CN111072032A - System and method for filtering chlorosilane residual liquid - Google Patents
System and method for filtering chlorosilane residual liquid Download PDFInfo
- Publication number
- CN111072032A CN111072032A CN202010060396.4A CN202010060396A CN111072032A CN 111072032 A CN111072032 A CN 111072032A CN 202010060396 A CN202010060396 A CN 202010060396A CN 111072032 A CN111072032 A CN 111072032A
- Authority
- CN
- China
- Prior art keywords
- filter
- valve
- cavity
- pipeline
- chlorosilane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 137
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 107
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 238000001914 filtration Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 93
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 41
- 239000000203 mixture Substances 0.000 claims abstract description 37
- 239000004744 fabric Substances 0.000 claims abstract description 36
- 238000003860 storage Methods 0.000 claims abstract description 35
- 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
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 239000012065 filter cake Substances 0.000 claims description 58
- 230000007062 hydrolysis Effects 0.000 claims description 24
- 238000006460 hydrolysis reaction Methods 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 11
- 239000002893 slag Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 abstract description 17
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 29
- 239000011863 silicon-based powder Substances 0.000 description 21
- 229910001873 dinitrogen Inorganic materials 0.000 description 11
- 235000013312 flour Nutrition 0.000 description 11
- 229910001510 metal chloride Inorganic materials 0.000 description 11
- 239000007787 solid Substances 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000007921 spray Substances 0.000 description 10
- 239000000377 silicon dioxide Substances 0.000 description 9
- 239000012535 impurity Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229920005591 polysilicon Polymers 0.000 description 5
- 239000005909 Kieselgur Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 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
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 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
- 238000009835 boiling Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910003910 SiCl4 Inorganic materials 0.000 description 2
- 229910003818 SiH2Cl2 Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 238000005406 washing 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
- 229910007245 Si2Cl6 Inorganic materials 0.000 description 1
- 229910003822 SiHCl3 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 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
- 238000004821 distillation Methods 0.000 description 1
- -1 etc. Chemical compound 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 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
- 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
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
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
Abstract
The invention discloses a system and a method for filtering chlorosilane residual liquid, wherein the system comprises the following steps: the device comprises a stirrer, a nitrogen storage tank, a filter and a chlorosilane residual liquid storage tank, wherein 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; a clean liquid cavity, a filter cavity and a feeding cavity are defined in the filter from top to bottom, a filter element arranged along the axial direction of the filter cavity is arranged in the filter cavity, the lower end of the filter element is closed, the side wall of the filter element is wrapped by 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 feeding cavity, the clean liquid cavity is provided with a chlorosilane clear liquid outlet, a 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. By adopting the system, the problems that amorphous silicon and aluminum chloride educts in chlorosilane residual liquid are difficult to filter and the filtering cost is high in the prior art can be solved.
Description
Technical Field
The invention belongs to the field of polycrystalline silicon, and particularly relates to a system and a method for filtering chlorosilane residual liquid.
Background
A large amount of silicon tetrachloride is produced in the process of producing polysilicon by the improved Siemens method. At present, more than 90 percent of polysilicon enterprises adopt a silicon tetrachloride cold hydrogenation technology to treat byproducts and convert the byproducts into trichlorosilane which is a raw material for producing polysilicon. The silicon tetrachloride cold hydrogenation technology is that metallurgical grade silicon powder, hydrogen and silicon tetrachloride react under the action of a catalyst under the conditions of certain temperature and pressure to generate trichlorosilane. Because 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 bottom of the tower along with silicon tetrachloride liquid, and the discharged part of solid-liquid mixture is hydrogenated residual liquid. In addition, in the reduction process, silicon and SiCl are removed4、SiH2Cl2、H2And HCl, etc., and Si2Cl6、Si2HCl5、Si2H2Cl4、Cl6OSi2And Si3Cl8And the by-products of some series of compounds with double silicon atoms and multiple silicon atoms are generated, and the boiling points of the compounds with double silicon atoms and multiple silicon atoms are higher compared with trichlorosilane and silicon tetrachloride, namely the compounds with double silicon atoms and multiple silicon atoms are chlorosilane high-boiling residues. After the reduction tail gas is recovered by a dry method and rectified and purified, SiHCl3、SiCl4、SiH2Cl2、H2And materials such as HCl and the like are returned to the system for recycling, and after 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 purification residual liquid. The hydrogenation residual liquid and the purification residual liquid are generally mixed and then are treated together, and the chlorosilane residual liquid in the polysilicon industry is obtained.
