CN111072032B - Chlorosilane raffinate filtration system and method - Google Patents
Chlorosilane raffinate filtration system and method Download PDFInfo
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- CN111072032B CN111072032B CN202010060396.4A CN202010060396A CN111072032B CN 111072032 B CN111072032 B CN 111072032B CN 202010060396 A CN202010060396 A CN 202010060396A CN 111072032 B CN111072032 B CN 111072032B
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- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 91
- 238000001914 filtration Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 115
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 94
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 40
- 239000004744 fabric Substances 0.000 claims abstract description 30
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 29
- 238000003860 storage Methods 0.000 claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 15
- 239000012065 filter cake Substances 0.000 claims description 62
- 230000007062 hydrolysis Effects 0.000 claims description 26
- 238000006460 hydrolysis reaction Methods 0.000 claims description 26
- 239000002002 slurry Substances 0.000 claims description 16
- 239000002893 slag Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 abstract description 18
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract description 12
- 239000002244 precipitate Substances 0.000 abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 26
- 239000011863 silicon-based powder Substances 0.000 description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 229910001510 metal chloride Inorganic materials 0.000 description 11
- 239000007787 solid Substances 0.000 description 11
- 239000007921 spray Substances 0.000 description 10
- 239000011148 porous material Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 238000012423 maintenance Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 230000000712 assembly Effects 0.000 description 6
- 238000000429 assembly Methods 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 6
- 229920005591 polysilicon Polymers 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000005909 Kieselgur Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000013312 flour Nutrition 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 4
- 239000005052 trichlorosilane Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910003902 SiCl 4 Inorganic materials 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 3
- CYVTYWBDUINCRE-UHFFFAOYSA-N [Si].[SiH3]Cl Chemical compound [Si].[SiH3]Cl CYVTYWBDUINCRE-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 239000011152 fibreglass Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D24/00—Filters comprising loose filtering material, i.e. filtering material without any binder between the individual particles or fibres thereof
- B01D24/02—Filters comprising loose filtering material, i.e. filtering material without any binder between the individual particles or fibres thereof with the filter bed stationary during the filtration
- B01D24/10—Filters comprising loose filtering material, i.e. filtering material without any binder between the individual particles or fibres thereof with the filter bed stationary during the filtration the filtering material being held in a closed container
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The application discloses a chlorosilane raffinate filtering system and a chlorosilane raffinate filtering method, wherein the system comprises: the stirrer is provided with a diatomite inlet, a silicon tetrachloride inlet and a mixture outlet; the nitrogen storage tank is connected with the stirrer through a first pipeline, and a first valve is arranged on the first pipeline; the filter is internally provided with a filter element which is arranged along the axial direction of the filter element, the lower end of the filter element is sealed, the side wall of the filter element is wrapped with filter cloth, the upper port of the filter element is communicated with the clean liquid cavity, a pressure difference detection device is arranged between the clean liquid cavity and the feed cavity, the clean liquid cavity is provided with a chlorosilane clear liquid outlet, the mixture outlet is communicated with the feed cavity through a second pipeline, and the second pipeline is provided with a second valve; the chlorosilane residual liquid storage tank is connected with the feeding cavity through a third pipeline, and a third valve is arranged on the third pipeline. The system can solve the problems that amorphous silicon and aluminum chloride precipitates in chlorosilane residual liquid are difficult to filter and the filtering cost is high in the prior art.
Description
Technical Field
The application belongs to the field of polysilicon, and particularly relates to a chlorosilane residual liquid filtering system and a chlorosilane residual liquid filtering method.
Background
The improved Siemens method produces a great amount of silicon tetrachloride as a byproduct in the process of producing polysilicon. At present, more than 90% of polysilicon enterprises all adopt silicon tetrachloride cold hydrogenation technology for treatmentThe byproduct is converted into trichlorosilane which is a raw material for producing polysilicon. The cold hydrogenation technology of silicon tetrachloride is to react metallurgical grade silicon powder, hydrogen and silicon tetrachloride under the condition of certain temperature and pressure under the action of a catalyst to generate trichlorosilane. Since metallurgical grade silicon powder contains metal impurities, fine silicon powder and metal impurities are introduced into the hydrogenated product (chlorosilane). In the quenching tower or the leaching tower and the subsequent chlorosilane rough distillation process, in order to prevent equipment blockage and remove metal impurities, the fine silicon powder and the metal impurities are discharged from the tower bottom along with silicon tetrachloride liquid, and the discharged solid-liquid mixture is hydrogenated residual liquid. In addition, in the reduction process, besides silicon and SiCl 4 、SiH 2 Cl 2 、H 2 Si in addition to HCl or the like 2 Cl 6 、Si 2 HCl 5 、Si 2 H 2 Cl 4 、Cl 6 OSi 2 And Si (Si) 3 Cl 8 And the byproduct of the double-silicon and multi-silicon atom compounds is generated, and the boiling point of the double-silicon and multi-silicon atom compounds is higher than that of trichlorosilane and silicon tetrachloride, namely the chlorosilane high-boiling-point compound. The reduction tail gas is recovered by a dry method and purified by rectification, and then SiHCl is obtained 3 、SiCl 4 、SiH 2 Cl 2 、H 2 And materials such as HCl and the like are returned to the system for recycling, and after the chlorosilane high-boiling residues, part of silicon tetrachloride and a small amount of amorphous silicon are discharged from the rectifying tower kettle, the discharged materials are solid-liquid mixtures, namely the purified residual liquid. The hydrogenated raffinate and the purified raffinate are generally mixed and then treated together, so that the chlorosilane raffinate in the polysilicon industry is obtained.
