CN104909400A - Treatment system and treatment method of chlorosilane slurry raffinate - Google Patents
Treatment system and treatment method of chlorosilane slurry raffinate Download PDFInfo
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- CN104909400A CN104909400A CN201410092484.7A CN201410092484A CN104909400A CN 104909400 A CN104909400 A CN 104909400A CN 201410092484 A CN201410092484 A CN 201410092484A CN 104909400 A CN104909400 A CN 104909400A
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/584—Recycling of catalysts
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Abstract
The invention provides a treatment system and a treatment method of chlorosilane slurry raffinate. The treatment method comprises the following steps: carrying out solid-liquid separation on chlorosilane slurry raffinate to obtain a first filtrate and a first solid phase solid phase; carrying out subsection distillation on the first filtrate to obtain a silicon tetrachloride crude product and a hexachlorodisilane crude product; mixing the first solid phase and water, and filtering to obtain a second filtrate and a silicon powder; mixing the second filtrate and an alkaline substance containing an amino group, and filtering to obtain a third filtrate and a second solid phase; and heating the third filtrate to obtain copper hydroxide. In comparison with the prior art, chlorosilane is separated from the silicon powder and a metal chloride impurity through solid-liquid separation, silicon tetrachloride and hexachlorodisilane are separated due to different boiling points, and simultaneously, copper ion in the metal chloride is separated from other metals by forming cuprammonium-ion so as to recycle a catalyst. The treatment method is simple and low-cost. In addition, consumption of lye and water resources for treating raffinate are also minimized, and environmental stress is greatly reduced.
Description
Technical field
The invention belongs to chlorosilane production field, particularly relate to treatment system and the treatment process of chlorosilane slag slurry raffinate.
Background technology
In recent years, along with the fast development of photovoltaic industry, the demand of solar cell to semiconductor silicon (comprising polysilicon, silicon single crystal and thin film silicon) also increases day by day.Crystalline silicon material is topmost photovoltaic material, and its share of market more than 90%, and is also still the mainstay material of solar cell in one quite long from now on period.
At present, produce main technique or the chemical process of crystalline silicon material in the world, comprise Siemens Method and the silane thermal decomposition process developed rapidly and the fluidized bed process etc. of comparative maturity.Adopt these methods to produce crystalline silicon material, chlorosilane is all its necessary intermediates.
Common chlorosilane comprises silicon tetrachloride (SiCl
4), trichlorosilane (SiHCl
3), dichlorosilane (SiH
2cl
2) and disilicone hexachloride (Si
2cl
6) etc.Silicon tetrachloride, trichlorosilane and dichlorosilane are mainly the intermediate raw material alive of Siemens Method and silane thermal decomposition process production of polysilicon, also a large amount of for the manufacture of photoconductive fiber, extension, etching, chemical vapour deposition and thermal silica etc.Disilicone hexachloride can be used to make amorphous si film and epitaxial film (as SiN, SiGe, SiC etc.) thereof, is used in silicon manufacture increasingly extensively.Relative to traditional silane or dichlorosilane vapour deposition process, Si
2cl
6depositing temperature is low, selectivity is high, density of film is even and superior performance, Si in addition
2cl
6also be the extremely highly active reductor of one, the raw material of optical fiber raw material, glass and silicoethane etc.