At present, a filtration method is commonly used for pretreating chlorosilane residual liquid in polysilicon enterprises to remove solid impurities in the chlorosilane residual liquid, such as silicon powder, hydrogenation catalysts, metal chlorides (aluminum, calcium, iron and titanium) and the like. The filtering method is often combined with other separation means, after filtration, the solid impurities in the residual liquid are obviously reduced, and the subsequent process treatment is convenient. The filtered clear liquid is generally purified and evaporated to separate out trichlorosilane and silicon tetrachloride, and finally high-boiling-point substances such as hexachlorodisilane and the like are recovered and purified or catalytically cracked, so that the maximum recovery and utilization of chlorosilane residual liquid are realized.
The existing filtration process usually uses a candle filter, and the filter 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 filtering precision of the filter cloth is poor, generally above 5um, silicon powder in the hydrogenated raffinate can be intercepted, but amorphous silicon with the granularity of 1-5 um in the purified raffinate accounts for about 40%, and the amorphous silicon cannot be effectively intercepted and enters a subsequent system to cause equipment and pipeline blockage. The adoption of the porous solid filter element has high precision, amorphous silicon can be effectively intercepted at 0.2-1 um, but metal chloride in residual liquid is jelly, micropores of a porous material are easily blocked or a compact layer is formed on the surface of the filter element through agglomeration, so that the pressure difference quickly rises in a short time before and after filtration, and the filter element is stopped for maintenance.
In addition, as the filtration progresses, the amount of solid impurities trapped in the filter increases, the pressure difference between before and after the filtration also increases, and finally the solid slag is deposited in the facility. Chlorosilane easily forms HCl acid mist in the air, and the reaction formula is SiCl4+4H2O＝SiO2·2H2O +4 HCl. The normal operation is that nitrogen is firstly used for replacement, namely, the liquid material is continuously volatilized by continuously introducing the nitrogenAnd the nitrogen enters the nitrogen to be taken 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 with air, chlorosilane attached to the surface of the filter element reacts with the air, generated hydrochloric acid corrodes the filter element, and generated SiO2The filter holes can be blocked, so that the filter element needs to be replaced after each overhaul, and the replacement cost of the filter element is high.
Therefore, the existing filtering technology of chlorosilane residual liquid needs to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide a system and a method for filtering chlorosilane residual liquid, and the system can solve the problems that amorphous silicon and aluminum chloride educts in the chlorosilane residual liquid are difficult to filter and the filtering cost is high in the prior art.
In one aspect of the invention, the invention provides a chlorosilane residual liquid filtering system. According to an embodiment of the invention, 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 clean liquid cavity, a filter cavity and a feeding cavity are defined from top to bottom in the filter, a filter element arranged along the axial direction of the filter cavity is arranged in the filter cavity, the lower end of the filter element is closed, the side wall of the filter element is wrapped by 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 feeding cavity, the clean liquid 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;
and 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 of the chlorosilane residual liquid, disclosed by the embodiment of the invention, the filter cloth is wrapped on the side wall of the filter element of the filter, then the nitrogen is supplied into the stirrer through the first pipeline by the nitrogen storage tank, the mixture containing the kieselguhr and the silicon tetrachloride in the stirrer is supplied to the filter to form the filter cake layer containing the kieselguhr on the surface of the filter cloth of the filter element, when the chlorosilane residual liquid flows through the kieselguhr filter cake layer, fine silicon powder in the chlorosilane residual liquid has larger granularity and is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by the kieselguhr, and part of smaller amorphous silicon passing through the surface of the filter cake is intercepted by the tortuous micropore channels in the kieselguhr and the finer pores in the filter cake, so that metal chloride in the chlorosilane residual liquid is easily attached to the surface of the filter cake layer and the surface of the silicon powder to form looseness, the, compare in current filter core or filter cloth and filter, the unable amorphous silica flour of interception of filter cloth and the problem that leads to equipment to block up can not exist in this application, also can not exist the filter core simultaneously and filter the problem that the short time of front and back pressure differential rises rapidly and the inspection of stopping. 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 chlorosilane residual liquid filtering system according to the embodiment of the invention can also have the following additional technical characteristics:
in some embodiments of the present invention, a plurality of the filter elements are disposed in the filter cavity, and the plurality of the filter elements are distributed at intervals along a radial direction of the filter cavity. Therefore, the chlorosilane residual liquid filtering efficiency can be improved.