At present, the polysilicon enterprises commonly use a filtration method to pretreat the chlorosilane residual liquid, so as to remove solid impurities such as silicon powder, hydrogenation catalyst, metal chlorides (aluminum, calcium, iron, titanium) and the like. The filtering method is often combined with other separation means, and after filtering, the solid impurities in the residual liquid are obviously reduced, so that the treatment of subsequent procedures is convenient. The filtered clear liquid generally separates trichlorosilane and silicon tetrachloride through purification and evaporation, and finally high-boiling-point substances such as hexachlorodisilane and the like are recovered, purified or catalytically cracked, so that the maximum recovery and utilization of chlorosilane residual liquid are realized.
The conventional filtering process commonly uses a candle filter, and the filtering element is a filter cloth or a porous solid filter element, such as a porous ceramic filter element and a porous metal filter element. The adoption of the filter cloth is poor in filtering precision, the silicon powder in the hydrogenated residual liquid can be intercepted generally by more than 5um, but the amorphous silicon with the granularity of 1-5 um in the amorphous silicon in the purified residual liquid accounts for about 40%, and the amorphous silicon cannot be effectively intercepted and enters a subsequent system to cause equipment and pipeline blockage. The porous solid filter element has high precision, can effectively intercept amorphous silicon at 0.2-1 um, but metal chloride in residual liquid is jelly, is easy to block micropores of porous materials or is agglomerated on the surface of the filter element to form a compact layer, so that pressure difference before and after filtration is rapidly increased in a short time to stop maintenance.
In addition, as the filtration proceeds, the solid impurities trapped in the filter gradually increase, and the pressure difference between before and after the filtration gradually increases, and eventually the solid slag is packed into the equipment, so that the slag in the filter needs to be discharged periodically. Chlorosilane is easy to form HCl acid mist in air, and the reaction formula is SiCl 4 +4H 2 O=SiO 2 ·2H 2 O+4HCl. The normal operation is to replace with nitrogen firstly, namely, the liquid material is continuously volatilized into the nitrogen by continuously introducing the nitrogen to be carried out of the equipment, and the equipment is opened for maintenance when the nitrogen replaced from the equipment has almost no acid mist. After the filter element contacts air, chlorosilane attached to the surface of the filter element can react with the air, generated hydrochloric acid can corrode the filter element, and generated SiO (SiO) 2 The filter holes can be blocked, so that the filter element needs to be replaced after each maintenance, and the replacement cost of the filter element is high.
Therefore, the existing filtration technology of chlorosilane residual liquid needs to be improved.
Disclosure of Invention
The present application aims to solve at least one of the technical problems in the related art to some extent. Therefore, an objective of the present application is to provide a system and a method for filtering chlorosilane residual liquid, which can solve the problems of difficult filtration and high filtration cost of amorphous silicon and aluminum chloride precipitates in chlorosilane residual liquid in the prior art.
In one aspect of the application, a filtration system for chlorosilane residue is provided. According to an embodiment of the application, the system comprises:
the stirrer is provided with a diatomite inlet, a silicon tetrachloride inlet and a mixture outlet;
the nitrogen storage tank is connected with the stirrer through a first pipeline, and a first valve is arranged on the first pipeline;
the filter comprises a filter, wherein a liquid purifying cavity, a filter cavity and a feeding cavity are defined from top to bottom in the filter, a filter element which is axially arranged along the filter cavity is arranged in the filter cavity, the lower end of the filter element is sealed, the side wall of the filter element is wrapped with filter cloth, the upper port of the filter element is communicated with the liquid purifying cavity, a pressure difference detection device is arranged between the liquid purifying cavity and the feeding cavity, the liquid purifying cavity is provided with a chlorosilane clear liquid outlet, the mixture outlet is communicated with the feeding cavity through a second pipeline, and a second valve is arranged on the second pipeline;
the chlorosilane residual liquid storage tank is connected with the feeding cavity through a third pipeline, and a third valve is arranged on the third pipeline.