In chlorosilane is produced, no matter be synthesizing trichlorosilane or prepare trichlorosilane by hydro-reduction, or disproportionation between various chlorosilane or anti-disproportionation reaction, a large amount of slag slurry raffinates can be produced all unavoidably in its corresponding reaction unit and purification process.In production of polysilicon, slag slurry raffinate, mainly from devices such as hydrogenation of silicon tetrachloride reduction, trichlorosilane synthesis, chlorosilane separating-purifyings, especially adopts cold hydrogenation process, and the slag slurry raffinate amount of cold hydrogenation apparatus and the discharge of separating-purifying device increases greatly.The principle that trichlorosilane prepared by cold hydro-reduction silicon tetrachloride is as follows:
It is high that trichlorosilane specific heat hydrogenation efficiency is prepared in cold hydrogenation, but need to add catalyzer in reaction, and the quantity discharged of slag slurry raffinate too increases a lot.The slag slurry raffinate of chlorosilane be usually all bottom Reaktionsofen, separator bottom or rectifier bottoms discharge, so its chlorosilane composition is mainly based on silicon tetrachloride, another containing part disilicone hexachloride and high boiling point polymeric silane, solid is then mainly the muriate of silica flour, catalyzer and other metallic impurity.The reaction of disilicone hexachloride and water or moisture can discharge HCl gas usually; this gas can attack Si-Si bond; this comprises the hydrolysate of Si-H-by producing; it decomposes when mechanical contact; such as due to the mechanical contact caused that rubs; and produce spark; the hydrolysate of solid form even can have under water and pyrotechnically decomposes; it is more dangerous that this just makes the slag slurry raffinate not through reclaiming directly enter three-protection design; often explosion is had to send; hydrolyzate can often spill, and even crosses the filter cake be filtered dry after hydrolysis and all also has explosion in transit.The principle of process chlorosilane slag slurry raffinate is as follows:
Si
4++ 4Cl
-+ 2H
2o → 4HCl ↑+SiO
2↓ (absorbing chlorosilane with water)
H
++ OH
-→ H
2o(neutralization reaction)
According to statistics; cold hydrogenation is adopted to prepare trichlorosilane; average often production one ton of trichlorosilane can produce chlorosilane slag slurry raffinate 0.04 ton; namely the cold hydrogenation apparatus producing 100000 tons of trichlorosilanes per year can produce chlorosilane slag slurry raffinate 4000 tons for 1 year; if energy efficient recovery useful component wherein; this not only can save a lot of Material Costs; and the financial resource and material resource manpower of process spent by these raffinates can be greatly reduced; the prior solid liquid waste entered environment be the reduction of in production, fundamentally protects ecotope not contaminated.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is the treatment system and the treatment process that provide chlorosilane slag slurry raffinate, silicon tetrachloride, disilicone hexachloride, silica flour and catalyzer in the recyclable raffinate of the method.
The invention provides treatment system and the treatment process of a kind of chlorosilane slag slurry raffinate, chlorosilane slag slurry raffinate is carried out solid-liquid separation by the method, obtains the first filtrate and the first solid phase; Described first filtrate is carried out stepwise distillation, obtains silicon tetrachloride crude product and disilicone hexachloride crude product; Described first solid phase is mixed with water, filters, obtain the second filtrate and silica flour; Described second filtrate is mixed with the alkaline matter comprising amino, filters, obtain the 3rd filtrate and second solid phase; By described 3rd filtrate heating, obtain copper hydroxide.Compared with prior art, the present invention passes through solid-liquid separation, chlorosilane and silica flour and metallic chloride impurities are separated, be separated by silicon tetrachloride is different from disilicone hexachloride boiling point, cupric ion in metal chloride passed through to form ammino cupric ion and other metal separation simultaneously, thus recyclable catalyzer, treatment process is simple, cost is low, and decreases the alkali lye of process spent by raffinate and water resources, significantly reduces environmental stress.
Accompanying drawing explanation
Fig. 1 is the treatment system schematic diagram of chlorosilane slag of the present invention slurry raffinate;
Fig. 2 is the embodiment of the present invention 1 main device system used used and schematic flow sheet.
Embodiment
The invention provides the treatment process of a kind of chlorosilane slag slurry raffinate, comprising:
Chlorosilane slag slurry raffinate is carried out solid-liquid separation, obtains the first filtrate and the first solid phase;
Described first filtrate is carried out stepwise distillation, obtains silicon tetrachloride crude product and disilicone hexachloride crude product;
Described first solid phase is mixed with water, filters, obtain the second filtrate and silica flour;
Described second filtrate is mixed with the alkaline matter comprising amino, filters, obtain the 3rd filtrate and second solid phase;
By described 3rd filtrate heating, obtain copper hydroxide.
Wherein, described chlorosilane slag slurry raffinate is the slag slurry raffinate produced during chlorosilane well known to those skilled in the art is produced, there is no special restriction, the present invention is preferably cold hydro-reduction silicon tetrachloride and prepares the chlorosilane slag slurry raffinate produced in trichlorosilane process.