In some embodiments of the present invention, the nitrogen storage tank is communicated with the liquid purifying chamber through a fourth pipeline, and a fourth valve is arranged on the fourth pipeline. From this, when net sap cavity and feeding chamber pressure differential are great, can supply with nitrogen gas and wash the filter core, compare than current renew cartridge, this application cost of overhaul is lower.
In some embodiments of the invention, 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 invention, the system further comprises: and the control unit is connected with the differential pressure detection device and the first valve, the second valve, the third valve, the fourth valve and the fifth valve. Therefore, the automation level of the system is improved.
In yet another aspect, the present invention provides a method for filtering a chlorosilane raffinate. According to an embodiment of the invention, the method comprises:
(1) feeding diatomite and silicon tetrachloride into the stirrer for mixing so as to obtain a mixture;
(2) supplying nitrogen into the agitator through the first pipe using the nitrogen storage tank so as to supply the mixture into the filter so as to form a cake layer on the filter cloth;
(3) and feeding chlorosilane residual liquid into the feeding cavity of the filter through the third conveying pipeline by adopting the chlorosilane residual liquid storage tank, so that the chlorosilane residual liquid is filtered through the filter cake layer to obtain slag slurry and chlorosilane clear liquid.
According to the method for filtering the chlorosilane residual liquid, disclosed by the embodiment of the invention, the filter cloth is wrapped on the side wall of the filter element of the filter, then the nitrogen is supplied into the stirrer through the first pipeline by the nitrogen storage tank, the mixture containing the kieselguhr and the silicon tetrachloride in the stirrer is supplied to the filter to form the filter cake layer containing the kieselguhr on the surface of the filter cloth of the filter element, when the chlorosilane residual liquid flows through the kieselguhr filter cake layer, fine silicon powder in the chlorosilane residual liquid has larger granularity and is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by the kieselguhr, and part of smaller amorphous silicon passing through the surface of the filter cake is intercepted by a tortuous micropore channel inside the kieselguhr and finer pores inside the filter cake, so that metal chloride in the chlorosilane residual liquid is easily attached to the surface of the filter cake layer and the surface of the silicon powder to form looseness, the chlorosilane, compare in current filter core or filter cloth and filter, the unable amorphous silica flour of interception of filter cloth and the problem that leads to equipment to block up can not exist in this application, also can not exist the filter core simultaneously and filter the problem that the short time of front and back pressure differential rises rapidly and the inspection of stopping. 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 method for filtering chlorosilane residual liquid according to the embodiment of the invention can also have the following additional technical characteristics:
in some embodiments of the invention, in the step (1), the mass concentration of the diatomite in the mixture is 15-25%. 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 invention, the method further comprises: (4) and when the pressure difference detection device displays that the pressure difference is higher than 0.2bar, the control unit controls to close the third valve, open the fourth valve and the fifth valve, and supply nitrogen from the liquid purifying cavity of the filter through the fourth pipeline by using the nitrogen storage tank so as to flush the filter cloth. From this, when net sap cavity and feeding chamber pressure differential are great, can supply with nitrogen gas and wash the filter core, compare than current renew cartridge, this application cost of overhaul is lower.
In some embodiments of the invention, the method further comprises: (5) and feeding the slag slurry to a hydrolysis unit for hydrolysis treatment.
In some embodiments of the invention, the method further comprises: (6) and when the pressure difference detection device is lower than 0.05bar, the control unit controls to close the fourth valve and the fifth valve, open the first valve and the second valve so as to form a filter cake layer on the filter cloth, close the first valve and the second valve and open the third valve. Therefore, the automation level of the system is improved.
Additional aspects and advantages of the invention 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 invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic diagram of a chlorosilane raffinate filtration system according to one embodiment of the present invention;
FIG. 2 is a schematic diagram of a chlorosilane raffinate filtration system according to yet another embodiment of the present invention;
FIG. 3 is a schematic diagram of a chlorosilane raffinate filtration system according to yet another embodiment of the present invention;
FIG. 4 is a schematic flow diagram of a method for filtering a chlorosilane raffinate according to one embodiment of the invention;
FIG. 5 is a schematic flow diagram of a process for filtering a chlorosilane raffinate according to yet another embodiment of the invention;
FIG. 6 is a schematic flow diagram of a chlorosilane raffinate filtration process according to yet another embodiment of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In one aspect of the invention, the invention provides a chlorosilane residual liquid filtering system. Referring to fig. 1-3, the system includes, according to an embodiment of the invention: a stirrer 100, a nitrogen storage tank 200, a filter 300 and a chlorosilane residual liquid storage tank 400.