According to the filtering system for the chlorosilane residual liquid, the filter cloth is wrapped on the side wall of the filter element of the filter, then nitrogen is supplied to the stirrer through the first pipeline by adopting the nitrogen storage tank, the mixture containing diatomite and silicon tetrachloride in the stirrer is supplied to the filter to form the filter cake layer containing diatomite on the surface of the filter cloth of the filter element, when the chlorosilane residual liquid flows through the diatomite filter cake layer, the fine silicon powder in the mixture is larger in granularity and is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by diatomite, and part of the amorphous silicon which passes through the surface of the filter cake is intercepted by a micropore channel which is in the diatomite and is in a zigzag way and finer pores in the filter cake, and metal chloride in the chlorosilane residual liquid is easily adhered to the surface of the filter cake layer and the surface of the silicon powder to form a loose filter cake, so that the pressure difference between a clean liquid cavity and a feeding cavity cannot rapidly rise. Therefore, the system can solve the problems that amorphous silicon and aluminum chloride precipitates in chlorosilane residual liquid are difficult to filter and the filtering cost is high in the prior art.
In addition, the filtration system of chlorosilane residual liquid according to the above embodiment of the application can also have the following additional technical features:
in some embodiments of the present application, a plurality of the filter elements are disposed in the filter chamber, and the plurality of filter elements are spaced apart along the radial direction of the filter chamber. Thus, the filtration efficiency of the chlorosilane residual liquid can be improved.
In some embodiments of the application, the nitrogen storage tank is communicated with the clean liquid cavity through a fourth pipeline, and a fourth valve is arranged on the fourth pipeline. Therefore, when the pressure difference between the clean liquid cavity and the feeding cavity is large, nitrogen can be supplied to flush the filter element, and compared with the existing filter element replacement, the application has lower maintenance cost.
In some embodiments of the application, the system further comprises: the hydrolysis unit is connected with the feeding cavity through a fifth pipeline, and a fifth valve is arranged on the fifth pipeline.
In some embodiments of the application, the system further comprises: and the control unit is connected with the differential pressure detection device, the first valve, the second valve, the third valve, the fourth valve and the fifth valve. Thereby increasing the level of automation of the system of the present application.
In yet another aspect of the application, the application provides a method for filtering chlorosilane raffinate. According to an embodiment of the application, the method comprises:
(1) Feeding diatomite and silicon tetrachloride into the stirrer for mixing so as to obtain a mixture;
(2) Feeding nitrogen into the agitator through the first conduit using the nitrogen reservoir to feed the mixture into the filter to form a cake layer on the filter cloth;
(3) And the chlorosilane residual liquid storage tank is used for supplying chlorosilane residual liquid to the feeding cavity of the filter through the third conveying pipeline, so that the chlorosilane residual liquid is filtered through the filter cake layer, and slag slurry and chlorosilane clear liquid are obtained.
According to the method for filtering the chlorosilane residual liquid, the filter cloth is wrapped on the side wall of the filter element of the filter, then nitrogen is supplied to the stirrer through the first pipeline by adopting the nitrogen storage tank, the mixture containing diatomite and silicon tetrachloride in the stirrer is supplied to the filter to form a filter cake layer containing diatomite on the surface of the filter cloth of the filter element, when the chlorosilane residual liquid flows through the diatomite filter cake layer, fine silicon powder in the mixture is larger in granularity and is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by diatomite, and part of the amorphous silicon which passes through the surface of the filter cake is intercepted by a micropore channel which is in the diatomite and is in a zigzag way and finer pores in the filter cake, and metal chloride in the chlorosilane residual liquid is easily adhered to the surface of the filter cake layer and the surface of the silicon powder to form a loose filter cake, so that the pressure difference between a clean liquid cavity and a feeding cavity cannot rapidly rise. Therefore, the method can solve the problems that amorphous silicon and aluminum chloride precipitates in chlorosilane residual liquid are difficult to filter and the filtering cost is high in the prior art.
In addition, the filtration method of chlorosilane residual liquid according to the above embodiment of the application may further have the following additional technical features:
in some embodiments of the present application, in step (1), the concentration of diatomite in the mixture is 15-25% by mass. Therefore, the metal chloride and amorphous silicon in the chlorosilane residual liquid can be effectively intercepted and improved at the same time.