Chlorosilane slag slurry raffinate is carried out solid-liquid separation, obtains the first filtrate and solid phase.Wherein, the method for described solid-liquid separation is method well known to those skilled in the art, there is no special restriction, and the present invention preferably adopts the one in decant, centrifugation, filtration, press filtration and suction filtration to carry out solid-liquid separation; To contact with air to prevent chlorosilane and produce SiO
2have influence on the recovery of silica flour, prevent chlorosilane from escaping in air simultaneously and endanger Environmental Health, described solid-liquid separation is preferably carried out in airtight device.
Described filtrate is carried out stepwise distillation, obtains silicon tetrachloride crude product and disilicone hexachloride crude product; The method of described stepwise distillation is distillating method well known to those skilled in the art, there is no special restriction, collects the effluent near silicon tetrachloride boiling point and near disilicone hexachloride boiling point, obtains silicon tetrachloride crude product and disilicone hexachloride crude product.
According to the present invention, preferably described silicon tetrachloride crude product is refined, obtain silicon tetrachloride; Described refining method is method well known to those skilled in the art, and there is no special restriction, the present invention preferably adopts rectification and purification; The present invention is also preferred to refine described disilicone hexachloride crude product, obtains disilicone hexachloride; The process for purification of described disilicone hexachloride crude product is method well known to those skilled in the art, and there is no special restriction, the present invention preferably adopts rectification and purification.
Described first filtrate is carried out stepwise distillation, except obtaining silicon tetrachloride crude product and disilicone hexachloride crude product, also has some other impurity, and silicon tetrachloride crude product and disilicone hexachloride crude product carry out refining after, also have the generation of impurity, these impurity preferably pass into and carry out neutralizing hydrolysis process to hydrolysis kettles by the present invention.
After chlorosilane slag slurry raffinate is carried out solid-liquid separation by the present invention, except obtaining the first above-mentioned filtrate, also have the first solid phase, the first solid phase is mainly silica flour and metal chloride, and metal chloride mainly comprises CuCl
2with FeCl
3, AlCl
3described first solid phase mixed with water Deng muriate, metal chloride is soluble in water, filters, obtains the second filtrate and silica flour.This silica flour is preferably also through drying treatment.
Described second filtrate is mixed with the alkaline matter comprising amino, now, the Fe in filtrate
3+with Al
3+become precipitation of hydroxide, and Cu
2+then forming ammino cupric ion is dissolved in solution, filters, can obtain the 3rd filtrate and second solid phase.
By described 3rd filtrate heating, ammino cupric ion decomposes, ammonia is overflowed, and preferably filters, dry, obtains copper hydroxide.
According to the present invention, preferably by copper hydroxide and mixed in hydrochloric acid, there is replacement(metathesis)reaction, obtain CuCl
2solution, after concentrated, obtains solid CuCl
2, it is reusable as catalyzer.
The present invention contacts with air to prevent chlorosilane, and also in order to accelerate treating processes, whole treatment process is preferably carried out under the pressure of 0 ~ 15barA, is more preferably 5 ~ 10barA; The temperature of whole treatment process is preferably-50 DEG C ~ 100 DEG C, is more preferably 0 DEG C ~ 100 DEG C.
The present invention passes through solid-liquid separation, chlorosilane and silica flour and metallic chloride impurities are separated, be separated by silicon tetrachloride is different from disilicone hexachloride boiling point, cupric ion in metal chloride is passed through to form ammino cupric ion and other metal separation simultaneously, thus recyclable catalyzer, treatment process is simple, and cost is low, and decrease the alkali lye of process spent by raffinate and water resources, significantly reduce environmental stress.
Present invention also offers the treatment system of a kind of chlorosilane slag slurry raffinate, its schematic diagram as shown in Figure 1, comprising: equipment for separating liquid from solid (1), mixing device (2), tripping device (3), alkaline setting device (4), tripping device (5), heating unit (6), stepwise distillation device (7); Described mixing device comprises water in (2); Containing comprising amino alkaline matter in described alkaline setting device (4); The solid outlet of described equipment for separating liquid from solid (1) is connected with the import of described mixing device (2); The outlet of described mixing device (2) is connected with the import of alkaline setting device (4) by the liquid exit of tripping device (3); The outlet of described alkaline setting device (4) is connected with the import of heating unit (6) by the liquid exit of tripping device (5); The liquid exit of described equipment for separating liquid from solid (1) is connected with the import of stepwise distillation device (7).Above-mentioned treatment process can adopt this system to carry out.
