless while carrying out rational conversion and reclaiming sharp into the solid waste in product, liquid
With, reduce raffinate and slurry processing cost while realize high value added product return
Receive；Raffinate and the bottleneck problem of slurry treatment in production of polysilicon are solved, makes polysilicon
The product diversification of production；The discharge capacity of the three wastes in being produced on polysilicon is significantly reduced,
Make the production more environmental protection of polysilicon.
Preferably, stirred tank reactor 1 is flow reactor.Certainly, it is described to stir
It can also be batch reactor to mix kettle reactor 1.
Preferably, in the step a), when the raffinate and slurry material that need to process are less
And when can not realize the continuous operation of follow-up rectification working process, can be in stirred tank reactor 1
The silicon tetrachloride and silica flour of stoichiometric proportion is added to improve the yield of hexachloro-silane.
B) reacted raffinate and slurry material are filtered by filter 2, is removed
Solid impurity therein；Preferably, it is described to be filtered into press filtration, vacuum filter or centrifugation
One kind in press filtration.
Main component in the filter cake or filter residue that are obtained after filtering for metal chloride (wherein,
Metal chloride is mainly the chloride of copper, iron, aluminium, titanium) unreacted silica flour, urge
Agent, contains unreacted silica flour, in order to fill in the filter cake obtained after filtering or filter residue
Point utilize silica flour, therefore enter during filter cake or filter residue can return to stirred tank reactor 1
Row reaction, while catalyst can also be recycled；Metal chlorination in filter cake or filter residue
During the too high levels of thing, the treatment that can directly be hydrolyzed is then outer to arrange to remove chlorosilane.
C) the clean material of raffinate and slurry after filtering is entered into rectifying column, respectively is isolated by
Heavy constituent hexachloro-silane, light component silicon tetrachloride and trichlorosilane；
Rectifying column in specific step c) is topping still 3, is made in the rectifying of topping still 3
Under, light component silicon tetrachloride and trichlorosilane, light group are obtained in the tower top 31 of topping still
Point silicon tetrachloride and trichlorosilane are participated in again in can reentering stirred tank reactor 1
Reaction, it is also possible to enter polycrystalline silicon production system；Recombinated in the tower reactor 32 of topping still
Divide hexachloro-silane, heavy constituent hexachloro-silane namely thick hexachloro-silane.Specifically,
The operating pressure of the topping still 3 in step c) is 0.1MPa, the temperature of tower top 31 of topping still
It is 57.1 DEG C to spend, and the theoretical stage of topping still 3 is 75, and reflux entry ratio is 0.8.
D) the heavy constituent hexachloro-silane that will be isolated in step c) sequentially enters other two
Individual rectifying column carries out dehydrogenation and de- weight, respectively is isolated by light in heavy constituent hexachloro-silane
Heavy constituent in component, heavy constituent hexachloro-silane, obtains the hexachloro-silane of high-purity.
The heavy constituent hexachloro-silane isolated in step c) sequentially enters two other rectifying
Tower carries out dehydrogenation and de- weight, and the two rectifying columns are followed successively by hexachloro-silane lightness-removing column 4, six
Chlorine disilane weight-removing column 5.Heavy constituent hexachloro-silane initially enters hexachloro-silane lightness-removing column
4, the light component such as organochlorosilane therein is such as：Allyl chloride etc. is from hexachloro-silane
Downstream treatment process is delivered in the extraction of tower top 41 of lightness-removing column, from hexachloro-silane lightness-removing column
Tower reactor 42 obtains the hexachloro-silane after taking off gently, and the hexachloro-silane after taking off gently enters back into six
Chlorine disilane weight-removing column 5.In hexachloro-silane weight-removing column 5, the silicon of chlordene two after taking off gently
Heavy constituent in alkane is such as：High boiling point silicon oil is discharged from the tower reactor 52 of hexachloro-silane weight-removing column,
The tower top 51 of hexachloro-silane weight-removing column then produces purity up to the high-purity of more than 99.3wt%
Hexachloro-silane product.The operation of the hexachloro-silane lightness-removing column 4 in specific step d)
Pressure is 0.1MPa, and the temperature of tower top 41 of hexachloro-silane lightness-removing column is 135.7 DEG C, six
The theoretical stage of chlorine disilane lightness-removing column 4 is 55, and reflux entry ratio is 8.5.Specific step
It is rapid d) in the operating pressure of hexachloro-silane weight-removing column 5 be 0.1MPa, the silicon of chlordene two
The temperature of tower top 51 of alkane weight-removing column is 141.5 DEG C, the tower of hexachloro-silane weight-removing column 5
Theoretical stage is 45, and reflux entry ratio is 6.0.