According to an embodiment of the invention, the stirrer 100 is provided with an inlet 101 for diatomaceous earth, an inlet 102 for silicon tetrachloride and an outlet 103 for the mixture, and is adapted to mix diatomaceous earth and silicon tetrachloride so as to obtain a mixture. Specifically, the diatomite has a good microporous structure, good adsorption performance and good compression resistance, a good flow rate ratio of a filtered liquid can be obtained, fine suspended matters can be filtered, and the clarity is guaranteed, and the particle size of the diatomite particles used in the application is about 0.01-1 micron, so that a formed filter cake layer has high precision, and the preferable mass concentration of the diatomite in a mixture is 15-25%. The inventor finds that if the concentration of the diatomite in the mixture is too high, the mixture has poor fluidity and is easy to block pipelines; and if the concentration of the diatomite in the mixture is too low, the forming speed of the filter cake layer is slow, and the working efficiency is low. Therefore, the mass concentration can be adopted to avoid pipeline blockage and improve the working efficiency.
According to the embodiment of the present invention, the nitrogen storage tank 200 is connected to the stirrer 100 through the first pipe 21, and the first pipe 21 is provided with the first valve 211 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 invention, 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 is arranged in the filter cavity 32 along the axial direction of the filter element, the lower end of the filter element 321 is closed, 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, by wrapping filter cloth on the side wall of a filter element 321 of a filter 300, then supplying nitrogen into a stirrer 100 through a first pipeline 21 by using a nitrogen storage tank 200, and supplying a mixture containing diatomite and silicon tetrachloride in the stirrer 100 into the filter 300, and allowing the mixture to enter a filter cavity 32 through a feeding cavity 33 to form a filter cake layer (with a thickness of 8-12 mm, preferably 10mm) 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 an inner cavity of the filter element 321, wherein the fine silicon powder has a larger particle size (10-100 μm), is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by the diatomite, and is intercepted by smaller amorphous silicon (1-10 μm) partially passing through the surface of the filter cake, by microporous channels bent inside the diatomite and finer pores inside the filter cake, and metal chloride in the chlorosilane residual liquid is easily attached to the surface of the filter, a loose filter cake is formed, so that the chlorosilane residual liquid flows smoothly, the pressure difference between the clean liquid cavity and the feeding cavity cannot rise rapidly, and the chlorosilane clear liquid entering the inner cavity of the filter element 321 flows into the clean liquid cavity 31 along the axial direction of the filter element 321 and is discharged through the chlorosilane clear liquid outlet 301. Preferably, a plurality of filter elements 321 are arranged in the filter cavity 32, and the plurality of filter elements 321 are distributed at intervals along the radial direction of the filter cavity 32, that is, filter cloth is uniformly 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 filtration efficiency can be remarkably improved. It should be noted that the differential pressure detecting device 322 is a conventional component in the art, as long as it can detect the differential pressure, and is not described herein again.
According to the embodiment of the invention, the chlorosilane residual liquid storage tank 400 is connected with the feeding cavity 33 through the third pipeline 41, the third pipeline 41 is provided with the third valve 411, and the chlorosilane residual liquid is suitable for being supplied into the feeding cavity 33 of the filter 300 through the third pipeline 41, so that the chlorosilane residual liquid is filtered through the filter cake layer to obtain the slag slurry and the chlorosilane clear liquid. Specifically, the chlorosilane residual liquid mainly comprises the following components: monosilicchlorosilane mainly containing silicon tetrachloride, polysilichlorosilane 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 conveyed to the second pipeline 34 through the third pipeline 41, i.e., the chlorosilane residual liquid is supplied to the feeding cavity 33 of the filter 300 after passing through the third pipeline 41 and the second pipeline 34.