Chlorosilane slag slurry raffinate is passed in equipment for separating liquid from solid (1), obtain the first filtrate and the first solid, described first solid passes in mixing device (2) by the solid outlet of equipment for separating liquid from solid (1), mix with the water in mixing device (2), pass in tripping device (3) again, obtain the second filtrate and silica flour, second filtrate enters in alkaline setting device (4) by the liquid exit of tripping device (3), mix with the amino alkaline matter that comprises wherein, pass in tripping device (5) again, be separated by tripping device (5) and obtain the 3rd filtrate and second solid phase, 3rd filtrate is passed into by the liquid exit of tripping device (5) heats to heating unit (6), obtain copper hydroxide.
The present invention preferably also comprises replacement(metathesis)reaction device (12), and its import is connected with the solid outlet of heating unit (6), and copper hydroxide carries out replacement(metathesis)reaction with hydrochloric acid in replacement(metathesis)reaction device (12), obtains catalyzer cupric chloride.
First filtrate is entered in stepwise distillation device (7) by the liquid exit of equipment for separating liquid from solid (1), carries out stepwise distillation and obtains silicon tetrachloride crude product and disilicone hexachloride crude product.
According to the present invention, described chlorosilane slag slurry raffinate treatment system preferably also comprises Tetrachlorosilane refining device (8) and disilicone hexachloride refining plant (9).Silicon tetrachloride crude product exports to pass into preferably by first of stepwise distillation device (7) and refines to Tetrachlorosilane refining device (8), thus obtains silicon tetrachloride; Disilicone hexachloride is passed into by the second outlet of stepwise distillation device (7) and refines to disilicone hexachloride refining plant (9), thus obtains disilicone hexachloride.
This treatment system preferably also comprises three wastes processing unit (11), and stepwise distillation device (7), Tetrachlorosilane refining device (8) can pass in three wastes processing unit (11) with the middle impurity produced of disilicone hexachloride refining plant (9) and process.
According to the present invention, this treatment system preferably also comprises solid drying device (10), and the import of described solid drying device (10) is connected with the solid outlet of tripping device (3).In tripping device (3), isolated silica flour carries out drying in solid drying device (10); In addition another import of solid drying device (10) is preferably connected with the outlet of replacement(metathesis)reaction device (12), can be used to dry cupric chloride.
In order to further illustrate the present invention, below in conjunction with embodiment, the treatment system of a kind of chlorosilane slag slurry raffinate provided by the invention and treatment process are described in detail.
Reagent used in following examples is commercially available.
Embodiment 1
Main device system used and schematic flow sheet are as shown in Figure 2.Wherein: F-01 ~ F-04 is filtration unit.T01 is chlorosilane water distilling apparatus; T-02 is silicon tetrachloride rectifier unit; T-03 is two silicon hexachloride rectifier units.R-01 is chlorosilane waste gas, raffinate hydrolysis device; R-02 is metal chloride dissolver; R-03 is that ammonification depositing in water amasss Fe
3+and Al
3+ion; R-04 is the ammonia that heating discharges in ammino cupric ion, deposits Cu (OH)
2; R-05 is hydrochloric acid and Cu Cu (OH)
2replacement(metathesis)reaction still.M-01 is non-condensable gas mixing tank; M-02 is raffinate mixing tank.DRYER-01 is silica powder drying machine; DRYER-02 is CuCl
2drying installation; 1 is chlorosilane slag slurry raffinate; 2 is liquid chlorosilanes mixture; 3 is silica flour and metal chloride; 4 is thick silicon tetrachloride; 5 is thick disilicone hexachloride; 6 is refining disilicone hexachloride; 13 is refining silicon tetrachloride; 7,8,9,14 is chlorosilane non-condensable gas and the disposable chlorosilane of other lower boiling; 10,11,12,15 is chlorosilane raffinate; 16 is water; 17 is silica flour and metal chloride aqueous mixture; 18 is the metal chloride aqueous solution; 19 is moisture silica flour; 20 is water vapor; 21 is dried recovered silica flour; 22 is the mixture of ferric hydroxide precipitate, aluminum hydroxide precipitation and copper ammonia complexation ion, other foreign ion, chlorion, ammoniacal liquor; 23 is 22wt% ammoniacal liquor; 24 is the mixture of copper ammonia complexation ion, other foreign ion, chlorion, ammoniacal liquor; 25 is the solid mixture of ironic hydroxide and aluminium hydroxide; 26 is ammonia; 27 mixtures that are copper hydroxide precipitation, other foreign ion, chlorion; 28 is the mixing solutions of other foreign ion and chlorion; 29 is copper hydroxide solid; 30 is dilute hydrochloric acid; 31 is Cupric Chloride Solution (pH value approximates 6); 32 is weakly acidic water steam; 33 for reclaiming cupric chloride.
Solid and liquid separate by slag slurry raffinate (1) closed filtering device (F-01) of being discharged by 8 tons of cold hydrogenation apparatuss, obtain 1.30 tons of solid filter cakes (3) and 6.70 tons of liquid chlorosilanes (2).Added in evaporating kettle (T-01) by liquid chlorosilanes (2), adopt steam-heated mode, air distillation, low-boiling point material (7) is by mixing tank (M-01) directly venting non-condensable gas house steward (14), and then unification is hydrolyzed to hydrolysis kettle (R-01).Collect the overhead product (4) 5.54 ton of temperature between 50 DEG C ~ 60 DEG C, be detected as the silicon tetrachloride crude product of main content 96%; Continue heating again, after still liquid temp rises to 140 DEG C, collect the overhead product (5) 0.92 ton of temperature between 140 DEG C ~ 150 DEG C, detect the disilicone hexachloride crude product that its main content is 93%, stop heating.By high boiling material at the bottom of still (10) by mixing tank (M-02) directly venting raffinate house steward (15), then unification enters in hydrolysis kettle (R-01) and is hydrolyzed.Be passed into by the silicon tetrachloride crude product (4) distilled in (T-02) after rectification and purification, obtain the silicon tetrachloride (13) 5.11 tons of main content 99%, the light constituent (8) separated goes non-condensable gas house steward, and heavy constituent (11) goes raffinate house steward.After disilicone hexachloride crude product (5) being passed into (T-03) middle rectification and purification, obtain the disilicone hexachloride (6) that the main content of 810kg is greater than 99%, the light constituent (9) separated goes non-condensable gas house steward, heavy constituent (12) goes raffinate house steward, and then enter in hydrolysis kettle (R-01) and be hydrolyzed, be discharged to three wastes processing unit outside hydrolyzate (34) and carry out neutralizing treatment.
1.30 of above-mentioned gained tons of filter cakes (3) and 1.5 tons of water (16) are joined in (R-02), is heated to 50 DEG C and stirs simultaneously, the muriate in filter cake being fully dissolved in the water, obtaining mixture (17), filter with filtration unit (F-02).Filter cake (19) is mainly silica flour, and dry at being placed in baker (DRYER-01) 125 DEG C, water vapour (20) is directly disposed in air, obtains 940kg and reclaims silica flour (21).Main containing Catalysts Cu Cl in filtrate (18)
2and FeCl
3, AlCl
3deng metal chloride, add (23) 800k
gcontent is the ammoniacal liquor (ensureing that ammoniacal liquor is excessive) of 22wt%, makes the Fe in solution (18)
3+and Al
3+become precipitation of hydroxide (22), filtered by filtration unit (F-03), Cu
2+becoming ammino cupric ion stays in solution (24), with Fe (OH)
3with Al (OH)
3solid (25) is separated, then is added hot filtrate (24) by reactor (R-04) ammonia (26) is thrown out, then slowly have Cu (OH)
2solid is precipitated out from solution (27), is filtered, obtain pure Cu (OH) by (F-03)
2(29), other muriate be then present in filtrate (28) separated fall.Pure Cu (OH)
2(29) there is replacement(metathesis)reaction (controlling pH value about 6) with appropriate dilute hydrochloric acid (30) in (R-05) middle mixing, obtain (31) CuCl
2solution, by solution by (DRYER-02) concentrate drying, weakly acidic water vapor (32) removes three wastes processing unit, finally obtains the pure CuCl of 190kg
2catalyzer (33).
The recovery situation of useful component involved in chlorosilane slag slurry raffinate gathers as shown in table 1.
Table 1 chlorosilane slag slurry raffinate main component and the situation of recovery
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a treatment process for chlorosilane slag slurry raffinate, is characterized in that, comprising:
Chlorosilane slag slurry raffinate is carried out solid-liquid separation, obtains the first filtrate and the first solid phase;
Described first filtrate is carried out stepwise distillation, obtains silicon tetrachloride crude product and disilicone hexachloride crude product;
Described first solid phase is mixed with water, filters, obtain the second filtrate and silica flour;
Described second filtrate is mixed with the alkaline matter comprising amino, filters, obtain the 3rd filtrate and second solid phase;
By described 3rd filtrate heating, obtain copper hydroxide.
2. treatment process according to claim 1, is characterized in that, the method for described solid-liquid separation is the one in decant, centrifugation, filtration, press filtration and suction filtration.
3. treatment process according to claim 1, is characterized in that, described solid-liquid separation is carried out in closed unit.
4. treatment process according to claim 1, is characterized in that, also comprises:
Described silicon tetrachloride crude product is refined, obtains silicon tetrachloride.
5. treatment process according to claim 1, is characterized in that, also comprises:
Described disilicone hexachloride crude product is refined, obtains disilicone hexachloride.
6. treatment process according to claim 1, is characterized in that, described in comprise amino alkaline matter be ammoniacal liquor.
7. treatment process according to claim 1, is characterized in that, the pressure of described treatment process is 0 ~ 15barA, and temperature is-50 DEG C ~ 100 DEG C.
8. the treatment system of a chlorosilane slag slurry raffinate, it is characterized in that, comprising: equipment for separating liquid from solid (1), mixing device (2), tripping device (3), alkaline setting device (4), tripping device (5), heating unit (6), stepwise distillation device (7); Described mixing device comprises water in (2); Containing comprising amino alkaline matter in described alkaline setting device (4);
The solid outlet of described equipment for separating liquid from solid (1) is connected with the import of described mixing device (2);
The outlet of described mixing device (2) is connected with the import of alkaline setting device (4) by the liquid exit of tripping device (3);
The outlet of described alkaline setting device (4) is connected with the import of heating unit (6) by the liquid exit of tripping device (5);
The liquid exit of described equipment for separating liquid from solid (1) is connected with the import of stepwise distillation device (7).
9. treatment system according to claim 8, is characterized in that, also comprises Tetrachlorosilane refining device (8) and disilicone hexachloride refining plant (9);
First outlet of described stepwise distillation device (7) is connected with the import of Tetrachlorosilane refining device (8);
Second outlet of described stepwise distillation device (7) is connected with the import of disilicone hexachloride refining plant (9).
10. treatment system according to claim 8, is characterized in that, also comprises solid drying device (10); The import of described solid drying device (10) is connected with the solid outlet of tripping device (3).
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| CN106946261A (en) * | 2017-04-06 | 2017-07-14 | 洛阳中硅高科技有限公司 | The retracting device of disilicone hexachloride |
| CN106966397A (en) * | 2017-04-06 | 2017-07-21 | 洛阳中硅高科技有限公司 | The recovery method of disilicone hexachloride |
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| CN113666376A (en) * | 2021-08-23 | 2021-11-19 | 武汉纺织大学 | Recycling treatment method for silicon slag |
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| CN106946261A (en) * | 2017-04-06 | 2017-07-14 | 洛阳中硅高科技有限公司 | The retracting device of disilicone hexachloride |
| CN106966397A (en) * | 2017-04-06 | 2017-07-21 | 洛阳中硅高科技有限公司 | The recovery method of disilicone hexachloride |
| CN108569700A (en) * | 2018-07-10 | 2018-09-25 | 四川绿源聚能环保科技有限责任公司 | A kind of technique of recycling chlorosilane dreg slurry |
| CN111072031A (en) * | 2019-12-10 | 2020-04-28 | 新疆东方希望新能源有限公司 | Chlorosilane silicon powder filtering system and filtering method thereof |
| CN113666376A (en) * | 2021-08-23 | 2021-11-19 | 武汉纺织大学 | Recycling treatment method for silicon slag |
| CN113666376B (en) * | 2021-08-23 | 2023-03-03 | 武汉纺织大学 | Recycling treatment method for silicon slag |
| CN114524408A (en) * | 2022-02-14 | 2022-05-24 | 浙江大学 | Environment-friendly comprehensive recycling method of organic silicon pulp residues |
| 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: 20150916 |