As shown in figure 1, the place of the raffinate and slurry in the above-mentioned production of polysilicon of the present embodiment
Reason method has used the processing system of the raffinate and slurry in production of polysilicon, the system bag
Include：
Stirred tank reactor 1；
Filter 2, the filter 2 is connected with the stirred tank reactor 1；
Topping still 3, the topping still 3 is connected with the filter 2, the topping still 3
The tower reactor 32 of tower top 31 and topping still including topping still；
Hexachloro-silane lightness-removing column 4, the hexachloro-silane lightness-removing column 4 and the topping still
Tower reactor 32 connect, the hexachloro-silane lightness-removing column 4 include hexachloro-silane lightness-removing column
Tower top 41 and hexachloro-silane lightness-removing column tower reactor 42；
Hexachloro-silane weight-removing column 5, the hexachloro-silane weight-removing column 5 and the chlordene two
The tower reactor 42 of silane lightness-removing column is connected, and the hexachloro-silane weight-removing column 5 includes chlordene two
The tower reactor 52 of silane weight-removing column and the tower top 51 of hexachloro-silane weight-removing column.
Embodiment 3
The present embodiment provides the processing method of the raffinate and slurry in a kind of production of polysilicon,
Include silicon and silicon tetrachloride in the raffinate and slurry, it is residual in specific the present embodiment
The main composition of liquid and slurry material is trichlorosilane, the tetrachloro of 40.0wt% of 1.3wt%
SiClx, the hexachloro-silane of 13.3wt%, the silica flour of 14.1wt%, remaining component are metal
Chloride, organochlorosilane, high boiling point silicon oil etc., methods described include step：A) protecting
Under shield gas nitrogen, to adding catalytic amount in the raffinate and slurry in stirred tank reactor
Catalyst, the mol ratio of the catalyst and the silicon tetrachloride is 1:200, the catalysis
Agent is the complex compound { Cu [(Ph) of copper2PCH2CH2CH2P(Ph)2]2Cl and
{Cu[P(Ph)3]3Cl mixture (mass ratio 1:1) so that the silicon and the tetrachloro
SiClx is reacted 18 hours at 250 DEG C, generates hexachloro-silane, wherein, by step
The content of the hexachloro-silane in rapid a) the reacted raffinate and slurry is
38.5wt%, the protection gas is used to keep anhydrous atmosphere.
B) reacted raffinate and slurry material are filtered by filter, is removed it
In solid impurity.
C) the clean material of raffinate and slurry after filtering is entered into rectifying column, respectively is isolated by
Heavy constituent hexachloro-silane, light component silicon tetrachloride and trichlorosilane.
D) the heavy constituent hexachloro-silane that will be isolated in step c) sequentially enters other two
Individual rectifying column carries out dehydrogenation and de- weight, respectively is isolated by light in heavy constituent hexachloro-silane
Heavy constituent in component, heavy constituent hexachloro-silane, obtains the hexachloro-silane of high-purity.
The processing method of raffinate in production of polysilicon and slurry in the present embodiment, passes through
The synthetic reaction of hexachloro-silane, improves the content of hexachloro-silane in raffinate and slurry,
The raffinate and slurry of high added value are obtained, the economy of hexachloro-silane recovery process is improved
Property；Polysilicon is useless while carrying out rational conversion and reclaiming sharp into the solid waste in product, liquid
With, reduce raffinate and slurry processing cost while realize high value added product return
Receive；Raffinate and the bottleneck problem of slurry treatment in production of polysilicon are solved, makes polysilicon
The product diversification of production；The discharge capacity of the three wastes in being produced on polysilicon is significantly reduced,
Make the production more environmental protection of polysilicon.