According to the filtering system of the chlorosilane residual liquid, disclosed by the embodiment of the invention, the filter cloth is wrapped on the side wall of the filter element of the filter, then the nitrogen is supplied into the stirrer through the first pipeline by the nitrogen storage tank, the mixture containing the kieselguhr and the silicon tetrachloride in the stirrer is supplied to the filter to form the filter cake layer containing the kieselguhr on the surface of the filter cloth of the filter element, when the chlorosilane residual liquid flows through the kieselguhr filter cake layer, fine silicon powder in the chlorosilane residual liquid has larger granularity and is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by the kieselguhr, and part of smaller amorphous silicon passing through the surface of the filter cake is intercepted by the tortuous micropore channels in the kieselguhr and the finer pores in the filter cake, so that metal chloride in the chlorosilane residual liquid is easily attached to the surface of the filter cake layer and the surface of the silicon powder to form looseness, the, compare in current filter core or filter cloth and filter, the unable amorphous silica flour of interception of filter cloth and the problem that leads to equipment to block up can not exist in this application, also can not exist the filter core simultaneously and filter the problem that the short time of front and back pressure differential rises rapidly and the inspection of stopping. 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 storage tank 200 is communicated with the clean liquid chamber 31 through a fourth pipeline 22, and a fourth valve 221 is disposed on the fourth pipeline 22. Specifically, treat that pressure difference detection device 322 shows to be higher than 0.2bar, certain thickness is piled up to the silica flour on filter 300 filter core 321 filter cake layer surface promptly, stop to supply with chlorosilane raffinate this moment, no fluid effect back, the adhesion of silica flour reduces on the filter cake layer, action of gravity can be greater than the adhesion, surperficial silica flour will drop by oneself and deposit to feeding chamber 33 bottom, and when nitrogen gas (6bar) that self-purification liquid chamber 31 supplied with washed, the fluid down flows from last, the silica flour effect of droing has been strengthened, more current parking is overhauld the filter and need adopt nitrogen gas to carry out long-time replacement and the operation of changing the filter core to the filter and compare, this application's washing mode labour saving and time saving and cost to the filter core are lower. And at this time, a hydrolysis unit 500 is provided, 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 flushing of the filter element 321, and supply the high-concentration solid residue slurry deposited at the bottom of the feed chamber 33 to the hydrolysis unit 500 for hydrolysis treatment. Specifically, the unit 500 that hydrolysises of this application adopts glass steel matter sediment thick liquid to get into from the unit 500 bottom of hydrolysising, atomize through spiral spray nozzle 52, and the unit 500 that hydrolysises establishes three-layer spray assembly 53 altogether, spray assembly 53 and adopt ordinary water as the eluent, thick liquid after spiral spray nozzle 52 atomizes and spray assembly 53 spun water contact abundant reaction, generate silica hydrate and hydrochloric acid, send the three wastes station to handle after the unit bottom discharge hydrolysises, it can not continuously increase to a certain amount to have realized piling up the silica flour in filter 300, regular overhaul has been 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 and 511. Specifically, the control unit 600 controls the filter core to be flushed from top to bottom by supplying nitrogen from the clean liquid chamber 31 of the filter 200 through the fourth pipe 22 by the nitrogen storage tank 200 when the differential pressure detecting device 322 shows more than 0.2bar, the third valve 411 is closed by the control unit 600, the fourth valve 221 and the fifth valve 511 are opened, and the high-concentration solid residue slurry deposited at the bottom of the feeding chamber 33 is supplied to the hydrolysis unit 500 for hydrolysis, based on the display of the differential pressure detecting device 322, and controls the fourth valve 221 and the fifth valve 511 to be closed by the control unit 600, the first valve 211 and the second valve 341 are opened, that is, the nitrogen is supplied to the mixer 100 through the first pipe 21 by the nitrogen storage tank 200, so that the mixture containing diatomite and silicon tetrachloride in the mixer 100 is supplied to the filter 300 through the feeding chamber 33 and into the filter chamber 32 to form a filter layer containing diatomite on the surface of the filter cloth of the filter core 321, then, the first valve 211 and the second valve 341 are closed, the third valve 411 is opened, and the chlorosilane residual liquid is supplied to the feeding cavity 33 of the filter 300 through the third pipeline 41 and then subjected to solid-liquid separation through a cake layer on the filter element 321. It should be noted that the control unit 600 is a conventional control device in the art, as long as the above functions can be achieved, and the structure thereof is not described herein again.
In still another aspect of the invention, the invention provides a method for filtering chlorosilane residual liquid by using the system. Referring to fig. 4-6, the method includes, in accordance with an embodiment of the present invention:
s100: feeding diatomite and silicon tetrachloride into a stirrer for mixing
In this step, diatomaceous earth and silicon tetrachloride were supplied to a stirrer to be mixed, so that a mixture was obtained. Specifically, the diatomite has a good microporous structure, good adsorption performance and good compression resistance, a good flow rate ratio of a filtered liquid can be obtained, fine suspended matters can be filtered, and the clarity is guaranteed, and the particle size of the diatomite particles used in the application is about 0.01-1 micron, so that a formed filter cake layer has high precision, and the preferable mass concentration of the diatomite in a mixture is 15-25%. The inventor finds that if the concentration of the diatomite in the mixture is too high, the mixture has poor fluidity and is easy to block pipelines; and if the concentration of the diatomite in the mixture is too low, the forming speed of the filter cake layer is slow, and the working efficiency is low. Therefore, the mass concentration can be adopted to avoid pipeline blockage and improve the working efficiency.