In some embodiments of the application, the above method further comprises: (4) And when the pressure difference detection device shows that the pressure difference is higher than 0.2bar, the control unit controls the third valve to be closed, the fourth valve and the fifth valve to be opened, and nitrogen is supplied from the clean liquid cavity of the filter through the fourth pipeline by utilizing the nitrogen storage tank so as to flush the filter cloth. Therefore, when the pressure difference between the clean liquid cavity and the feeding cavity is large, nitrogen can be supplied to flush the filter element, and compared with the existing filter element replacement, the application has lower maintenance cost.
In some embodiments of the application, the above method further comprises: (5) The slag slurry is supplied to a hydrolysis unit for hydrolysis treatment.
In some embodiments of the application, the above method further comprises: (6) And when the pressure difference detection device is lower than 0.05bar, the control unit controls the fourth valve and the fifth valve to be closed, the first valve and the second valve are opened so as to form a filter cake layer on the filter cloth, then the first valve and the second valve are closed, and the third valve is opened. Thereby increasing the level of automation of the system of the present application.
Additional aspects and advantages of the application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the application.
Drawings
The foregoing and/or additional aspects and advantages of the application will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic diagram of a filtration system for chlorosilane residue in accordance with one embodiment of the application;
FIG. 2 is a schematic diagram of a filtration system for chlorosilane residues according to a further embodiment of the application;
FIG. 3 is a schematic diagram of a filtration system for chlorosilane residue in accordance with yet another embodiment of the application;
FIG. 4 is a schematic flow diagram of a method for filtering chlorosilane residue according to one embodiment of the application;
FIG. 5 is a schematic flow chart of a method for filtering chlorosilane residues according to still another embodiment of the application;
FIG. 6 is a schematic flow chart of a method for filtering chlorosilane residues according to another embodiment of the application.
Detailed Description
Embodiments of the present application are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present application and should not be construed as limiting the application.
In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present application and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present application, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In the present application, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present application, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
In one aspect of the application, a filtration system for chlorosilane residue is provided. Referring to fig. 1-3, in accordance with an embodiment of the present application, the system includes: stirrer 100, nitrogen tank 200, filter 300 and chlorosilane raffinate tank 400.
According to an embodiment of the application, the stirrer 100 is provided with a diatomite inlet 101, a silicon tetrachloride inlet 102 and a mixture outlet 103 and is adapted to mix diatomite and silicon tetrachloride in order to obtain a mixture. Specifically, the diatomite has good micropore structure, adsorption performance and compression resistance, not only can the filtered liquid obtain a good flow rate ratio, but also fine suspended matters can be filtered out, the clarity is ensured, and the particle size of the diatomite particles used in the application is about 0.01-1 micron, so that the formed filter cake layer has high precision, and the mass concentration of the diatomite in the preferable mixture is 15-25%. The inventor finds that if the concentration of diatomite in the mixture is too high, the mixture has poor flowability and is easy to block a pipeline; if the concentration of diatomite in the mixture is too low, the forming speed of the filter cake layer is low, and the working efficiency is low. Therefore, the mass concentration can not only avoid the blockage of the pipeline, but also improve the working efficiency.
According to an embodiment of the present application, the nitrogen storage tank 200 is connected to the stirrer 100 through a first pipe 21, and a first valve 211 is provided on the first pipe 21 and adapted to press the mixture containing silicon tetrachloride and diatomaceous earth in the stirrer 100 into the filter 300 by supplying nitrogen into the stirrer 100.
According to the embodiment of the application, a clean liquid cavity 31, a filter cavity 32 and a feed cavity 33 are defined in the filter 300 from top to bottom, a filter element 321 arranged along the axial direction of the filter cavity is arranged in the filter cavity 32, the lower end of the filter element 321 is sealed, the side wall of the filter element is wrapped by filter cloth (not shown), the upper port of the filter element 321 is communicated with the clean liquid cavity 31, a pressure difference detection device 322 is arranged between the clean liquid cavity 31 and the feed cavity 33, the clean liquid cavity 31 is provided with a chlorosilane clear liquid outlet 301, the mixture outlet 103 is communicated with the feed cavity 33 through a second pipeline 34, and a second valve 341 is arranged on the second pipeline 34. Specifically, through wrapping the filter cloth on the side wall of the filter core 321 of the filter 300, then, nitrogen is supplied to the stirrer 100 through the first pipeline 21 by adopting the nitrogen storage tank 200, and the mixture containing diatomite and silicon tetrachloride in the stirrer 100 is supplied into the filter 300 and enters the filter cavity 32 through the feeding cavity 33 to form a filter cake layer (with the thickness of 8-12 mm, preferably 10 mm) containing diatomite on the surface of the filter cloth of the filter core 321, when chlorosilane residual liquid flows through the diatomite filter cake layer along the radial direction of the filter core 321, the chlorosilane residual liquid permeates into the inner cavity of the filter core 321, the fine silicon powder with larger granularity (10-100 μm) is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by diatomite, and part of the amorphous silicon (1-10 μm) which penetrates through the surface of the filter cake is intercepted by a microporous channel which is bent inside the diatomite and the finer pores inside the filter cake, and the metal chloride in the chlorosilane residual liquid is easily adhered on the surface of the filter cake layer and forms a loose filter cake, so that the chlorosilane residual liquid flows smoothly, and the pressure difference between the clean liquid cavity and the feeding cavity cannot rapidly rise, and the chlorosilane entering the inner cavity 321 flows into the inner cavity of the filter core 321 and flows into the axial direction of the filter core 321 and flows out of the clean liquid 301 through the chlorosilane outlet 301. Preferably, a plurality of filter elements 321 are arranged in the filter cavity 32, and the filter elements 321 are distributed along the radial direction of the filter cavity 32 at intervals, namely, filter cloth is arranged on the surface of each filter element 321, and a filter cake layer containing diatomite and silicon tetrachloride is formed on the filter cloth corresponding to each filter element 321, so that the chlorosilane filtering efficiency can be remarkably improved. It should be noted that, the differential pressure detecting device 322 is a conventional component in the art, so long as the differential pressure detection can be achieved, and will not be described herein.