Embodiment 4
The present embodiment provides the processing method of the raffinate and slurry in a kind of production of polysilicon,
Include silicon and silicon tetrachloride in the raffinate and slurry, it is residual in specific the present embodiment
The main composition of liquid and slurry material is trichlorosilane, the tetrachloro of 70.0wt% of 2.1wt%
SiClx, the hexachloro-silane of 6.7wt%, the silica flour of 10.2wt%, remaining component are metal chlorine
Compound, organochlorosilane, high boiling point silicon oil etc., methods described include step：A) in protection
Under gas nitrogen, to addition catalytic amount in the raffinate and slurry in stirred tank reactor
Catalyst, the catalyst is 1 with the mol ratio of the silicon tetrachloride:1000, the catalysis
Agent is the complex compound [(Ph) of nickel2PFcP(Ph)2]Ni(PhNCOCH3) so that the silicon and institute
Silicon tetrachloride is stated at 30 DEG C, is reacted 24 hours, generate hexachloro-silane, wherein, warp
The content of the hexachloro-silane crossed in the reacted raffinates of step a) and slurry is
27.6wt%, the protection gas is used to keep anhydrous atmosphere.
Embodiment 5
The present embodiment provides the processing method of the raffinate and slurry in a kind of production of polysilicon,
Include silicon and silicon tetrachloride in the raffinate and slurry, it is residual in specific the present embodiment
The main composition of liquid and slurry material is trichlorosilane, the tetrachloro of 55.5wt% of 1.6wt%
SiClx, the hexachloro-silane of 12.5wt%, the silica flour of 13.1wt%, remaining component are metal
Chloride, organochlorosilane, high boiling point silicon oil etc., methods described include step：A) protecting
Under shield gas nitrogen, to adding catalytic amount in the raffinate and slurry in stirred tank reactor
Catalyst, the mol ratio of the catalyst and the silicon tetrachloride is 1:700, the catalysis
Agent is the complex compound [(Ph) of nickel2PFcP(Ph)2]Ni(PhNCOCH3) so that the silicon and institute
Silicon tetrachloride is stated at 100 DEG C, is reacted 10 hours, generate hexachloro-silane, wherein,
By the content of the hexachloro-silane in the reacted raffinates of step a) and slurry
It is 34.7wt%, the protection gas is used to keep anhydrous atmosphere.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present
And the illustrative embodiments for using, but the invention is not limited in this.For ability
For those of ordinary skill in domain, the situation of spirit and substance of the present invention is not being departed from
Under, various changes and modifications can be made therein, and these variations and modifications are also considered as of the invention
Protection domain.
Claims (9)
1. raffinate in a kind of production of polysilicon and the processing method of slurry, the raffinate and
Include silicon and silicon tetrachloride in slurry, it is characterised in that methods described includes step：a)
To adding catalyst in the raffinate and slurry so that the silicon is anti-with the silicon tetrachloride
Hexachloro-silane should be generated.
2. the treatment of the raffinate and slurry in production of polysilicon according to claim 1
Method, it is characterised in that the catalyst is in complex compound, the complex compound of nickel of copper
One or more.
3. the treatment of the raffinate and slurry in production of polysilicon according to claim 2
Method, it is characterised in that the catalyst is [Cu (C12H8)2]BF4、{Cu
[(Ph)2PCH2CH2CH2P(Ph)2]2}Cl、{Cu[P(Ph)3]3}Cl、
[(Ph)2PFcP(Ph)2]Ni(PhNCOCH3) in one or more.
4. the treatment of the raffinate and slurry in production of polysilicon according to claim 1
Method, it is characterised in that the content of the silicon tetrachloride in the raffinate and slurry is
40wt%~70wt%.
5. the treatment of the raffinate and slurry in production of polysilicon according to claim 1
Method, it is characterised in that the catalyst is 1 with the mol ratio of the silicon tetrachloride:
(200~1000).
6. the treatment of the raffinate and slurry in production of polysilicon according to claim 1
Method, it is characterised in that the silicon is anti-with silicon tetrachloride reaction generation hexachloro-silane
It is 30~250 DEG C to answer temperature, and the reaction time is 4~24 hours.
7. the treatment of the raffinate and slurry in production of polysilicon according to claim 6
Method, it is characterised in that the silicon is anti-with silicon tetrachloride reaction generation hexachloro-silane
It is 100~200 DEG C to answer temperature.
8. the treatment of the raffinate and slurry in production of polysilicon according to claim 1
Method, it is characterised in that the step a) protect gas under carry out, it is described protection gas be
One kind in nitrogen, hydrogen, inert gas, the protection gas is used to keep anhydrous gas
Atmosphere.