S200: nitrogen gas is supplied into the stirrer through a first pipe by using a nitrogen gas storage tank, and the mixture is supplied into the filter
In the step, filter cloth is wrapped on the side wall of a filter element 321 of a filter 300, then nitrogen is supplied into a stirrer 100 through a first pipeline 21 by using a nitrogen storage tank 200, a mixture containing diatomite and silicon tetrachloride in the stirrer 100 is supplied into the filter 300 and enters a filter cavity 32 through a feeding cavity 33, a filter cake layer (with the thickness of 8-12 mm, preferably 10mm) containing diatomite is formed 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 an inner cavity of the filter element 321, fine silicon powder in the chlorosilane residual liquid has larger granularity (10-100 mu m), is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by the diatomite, and is intercepted by smaller amorphous silicon (1-10 mu m) which partially passes through the surface of the filter cake and is intercepted by a micropore channel bent inside the diatomite and finer pores inside the filter cake, and metal chloride in the chlorosilane residual liquid is easily attached to the surface, a loose filter cake is formed, so that the chlorosilane residual liquid flows smoothly, the pressure difference between the clean liquid cavity and the feeding cavity cannot rise rapidly, and the chlorosilane clear liquid entering the inner cavity of the filter element 321 flows into the clean liquid cavity 31 along the axial direction of the filter element 321 and is discharged through the chlorosilane clear liquid outlet 301.
S300: a chlorosilane residual liquid storage tank is adopted to supply chlorosilane residual liquid to a feeding cavity of the filter through a third conveying pipeline
In the step, a chlorosilane residual liquid storage tank 400 is adopted to supply chlorosilane residual liquid into a feeding cavity 33 of a filter 300 through a third pipeline 41, so that the chlorosilane residual liquid is filtered through a filter cake layer to obtain slag slurry and a chlorosilane clear liquid. Specifically, the chlorosilane residual liquid mainly comprises the following components: monosilicchlorosilane mainly containing silicon tetrachloride, polysilichlorosilane 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 conveyed to the first pipeline 21 through the third pipeline 41, i.e., the chlorosilane residual liquid is supplied to the feeding 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, disclosed by the embodiment of the invention, the filter cloth is wrapped on the side wall of the filter element of the filter, then the nitrogen is supplied into the stirrer through the first pipeline by the nitrogen storage tank, the mixture containing the kieselguhr and the silicon tetrachloride in the stirrer is supplied to the filter to form the filter cake layer containing the kieselguhr on the surface of the filter cloth of the filter element, when the chlorosilane residual liquid flows through the kieselguhr filter cake layer, fine silicon powder in the chlorosilane residual liquid has larger granularity and is easily intercepted on the surface of the filter cake layer by the filter cake layer formed by the kieselguhr, and part of smaller amorphous silicon passing through the surface of the filter cake is intercepted by a tortuous micropore channel inside the kieselguhr and finer pores inside the filter cake, so that metal chloride in the chlorosilane residual liquid is easily attached to the surface of the filter cake layer and the surface of the silicon powder to form looseness, the chlorosilane, compare in current filter core or filter cloth and filter, the unable amorphous silica flour of interception of filter cloth and the problem that leads to equipment to block up can not exist in this application, also can not exist the filter core simultaneously and filter the problem that the short time of front and back pressure differential rises rapidly and the inspection of stopping. 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 the fourth valve and the fifth valve to be opened
In this step, when the pressure difference detecting device 322 indicates 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, namely, the chlorosilane residual liquid is stopped to be supplied at the moment, after no fluid action exists, the adhesive force of the silicon powder on the filter cake layer is reduced, the gravity action is larger than the adhesive force, the silicon powder on the surface can automatically fall off and deposit to the bottom of the feeding cavity 33, and the fourth valve 221 is opened, so that when the filter element 321 is flushed by the nitrogen (6bar) supplied from the clean liquid chamber 31, the fluid has been strengthened the silica flour effect that drops from last down flowing, and the solid sediment thick liquid of the high concentration of deposit to feeding chamber 33 bottom is discharged from feeding chamber 33 bottom, and the parking more current is overhauld the filter and need adopt nitrogen gas to carry out long-time replacement and the operation of renew cartridge to the filter and compare, and this application is lower to the washing mode labour saving and time saving and the cost of filter core.