According to an embodiment of the present application, the chlorosilane residual liquid storage tank 400 is connected to the feed cavity 33 through a third pipe 41, a third valve 411 is provided on the third pipe 41, and the chlorosilane residual liquid is adapted to be supplied into the feed cavity 33 of the filter 300 through the third pipe 41, so that the chlorosilane residual liquid is filtered through the filter cake layer, and a slag slurry and a chlorosilane clear liquid are obtained. Specifically, the chlorosilane raffinate mainly comprises the following components: monosilicon chlorosilane mainly containing silicon tetrachloride, polysilico chlorosilane high-boiling substances mainly containing hexachlorodisilane, fine silicon powder, and metal chlorides of aluminum, titanium, iron and the like. Preferably, in the present application, the chlorosilane residual liquid can also be directly supplied to the second pipeline 34 through the third pipeline 41, that is, the chlorosilane residual liquid is supplied to the feed cavity 33 of the filter 300 after passing through the third pipeline 41 and the second pipeline 34.
According to the filtering system for the chlorosilane residual liquid, the filter cloth is wrapped on the side wall of the filter element of the filter, then nitrogen is supplied to the stirrer through the first pipeline by adopting the nitrogen storage tank, the mixture containing diatomite and silicon tetrachloride in the stirrer is supplied to the filter to form the filter cake layer containing diatomite on the surface of the filter cloth of the filter element, when the chlorosilane residual liquid flows through the diatomite filter cake layer, the fine silicon powder in the mixture is larger in granularity and is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by diatomite, and part of the amorphous silicon which passes through the surface of the filter cake is intercepted by a micropore channel which is in the diatomite and is in a zigzag way and finer pores in the filter cake, and metal chloride in the chlorosilane residual liquid is easily adhered to the surface of the filter cake layer and the surface of the silicon powder to form a loose filter cake, so that the pressure difference between a clean liquid cavity and a feeding cavity cannot rapidly rise. Therefore, the system can solve the problems that amorphous silicon and aluminum chloride precipitates in chlorosilane residual liquid are difficult to filter and the filtering cost is high in the prior art.
Further, in the above system, referring to fig. 2, the nitrogen tank 200 is communicated with the clean liquid chamber 31 through the fourth pipe 22, and the fourth pipe 22 is provided with a fourth valve 221. Specifically, wait that differential pressure detection device 322 shows to be higher than 0.2bar, i.e. the silica flour of filter 300 filter core 321 filter cake layer surface piles up to certain thickness, stop supplying chlorosilane raffinate this moment, after no fluid effect, the adhesion of silica flour on the filter cake layer reduces, gravity effect can be greater than adhesion, the silica flour of surface will drop by oneself and deposit to feed cavity 33 bottom, and when nitrogen gas (6 bar) that self-cleaning liquid chamber 31 supplied washes, fluid from top to bottom has strengthened silica flour and has dropped the effect, compared with the operation that the current stopping overhauld the filter and need adopt nitrogen gas to replace the filter for a long time and change the filter core, the washing mode labour saving and time saving to the filter core of this application is lower. And a hydrolysis unit 500 is provided at this time, the hydrolysis unit 500 is connected to the feed chamber 33 through a fifth pipe 51, and a fifth valve 511 is provided on the fifth pipe 51, and is adapted to open the fifth valve 511 on the fifth pipe 51 at the bottom of the feed chamber 33 during the flushing of the filter element 321, and to supply the high-concentration solid slag slurry deposited at the bottom of the feed chamber 33 to the hydrolysis unit 500 for hydrolysis treatment. Specifically, the hydrolysis unit 500 of the application adopts glass fiber reinforced plastic slag slurry to enter from the bottom of the hydrolysis unit 500, is atomized by the spiral spray head 52, and the hydrolysis unit 500 is provided with three layers of spray assemblies 53, the spray assemblies 53 adopt common water as a eluent, the slurry atomized by the spiral spray head 52 fully reacts with water sprayed by the spray assemblies 53 to generate silicon dioxide hydrate and hydrochloric acid, and the silicon dioxide hydrate and the hydrochloric acid are discharged from the bottom of the hydrolysis unit and then sent to a three-waste station for treatment, so that silicon powder accumulated in the filter 300 is not continuously increased to a certain amount, and periodic maintenance is avoided.
Preferably, referring to fig. 3, by arranging the control unit 600, the control unit 600 is connected to the differential pressure detecting device 322 and the first, second, third, fourth and fifth valves 211, 341, 411, 221, 511. Specifically, the control unit controls 600 to flush the filter element from top to bottom by using the nitrogen tank 200 to supply nitrogen from the clean liquid chamber 31 of the filter 300 through the fourth pipeline 22, and to supply the high concentration solid slag slurry deposited to the bottom of the feed chamber 33 to the hydrolysis unit 500 for hydrolysis treatment, and to control 600 to close the fourth valve 221 and the fifth valve 511 and to open the first valve 211 and the second valve 341 when the pressure difference detection device 322 shows less than 0.05bar, namely, to supply nitrogen into the stirrer 100 through the first pipeline 21 by using the nitrogen tank 200, to make the mixture containing diatomite and silicon tetrachloride in the stirrer 100 enter the filter 300 through the feed chamber 33 to form a cake layer containing diatomite on the filter cloth surface of the filter element 321, then to close the first valve 211 and the second valve 341, to open the third valve 411, and to supply the chlorosilane to the filter 300 through the third pipeline 321 to the filter cloth surface of the filter element 321 for solid-liquid separation. It should be noted that, the control unit 600 is a control device that is conventional in the art, so long as the above functions can be achieved, and the structure thereof will not be described herein.
In yet another aspect of the present application, a method for filtering chlorosilane residue using the above system is provided. Referring to fig. 4-6, in accordance with an embodiment of the present application, the method includes:
s100: diatomite and silicon tetrachloride are supplied into a stirrer for mixing
In this step, diatomaceous earth and silicon tetrachloride are supplied to a stirrer to be mixed, so that a mixture is obtained. Specifically, the diatomite has good micropore structure, adsorption performance and compression resistance, not only can the filtered liquid obtain a good flow rate ratio, but also fine suspended matters can be filtered out, the clarity is ensured, and the particle size of the diatomite particles used in the method is about 0.01-1 micron, so that the formed filter cake layer has high precision, and the mass concentration of the diatomite in the preferable mixture is 15-25%. The inventor finds that if the concentration of diatomite in the mixture is too high, the mixture has poor flowability and is easy to block a pipeline; if the concentration of diatomite in the mixture is too low, the forming speed of the filter cake layer is low, and the working efficiency is low. Therefore, the mass concentration can not only avoid the blockage of the pipeline, but also improve the working efficiency.
S200: the nitrogen tank is used to supply nitrogen into the stirrer through a first pipeline, and the mixture is supplied into the filter
In the step, the filter cloth is wrapped on the side wall of the filter element 321 of the filter 300, then nitrogen is supplied to the stirrer 100 through the first pipeline 21 by adopting the nitrogen storage tank 200, the mixture containing diatomite and silicon tetrachloride in the stirrer 100 is supplied into the filter 300 and enters the filter cavity 32 through the feeding cavity 33 to form a filter cake layer (with the thickness of 8-12 mm, preferably 10 mm) containing diatomite on the surface of the filter cloth of the filter element 321, when chlorosilane residual liquid flows through the diatomite filter cake layer along the radial direction of the filter element 321, the chlorosilane residual liquid permeates into the inner cavity of the filter element 321, fine silicon powder with larger granularity (10-100 mu m) is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by diatomite, and part of the amorphous silicon (1-10 mu m) which penetrates through the surface of the filter cake is intercepted by a micro-pore channel which is bent inside the diatomite and a finer pore inside the filter cake, and metal chloride in the chlorosilane residual liquid is easily adhered on the surface of the filter cake layer and forms loose filter cake, so that the chlorosilane residual liquid flows smoothly, and the pressure difference between the clean liquid cavity and the feeding cavity cannot rapidly rise, and the chlorosilane entering the inner cavity 321 flows into the inner cavity of the filter element 321 and axially flows out of the clean liquid 301 along the filter element 31 through the filter element outlet 301.
S300: the chlorosilane raffinate storage tank is used for supplying the chlorosilane raffinate to the feed cavity of the filter through the third conveying pipeline
In this step, a chlorosilane residue is supplied into the feed chamber 33 of the filter 300 through the third pipe 41 using the chlorosilane residue tank 400, so that the chlorosilane residue is filtered through the cake layer to obtain a residue slurry and a chlorosilane clear liquid. Specifically, the chlorosilane raffinate mainly comprises the following components: monosilicon chlorosilane mainly containing silicon tetrachloride, polysilico chlorosilane high-boiling substances mainly containing hexachlorodisilane, fine silicon powder, and metal chlorides of aluminum, titanium, iron and the like. Preferably, in the present application, the chlorosilane residual liquid can also be directly supplied to the first pipeline 21 through the third pipeline 41, that is, the chlorosilane residual liquid is supplied to the feed cavity 33 of the filter 300 after passing through the third pipeline 41 and the first pipeline 21.
According to the method for filtering the chlorosilane residual liquid, the filter cloth is wrapped on the side wall of the filter element of the filter, then nitrogen is supplied to the stirrer through the first pipeline by adopting the nitrogen storage tank, the mixture containing diatomite and silicon tetrachloride in the stirrer is supplied to the filter to form a filter cake layer containing diatomite on the surface of the filter cloth of the filter element, when the chlorosilane residual liquid flows through the diatomite filter cake layer, fine silicon powder in the mixture is larger in granularity and is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by diatomite, and part of the amorphous silicon which passes through the surface of the filter cake is intercepted by a micropore channel which is in the diatomite and is in a zigzag way and finer pores in the filter cake, and metal chloride in the chlorosilane residual liquid is easily adhered to the surface of the filter cake layer and the surface of the silicon powder to form a loose filter cake, so that the pressure difference between a clean liquid cavity and a feeding cavity cannot rapidly rise. Therefore, the method can solve the problems that amorphous silicon and aluminum chloride precipitates in chlorosilane residual liquid are difficult to filter and the filtering cost is high in the prior art.
Referring to fig. 5, the above method further includes:
s400: when the pressure difference detection device shows that the pressure difference is higher than 0.2bar, the control unit controls the third valve to be closed and controls the fourth valve and the fifth valve to be opened
In this step, the pressure difference detecting device 322 displays that the pressure difference is higher than 0.2bar, that is, the silicon powder on the surface of the filter cake layer of the filter element 321 of the filter 300 is accumulated to a certain thickness, the control unit 600 controls to close the third valve 411, that is, the supply of chlorosilane residual liquid is stopped at this time, after no fluid action, the adhesion force of the silicon powder on the filter cake layer is reduced, the gravity action is larger than the adhesion force, the silicon powder on the surface can fall off and deposit to the bottom of the feeding cavity 33 by itself, and the fourth valve 221 is opened, so that when the filter element 321 is flushed by nitrogen (6 bar) supplied from the cleaning liquid cavity 31, the fluid flows downwards from top to bottom, the silicon powder falling effect is enhanced, and high-concentration solid slag slurry deposited to the bottom of the feeding cavity 33 is discharged from the bottom of the feeding cavity 33.
S500: the slag slurry is supplied to a hydrolysis unit for hydrolysis treatment
In this step, the high-concentration solid slag slurry deposited on the bottom of the feed chamber 33 is supplied to the hydrolysis unit 500 to be subjected to hydrolysis treatment. Specifically, the hydrolysis unit 500 of the application adopts glass fiber reinforced plastic slag slurry to enter from the bottom of the hydrolysis unit 500, is atomized by the spiral spray head 52, and the hydrolysis unit 500 is provided with three layers of spray assemblies 53, the spray assemblies 53 adopt common water as a eluent, the slurry atomized by the spiral spray head 52 fully reacts with water sprayed by the spray assemblies 53 to generate silicon dioxide hydrate and hydrochloric acid, and the silicon dioxide hydrate and the hydrochloric acid are discharged from the bottom of the hydrolysis unit and then sent to a three-waste station for treatment, so that silicon powder accumulated in the filter 300 is not continuously increased to a certain amount, and periodic maintenance is avoided. And supplying nitrogen from the clean liquid cavity of the filter through the fourth pipeline by using the nitrogen storage tank so as to flush the filter cloth.
Referring to fig. 6, the above method further includes:
s600: when the pressure difference detection device is lower than 0.05bar, the control unit controls the first valve, the second valve, the third valve, the fourth valve and the fifth valve
In this step, when the pressure difference detecting means 322 shows higher than 0.2bar, the control unit 600 closes the third valve 411, opens the fourth valve 221 and the fifth valve 511, supplies nitrogen gas from the clean liquid chamber 31 of the filter 300 through the fourth pipe 22 by using the nitrogen gas storage tank 200, washes the filter cartridge from top to bottom, and causes the high concentration solid slag slurry deposited to the bottom of the feed chamber 33 to be supplied to the hydrolysis unit 500 for hydrolysis treatment, and when the pressure difference detecting means 322 shows lower than 0.05bar, the control unit 600 controls to close the fourth valve 221 and the fifth valve 511, opens the first valve 211 and the second valve 341, i.e., supplies nitrogen gas into the stirrer 100 through the first pipe 21 by using the nitrogen gas storage tank 200, causes the mixture containing diatomaceous earth and silicon tetrachloride in the stirrer 100 to enter the filter chamber 32 through the feed chamber 33 in the filter 300 to form a cake layer containing diatomaceous earth on the filter cloth surface of the filter cartridge 321, then closes the first valve and the second valve 341, opens the third valve 411, supplies the chlorosilane residue to the filter cartridge 300 through the third pipe 41 to the feed chamber 33, and then performs solid-liquid separation on the filter cartridge 321.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present application have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the application, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the application.
Claims (2)
1. The method for filtering the chlorosilane residual liquid is characterized in that the system for filtering the chlorosilane residual liquid used in the method for filtering the chlorosilane residual liquid comprises the following steps:
the stirrer is provided with a diatomite inlet, a silicon tetrachloride inlet and a mixture outlet;
the nitrogen storage tank is connected with the stirrer through a first pipeline, and a first valve is arranged on the first pipeline;
the filter comprises a filter, wherein a liquid purifying cavity, a filter cavity and a feeding cavity are defined in the filter from top to bottom, a filter element which is axially arranged along the filter cavity is arranged in the filter cavity, the lower end of the filter element is sealed, the side wall of the filter element is wrapped with filter cloth, the upper port of the filter element is communicated with the liquid purifying cavity, a pressure difference detection device is arranged between the liquid purifying cavity and the feeding cavity, the liquid purifying cavity is provided with a chlorosilane clear liquid outlet, the mixture outlet is communicated with the feeding cavity through a second pipeline, a second valve is arranged on the second pipeline, the nitrogen storage tank is communicated with the liquid purifying cavity through a fourth pipeline, and a fourth valve is arranged on the fourth pipeline;
the chlorosilane residual liquid storage tank is connected with the feeding cavity through a third pipeline, and a third valve is arranged on the third pipeline;
the hydrolysis unit is connected with the feeding cavity through a fifth pipeline, and a fifth valve is arranged on the fifth pipeline;
the control unit is connected with the differential pressure detection device, the first valve, the second valve, the third valve, the fourth valve and the fifth valve;
the filtering method for implementing the chlorosilane residual liquid comprises the following steps:
(1) Supplying diatomite and silicon tetrachloride to the stirrer for mixing so as to obtain a mixture, wherein the mass concentration of the diatomite in the mixture is 15-25%;
(2) Feeding nitrogen into the agitator through the first conduit using the nitrogen reservoir to feed the mixture into the filter to form a cake layer on the filter cloth;
(3) The chlorosilane residual liquid storage tank is adopted to supply chlorosilane residual liquid to a feeding cavity of the filter through the third pipeline, so that the chlorosilane residual liquid is filtered through the filter cake layer to obtain slag slurry and chlorosilane clear liquid;
(4) When the pressure difference detection device shows that the pressure difference is higher than 0.2bar, the control unit controls the third valve to be closed, the fourth valve and the fifth valve to be opened, and nitrogen is supplied from the clean liquid cavity of the filter through the fourth pipeline by utilizing the nitrogen storage tank so as to flush the filter cloth;
(5) The slag slurry is supplied to a hydrolysis unit for hydrolysis treatment;
(6) And when the pressure difference detection device is lower than 0.05bar, the control unit controls the fourth valve and the fifth valve to be closed, the first valve and the second valve are opened so as to form a filter cake layer on the filter cloth, then the first valve and the second valve are closed, and the third valve is opened.
2. The method for filtering chlorosilane residual liquid as in claim 1, wherein a plurality of filter elements are arranged in said filter cavity, said plurality of filter elements being distributed at intervals along the radial direction of said filter cavity.
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| US20010053343A1 (en) * | 2000-06-20 | 2001-12-20 | Degussa Ag | Separation of metal chlorides from their suspensions in chlorosilanes |
| CN107758673A (en) * | 2017-11-03 | 2018-03-06 | 洛阳中硅高科技有限公司 | Chlorosilane Recovery Purifying device and method |
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