9. raffinate in the production of polysilicon according to claim 1~8 any one and
The processing method of slurry, it is characterised in that also including step：
B) reacted raffinate and slurry material are filtered, is removed solid therein miscellaneous
Matter；
C) the clean material of raffinate and slurry after filtering is entered into rectifying column, respectively is isolated by
Heavy constituent hexachloro-silane, light component silicon tetrachloride and trichlorosilane；
D) the heavy constituent hexachloro-silane that will be isolated in step c) sequentially enters other two
Individual rectifying column carries out dehydrogenation and de- weight, respectively is isolated by light in heavy constituent hexachloro-silane
Heavy constituent in component, heavy constituent hexachloro-silane, obtains the hexachloro-silane of high-purity.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905438A (en) * | 2020-09-01 | 2020-11-10 | 新疆协鑫新能源材料科技有限公司 | Process and device for drying and mixing residue and filter residue of slurry |
| CN112479213A (en) * | 2020-12-18 | 2021-03-12 | 武汉新硅科技潜江有限公司 | Method for producing electronic-grade hexachlorodisilane by continuous rectification method |
| CN115196635A (en) * | 2022-08-02 | 2022-10-18 | 新特能源股份有限公司 | Method and device for removing carbon-containing impurities and polycrystalline silicon production system |
| CN115557506A (en) * | 2022-09-26 | 2023-01-03 | 新特能源股份有限公司 | Slag slurry treatment process and device in polycrystalline silicon production process |
| CN116102018A (en) * | 2022-11-11 | 2023-05-12 | 石河子大学 | Method for separating hexachlorodisilane from polysilicon byproduct oligomeric chlorosilane |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011067331A1 (en) * | 2009-12-02 | 2011-06-09 | Spawnt Private S.À.R.L. | Method for producing hexachlorodisilane |
| CN103011173A (en) * | 2012-12-18 | 2013-04-03 | 江南大学 | Synthetic method for hexachlorodisilane |
| CN103180247A (en) * | 2010-11-09 | 2013-06-26 | 赢创德固赛有限公司 | Process for preparing trichlorosilane |
| CN104402002A (en) * | 2014-11-13 | 2015-03-11 | 李金金 | Device and method for treating chlorosilane slag slurry through extraction method |
-
2015
- 2015-08-03 CN CN201510482431.0A patent/CN106698441A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011067331A1 (en) * | 2009-12-02 | 2011-06-09 | Spawnt Private S.À.R.L. | Method for producing hexachlorodisilane |
| CN103180247A (en) * | 2010-11-09 | 2013-06-26 | 赢创德固赛有限公司 | Process for preparing trichlorosilane |
| CN103011173A (en) * | 2012-12-18 | 2013-04-03 | 江南大学 | Synthetic method for hexachlorodisilane |
| CN104402002A (en) * | 2014-11-13 | 2015-03-11 | 李金金 | Device and method for treating chlorosilane slag slurry through extraction method |
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| CN111905438A (en) * | 2020-09-01 | 2020-11-10 | 新疆协鑫新能源材料科技有限公司 | Process and device for drying and mixing residue and filter residue of slurry |
| CN112479213A (en) * | 2020-12-18 | 2021-03-12 | 武汉新硅科技潜江有限公司 | Method for producing electronic-grade hexachlorodisilane by continuous rectification method |
| CN112479213B (en) * | 2020-12-18 | 2023-09-19 | 武汉新硅科技潜江有限公司 | Method for producing electronic grade hexachlorodisilane by continuous rectification method |
| CN115196635A (en) * | 2022-08-02 | 2022-10-18 | 新特能源股份有限公司 | Method and device for removing carbon-containing impurities and polycrystalline silicon production system |
| CN115196635B (en) * | 2022-08-02 | 2023-10-27 | 新特能源股份有限公司 | Method and device for removing carbon-containing impurities and polysilicon production system |
| CN115557506A (en) * | 2022-09-26 | 2023-01-03 | 新特能源股份有限公司 | Slag slurry treatment process and device in polycrystalline silicon production process |
| CN115557506B (en) * | 2022-09-26 | 2024-04-26 | 新特能源股份有限公司 | Slag slurry treatment process and device in polycrystalline silicon production process |
| CN116102018A (en) * | 2022-11-11 | 2023-05-12 | 石河子大学 | Method for separating hexachlorodisilane from polysilicon byproduct oligomeric chlorosilane |
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Application publication date: 20170524 |