S500: feeding the slurry to a hydrolysis unit for hydrolysis
In this step, the above-mentioned high-concentration solid slag slurry deposited to the bottom of the feed chamber 33 is supplied to the hydrolysis unit 500 to be subjected to hydrolysis treatment. Specifically, the unit 500 that hydrolysises of this application adopts glass steel matter sediment thick liquid to get into from the unit 500 bottom of hydrolysising, atomize through spiral spray nozzle 52, and the unit 500 that hydrolysises establishes three-layer spray assembly 53 altogether, spray assembly 53 and adopt ordinary water as the eluent, thick liquid after spiral spray nozzle 52 atomizes and spray assembly 53 spun water contact abundant reaction, generate silica hydrate and hydrochloric acid, send the three wastes station to handle after the unit bottom discharge hydrolysises, it can not continuously increase to a certain amount to have realized piling up the silica flour in filter 300, regular overhaul has been 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 indicates a pressure 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 200 through the fourth pipe 22 by using the nitrogen gas storage tank 200, flushes the filter element from top to bottom, and supplies the solid slurry of high concentration deposited on the bottom of the feed chamber 33 to the hydrolysis unit 500 for hydrolysis, and when the pressure difference detecting means 322 indicates a pressure 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, that is, the nitrogen gas is supplied to the agitator 100 through the first pipe 21 by using the nitrogen gas storage tank 200, so that the mixture containing diatomite and silicon tetrachloride in the agitator 100 is supplied to the filter 300 through the feed chamber 33 into the filter chamber 32 to form a filter cake layer containing diatomite on the surface of the filter element 321, then, the first valve 211 and the second valve 341 are closed, the third valve 411 is opened, and the chlorosilane residual liquid is supplied to the feeding cavity 33 of the filter 300 through the third pipeline 41 and then subjected to solid-liquid separation through a cake layer on the filter element 321.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean 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 invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer 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, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A filtration system of chlorosilane raffinate which characterized in that includes:
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 clean liquid cavity, a filter cavity and a feeding cavity are defined in the filter from top to bottom, a filter element arranged along the axial direction of the filter cavity is arranged in the filter cavity, the lower end of the filter element is closed, the side wall of the filter element is wrapped by 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 feeding cavity, the clean liquid 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;
and 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.
2. The system of claim 1, wherein a plurality of the filter elements are disposed in the filter cavity, and the plurality of filter elements are spaced apart along a radial direction of the filter cavity.
3. The system of claim 1 or 2, wherein the nitrogen storage tank is in communication with the clean liquid chamber via a fourth conduit, and wherein a fourth valve is provided on the fourth conduit.
4. The system of claim 3, further comprising: the hydrolysis unit is connected with the feeding cavity through a fifth pipeline, and a fifth valve is arranged on the fifth pipeline.
5. The system of claim 4, further comprising: 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.
6. A method for filtering chlorosilane raffinate by using the system as claimed in any one of claims 1 to 5, comprising:
(1) feeding diatomite and silicon tetrachloride into the stirrer for mixing so as to obtain a mixture;
(2) supplying nitrogen into the agitator through the first pipe using the nitrogen storage tank so as to supply the mixture into the filter so as to form a cake layer on the filter cloth;
(3) and feeding chlorosilane residual liquid into the feeding cavity of the filter through the third conveying pipeline by adopting the chlorosilane residual liquid storage tank, so that the chlorosilane residual liquid is filtered through the filter cake layer to obtain slag slurry and chlorosilane clear liquid.
7. The method according to claim 6, wherein in the step (1), the mass concentration of the diatomite in the mixture is 15-25%.
8. The method of claim 6 or 7, further comprising:
(4) and when the pressure difference detection device displays that the pressure difference is higher than 0.2bar, the control unit controls to close the third valve, open the fourth valve and the fifth valve, and supply nitrogen from the liquid purifying cavity of the filter through the fourth pipeline by using the nitrogen storage tank so as to flush the filter cloth.
9. The method of claim 8, further comprising: (5) and feeding the slag slurry to a hydrolysis unit for hydrolysis treatment.
10. The method of claim 9, further comprising: (6) and when the pressure difference detection device is lower than 0.05bar, the control unit controls to close the fourth valve and the fifth valve, open the first valve and the second valve so as to form a filter cake layer on the filter cloth, close the first valve and the second valve and open the third valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010060396.4A CN111072032B (en) | 2020-01-19 | 2020-01-19 | Chlorosilane raffinate filtration system and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010060396.4A CN111072032B (en) | 2020-01-19 | 2020-01-19 | Chlorosilane raffinate filtration system and method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111072032A true CN111072032A (en) | 2020-04-28 |
| CN111072032B CN111072032B (en) | 2023-12-15 |
Family
ID=70323794
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010060396.4A Active CN111072032B (en) | 2020-01-19 | 2020-01-19 | Chlorosilane raffinate filtration system and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111072032B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498853A (en) * | 2020-04-28 | 2020-08-07 | 中国恩菲工程技术有限公司 | Cracking process for byproduct chlorosilane high-boiling residue in polycrystalline silicon production |
| CN111661827A (en) * | 2020-06-22 | 2020-09-15 | 四川永祥多晶硅有限公司 | System and method for recycling silicon powder in polycrystalline silicon reduction tail gas |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108862284A (en) * | 2018-07-18 | 2018-11-23 | 兰州天大华瑞环境工程技术有限公司 | A kind of production of polysilicon link slurry processing unit and method |
| CN209098195U (en) * | 2018-10-17 | 2019-07-12 | 中国恩菲工程技术有限公司 | The system that chlorosilane raffinate chilling removes metal chloride |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10030252A1 (en) * | 2000-06-20 | 2002-01-03 | Degussa | Separation of metal chlorides from their suspensions in chlorosilanes |
-
2020
- 2020-01-19 CN CN202010060396.4A patent/CN111072032B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108862284A (en) * | 2018-07-18 | 2018-11-23 | 兰州天大华瑞环境工程技术有限公司 | A kind of production of polysilicon link slurry processing unit and method |
| CN209098195U (en) * | 2018-10-17 | 2019-07-12 | 中国恩菲工程技术有限公司 | The system that chlorosilane raffinate chilling removes metal chloride |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498853A (en) * | 2020-04-28 | 2020-08-07 | 中国恩菲工程技术有限公司 | Cracking process for byproduct chlorosilane high-boiling residue in polycrystalline silicon production |
| CN111661827A (en) * | 2020-06-22 | 2020-09-15 | 四川永祥多晶硅有限公司 | System and method for recycling silicon powder in polycrystalline silicon reduction tail gas |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111072032B (en) | 2023-12-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111072032B (en) | Chlorosilane raffinate filtration system and method | |
| JP5511667B2 (en) | Method for producing hydrogen gas from hydrogen halide, mixed gas containing hydrogen and silicon halide, method for producing silicon compound using the hydrogen gas, and plant for the method | |
| CN109231217B (en) | System and method for rapidly cooling chlorosilane raffinate to remove metal chloride | |
| CN204735022U (en) | Purification recovery unit of chlorosilane waste liquid | |
| CN211920883U (en) | Filtration system of chlorosilane raffinate | |
| CN104841195A (en) | Purification and recovery device for chlorosilane waste liquid and purification and recovery method for chlorosilane waste liquid | |
| CN104955770A (en) | Method for producing trichlorosilane | |
| CN104085977B (en) | A kind of filler catalytic tower | |
| CN111072033A (en) | Pretreatment system and method for chlorosilane residual liquid | |
| CN101528665A (en) | Method for producing electronic grade 2,2'-aminoethoxyethanol | |
| JPH0568869A (en) | Reaction method for suspended catalyst system | |
| CN211920882U (en) | Pretreatment system for chlorosilane residual liquid | |
| CN214422397U (en) | Multi-stage water purifying device for treating wastewater | |
| CN106986345A (en) | A kind of method for producing silicochloroform | |
| CN212076413U (en) | Carbon dioxide filters eduction gear for hydrogen manufacturing of methanol-water | |
| CN210825757U (en) | Integrated combined air-float filtering device | |
| CN211946554U (en) | Greasy dirt clearing device of digit control machine tool cutting fluid | |
| CN220142732U (en) | Slag slurry filtering and recycling system | |
| CN103055769B (en) | Organic silicon monomer fluidized bed film reactor and technology thereof | |
| CN220424860U (en) | System for improve polycrystalline silicon reduction tail gas silica flour and retrieve | |
| CN203043727U (en) | Silica sol purifying and filtering device | |
| CN102557045A (en) | Method and device for producing white carbon black and carbon tetrachloride by adopting plasma process | |
| CN211770421U (en) | Regeneration-free resin oil removal and filtration device | |
| CN218280927U (en) | Solid-containing emptying tail gas separation system | |
| CN220460078U (en) | Chlorosilane slag slurry treatment device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |