CN116534864A - Chlorosilane rectifying and impurity removing process and system in polysilicon production - Google Patents
Chlorosilane rectifying and impurity removing process and system in polysilicon production Download PDFInfo
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- CN116534864A CN116534864A CN202310585447.9A CN202310585447A CN116534864A CN 116534864 A CN116534864 A CN 116534864A CN 202310585447 A CN202310585447 A CN 202310585447A CN 116534864 A CN116534864 A CN 116534864A
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- 239000012535 impurity Substances 0.000 title claims abstract description 67
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 50
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 45
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 38
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000008569 process Effects 0.000 title claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 213
- 238000007323 disproportionation reaction Methods 0.000 claims abstract description 162
- 239000002994 raw material Substances 0.000 claims abstract description 55
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000005052 trichlorosilane Substances 0.000 claims abstract description 50
- 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 46
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000001179 sorption measurement Methods 0.000 claims abstract description 28
- 238000000605 extraction Methods 0.000 claims description 118
- 238000010992 reflux Methods 0.000 claims description 53
- 238000011084 recovery Methods 0.000 claims description 8
- 238000011144 upstream manufacturing Methods 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 17
- 239000012071 phase Substances 0.000 description 17
- 239000007791 liquid phase Substances 0.000 description 15
- 239000000047 product Substances 0.000 description 14
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 239000002184 metal Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 229910003902 SiCl 4 Inorganic materials 0.000 description 5
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 102100030511 Stanniocalcin-1 Human genes 0.000 description 1
- 101710142157 Stanniocalcin-1 Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- YGHUUVGIRWMJGE-UHFFFAOYSA-N chlorodimethylsilane Chemical compound C[SiH](C)Cl YGHUUVGIRWMJGE-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000005048 methyldichlorosilane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000003786 synthesis reaction 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
- C01B33/10778—Purification
-
- 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
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/03—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a chlorosilane rectifying impurity-removing process and a chlorosilane rectifying impurity-removing system in polysilicon production, wherein raw chlorosilane is subjected to raw material adsorption tower to remove part of impurities; the raw material chlorosilane after impurity removal enters a rough separation tower, dichlorosilane and light impurities are removed from the tower top, silicon tetrachloride and heavy impurities are removed from the tower bottom, trichlorosilane is extracted from the side line of the tower and enters a light removal tower, light impurities are removed from the upper tower top of the light removal tower, and the extracted material from the lower tower bottom of the light removal tower enters a heavy removal tower; removing heavy impurities from the lower tower kettle of the heavy removal tower, and collecting qualified trichlorosilane products from the upper tower top of the heavy removal tower; the removed impurities are all recovered and then are sent into a separation tower for component separation after the reverse disproportionation, the separated dichlorosilane and silicon tetrachloride are sent into a reverse disproportionation reactor for reverse disproportionation reaction after being mixed, and the generated trichlorosilane, unreacted dichlorosilane and silicon tetrachloride enter the separation tower for component separation after the reverse disproportionation again; after the reverse disproportionation, separating trichlorosilane from the side line of the separating tower, and returning to carry out rectification and impurity removal.
Description
Technical Field
The invention belongs to the field of polysilicon production, and particularly relates to a chlorosilane rectification impurity removal process and system in polysilicon production.
Background
Trichlorosilane rectification is one of core technologies of a polysilicon production process, and the purification degree of the trichlorosilane directly influences the purity of polysilicon of a final product, and the purity of the polysilicon influences the power generation effect of a downstream solar cell. The silicon powder, hydrogen chloride and intermediate products produced in the chemical reaction of each procedure in the production of polysilicon contain phosphorus, boron, metal impurities and the like which affect the quality of the polysilicon.
Most of the existing electronic grade polysilicon production adopts an improved Siemens method, adopts a rectification system with four or five stages of rectification towers connected in series, and the trichlorosilane product has low yield and part of chlorosilane raw materials cannot be completely recycled. The production requirements of electronic grade polysilicon can not be met, and the problems of high energy consumption, low material utilization rate and the like can not be met.
At present, most of polysilicon production enterprises adopt multi-tower rectification for rectification and purification, generally adopts a 5-stage rectification process, and the flow is as follows: coarse separation tower, light component removing tower, heavy component removing tower, light component removing tower and heavy component removing tower. The process has the following problems: (1) the investment of multi-stage rectifying equipment is large; (2) the separation effect of each rectifying tower is poor, the tower is easy to cut off greatly, the product yield is low, the energy consumption is high, and the product is easy to disqualify; (3) the material is high, and the recycling rate is low; (4) the quality of the product is unstable under the influence of raw material impurities.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the invention provides a chlorosilane rectifying and impurity removing process and system in polysilicon production, which can reduce the equipment investment of the same productivity by more than 20 percent and effectively reduce the production energy consumption; closed circulation of the rectification system is realized, and material recycling is realized; stable quality of trichlorosilane and meets the production requirement of electronic grade polysilicon.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a chlorosilane rectifying and impurity removing process in polysilicon production comprises the following steps:
introducing upstream raw material chlorosilane into a raw material adsorption tower to remove impurities, and removing most of phosphorus, boron and metal impurities in the raw material chlorosilane;
the chlorsilane after impurity removal is sent to a rough separation tower, and the rough separation tower is provided with at least three outlets of a tower top extraction pipe of the rough separation tower, a tower bottom extraction pipe of the rough separation tower and a side extraction pipe of the middle line of the rough separation tower; removing dichlorosilane and light impurities from the tower top, removing silicon tetrachloride and heavy impurities from the tower bottom, and extracting trichlorosilane from the middle side line of the tower;
the materials extracted from the side extraction pipe in the coarse separation tower are sent into a light component removal tower and a heavy component removal tower, the light component removal tower is at least provided with two outlets of an upper tower top extraction pipe and a lower tower bottom extraction pipe of the light component removal tower, and light impurities (part of dichlorosilane DCS is mixed in the light impurities) are removed through the upper tower top of the light component removal tower; the materials extracted from the extraction pipe at the lower tower kettle of the light component removing tower are sent into the heavy component removing tower; the heavy impurity (part of silicon tetrachloride STC is mixed in the heavy impurity) is removed from the lower tower kettle of the heavy-removal tower, and a qualified trichlorosilane product is produced from the upper tower top extraction pipe of the heavy-removal tower;
the materials extracted from the top extraction pipe of the coarse separation tower, the extraction pipe of the bottom extraction pipe of the coarse separation tower, the upper top of the light component removal tower and the bottom extraction pipe of the heavy component removal tower are sent into the reverse disproportionation separation tower for component separation; the anti-disproportionation separation tower is configured to be provided with at least three outlets of an anti-disproportionation separation tower top extraction pipe, an anti-disproportionation separation tower kettle extraction pipe and a anti-disproportionation separation tower middle side extraction pipe, wherein the anti-disproportionation separation tower top extraction pipe and the anti-disproportionation separation tower kettle extraction pipe are used for feeding materials extracted from the anti-disproportionation separation tower kettle extraction pipe into an anti-disproportionation reactor for anti-disproportionation reaction, and then feeding the materials into the anti-disproportionation separation tower again; the dichlorosilane and the silicon tetrachloride separated by the separation tower after the reverse disproportionation are sent into a reverse disproportionation reactor for the reverse disproportionation reaction to generate trichlorosilane, and the generated trichlorosilane, unreacted dichlorosilane and silicon tetrachloride enter the separation tower after the reverse disproportionation again for component separation;
and (3) re-feeding the materials extracted from the side extraction pipe in the separation tower after the anti-disproportionation and the upstream raw material chlorosilane into the raw material adsorption tower, and recycling the steps to finally extract qualified trichlorosilane products from the upper tower top of the heavy removal tower.
Further, the dichlorosilane separated from the top of the separation tower after the anti-disproportionation and the silicon tetrachloride separated from the bottom of the separation tower after the anti-disproportionation are subjected to batching calculation before mixing, and the silicon tetrachloride is fed in from the outside, so that the dichlorosilane is completely reacted, and the reaction formula is as follows: siH (SiH) 2 Cl 2 +SiCl 4 →SiHCl 3 。
The invention further provides a chlorosilane rectifying and impurity removing system in the production of polysilicon, which comprises a raw material buffer tank, a coarse separation tower, a light removal tower, a heavy removal tower, a reverse disproportionation post-separation tower and a reverse disproportionation reactor; the raw material buffer tank rough separation tower, the light component removal tower and the heavy component removal tower are sequentially connected through pipelines;
the tower side of the rough separation tower is connected to a light component removal tower through a pipeline, the lower tower kettle of the light component removal tower is connected to a heavy component removal tower through a pipeline, and the upper tower top of the heavy component removal tower is used for extracting qualified trichlorosilane products through a pipeline;
the top and the bottom of the crude separation tower, the upper top of the light component removal tower and the lower bottom of the heavy component removal tower are respectively connected to the reverse disproportionation post-separation tower together through a production pipeline; the top and the bottom of the separation tower after the anti-disproportionation are respectively connected to the anti-disproportionation reactor through a extraction pipeline, and the tower side of the separation tower after the anti-disproportionation is reconnected to the raw material buffer tank through the extraction pipeline; the anti-disproportionation reactor returns to the separation tower after anti-disproportionation through the extraction pipeline, and the mixed gas generated by the reaction is separated again.
Further, a mixer is arranged between the reverse disproportionation post-separation tower and the reverse disproportionation reactor; the top and the bottom of the separation tower are respectively connected to a mixer through a extraction pipeline after the anti-disproportionation, and are mixed and then sent into the anti-disproportionation reactor.
Further, the feeding side of the mixer is also connected with a silicon tetrachloride feeding pipe.
Further, the system also comprises a feed buffer tank of the separation tower after the reverse disproportionation; the feeding buffer tank of the separation tower after the reverse disproportionation is arranged at the front end of the separation tower after the reverse disproportionation and is used for buffering the impurity-containing materials extracted from the coarse separation tower, the light component removal tower and the heavy component removal tower; the top and bottom of the coarse separation tower, the top of the light component removal tower and the bottom of the heavy component removal tower are respectively connected to a feed buffer tank of the anti-disproportionation separation tower together through a production pipeline, and then are sent to the anti-disproportionation separation tower after being buffered; the anti-disproportionation reactor is connected to a feed buffer tank of the separation tower after anti-disproportionation through a production line.
Further, a raw material adsorption tower is arranged between the raw material buffer tank and the coarse separation tower; the front end of the feeding side of the feeding buffer tank of the reverse disproportionation separation tower is provided with a reclaimed material adsorption tower; the top of the coarse separation tower, the tower kettle, the upper top of the light component removal tower and the lower tower kettle of the heavy component removal tower are respectively connected into the reclaimed material adsorption tower together through a production pipeline. And removing most of phosphorus, boron and metal impurities in the raw materials through the raw material adsorption tower and the reclaimed material adsorption tower.
Specifically, a crude separation tower top reflux pipe is arranged at the top of the crude separation tower, and a condenser and a crude separation tower top extraction pipe are arranged on the crude separation tower top reflux pipe; a reflux pipe of the coarse separation tower kettle is arranged at the lower tower kettle of the coarse separation tower, and a reboiler and a extraction pipe of the coarse separation tower kettle are arranged on the reflux pipe of the coarse separation tower kettle; the tower side of the rough separation tower is provided with a rough separation tower middle side line extraction pipe, and the rough separation tower middle side line extraction pipe is connected to the light component removal tower.
Specifically, the light component removing tower comprises an upper light component removing tower and a lower light component removing tower which are sequentially connected in series; the top of the upper tower of the light component removing tower is provided with a reflux pipe at the top of the upper tower of the light component removing tower; a condenser and a top extraction pipe of the light component removal tower are arranged on the top reflux pipe of the light component removal tower; the bottom of the upper tower of the light component removing tower is connected to the lower tower of the light component removing tower through a production pipe at the bottom of the upper tower of the light component removing tower;
the top of the lower light component removing tower is provided with a lower light component removing tower top gas phase pipe, and the lower light component removing tower top gas phase pipe is connected to an upper light component removing tower again; the bottom of the lower tower of the light component removal tower is provided with a return pipe of the lower tower kettle of the light component removal tower, the return pipe of the lower tower kettle of the light component removal tower is provided with a reboiler and a extraction pipe of the lower tower kettle of the light component removal tower, and the extraction pipe of the lower tower kettle of the light component removal tower is connected to the heavy component removal tower.
Specifically, the weight removing tower comprises a lower weight removing tower and an upper weight removing tower which are sequentially connected in series; the top of the lower tower of the weight removing tower is provided with a lower tower top gas phase pipe of the weight removing tower, and the lower tower top gas phase pipe of the weight removing tower is connected to an upper tower of the weight removing tower; the bottom of the lower tower of the weight removing tower is provided with a reflux pipe of the lower tower kettle of the weight removing tower, and the reflux pipe of the lower tower kettle of the weight removing tower is provided with a reboiler and a extraction pipe of the lower tower kettle of the weight removing tower;
the top of the upper tower of the weight removing tower is provided with a top reflux pipe of the upper tower of the weight removing tower, the top reflux pipe of the upper tower of the weight removing tower is provided with a condenser and a top extraction pipe of the upper tower of the weight removing tower, and qualified trichlorosilane products are extracted through the top extraction pipe of the upper tower of the weight removing tower; the bottom of the upper tower of the weight removing tower is provided with a extraction pipe at the bottom of the upper tower kettle of the weight removing tower, and the extraction pipe at the bottom of the upper tower kettle of the weight removing tower is reconnected to the lower tower of the weight removing tower.
Specifically, a top reflux pipe of the anti-disproportionation separation tower is arranged at the top of the anti-disproportionation separation tower, and a condenser and a top extraction pipe of the anti-disproportionation separation tower are arranged on the top reflux pipe of the anti-disproportionation separation tower; the lower tower kettle of the anti-disproportionation separation tower is provided with an anti-disproportionation separation tower kettle reflux pipe, and the anti-disproportionation separation tower kettle reflux pipe is provided with a reboiler and an anti-disproportionation separation tower kettle extraction pipe; the side of the anti-disproportionation separation tower is provided with a middle side line extraction pipe of the anti-disproportionation separation tower, and the middle side line extraction pipe of the anti-disproportionation separation tower is reconnected to the raw material buffer tank; and the extraction pipe at the top of the separation tower after the reverse disproportionation and the extraction pipe at the bottom of the separation tower after the reverse disproportionation are connected to the mixer together.
Specifically, the bottom of the anti-disproportionation reactor is provided with an anti-disproportionation reactor extraction pipe, and the anti-disproportionation reactor extraction pipe is reconnected to the feeding buffer tank of the separation tower after anti-disproportionation.
The beneficial effects are that:
(1) The invention utilizes the combination of adsorption and rectification coupling, and through two-stage adsorption impurity removal and high-efficiency coupling rectification, the rectification process level in the production of polysilicon is effectively solved, the trichlorosilane product meets the production requirement of electronic grade polysilicon, and the production energy consumption and material consumption are greatly reduced.
(2) After the secondary adsorption and impurity removal are carried out on the cut materials of each rectifying tower, the cut materials are recycled through a disproportionation system, trichlorosilane produced after the disproportionation reaction is supplemented into chlorosilane raw materials, dichlorosilane and silicon tetrachloride are recycled, and the complete circulation of the materials is realized.
(3) The invention relates to a device for rectifying and purifying trichlorosilane, which comprises a raw material adsorption tower, a coarse separation tower (baffle tower), a light component removing tower (string tower), a heavy component removing tower (string tower), a recovery adsorption tower, a reverse disproportionation reactor, a reverse disproportionation post-separation tower (baffle tower) and other key equipment, and can distinguish various boiling components under the condition of guaranteeing the rectifying quality so as to realize the effective utilization of resources.
Drawings
The foregoing and/or other advantages of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings and detailed description.
Fig. 1 is a schematic diagram of the overall structure of a chlorosilane rectification impurity removal system in the production of polysilicon.
Wherein each reference numeral represents:
10 raw material buffer tanks; 101 chlorosilane raw material guiding pipe; 102 chlorosilane raw material conveying pipes; 20 raw material adsorption towers; 30 coarse separation tower; 301 coarse separation tower top reflux pipe; 302 coarse separation tower kettle return pipe; 303 a side line extraction pipe in the rough separation tower; 304 a crude separation tower top extraction pipe; 305 a coarse separation tower kettle extraction pipe; 40, loading the light component into a tower; 401 a reflux pipe at the top of the light component removing tower; a extraction pipe is arranged at the bottom of the upper tower of the light component removing tower 402; 403 a light component removing tower top extraction pipe; 50, lower tower of the light component removing tower; 501 a gas phase pipe at the lower tower top of the light component removing tower; 502 reflux pipe of lower tower kettle of light component removing tower; 503 a light component removing tower bottom extraction pipe; 60, lower tower of the heavy-removal tower; 601 the lower overhead gas phase pipe of the de-weight tower; 602 a reflux pipe of a lower tower kettle of the heavy removal tower; 603 a stripping tower bottom extraction pipe; 70, loading the heavy-removal tower; 701, a reflux pipe at the top of the heavy-duty removing tower; a bottom extraction pipe of an upper tower kettle of the 702 heavy removal tower; 703 stripping the top extraction pipe of the heavy-duty tower; 80 a reclaimed material adsorption tower; feeding a buffer tank into the separation tower after 90-degree reverse disproportionation; 100 reverse disproportionation and separation tower; 1001, reversely disproportionating and separating a tower top return pipe; 1002 reverse disproportionation and separating a tower kettle return pipe; 1003 the side line extraction pipe in the separation tower after the reverse disproportionation; 1004 a recovery pipe at the top of the separation tower after the reverse disproportionation; 1005, a recovery pipe is arranged at the bottom of the separation tower after the reverse disproportionation; 110 a mixer; 1101 silicon tetrachloride feeding pipe; a 120-type anti-disproportionation reactor; 1201 a reverse disproportionation reactor extraction tube.
DCS is dichlorosilane; TCS is trichlorosilane (liquid phase); STC is silicon tetrachloride; LI is light impurity (light impurity); HI is heavy (heavies).
Detailed Description
The invention will be better understood from the following examples.
As shown in fig. 1, the chlorosilane rectifying and impurity removing system in the production of polysilicon comprises a raw material buffer tank 10, a raw material adsorption tower 20, a coarse separation tower 30, a light component removal tower, a heavy component removal tower, a reverse disproportionation rear separation tower feeding buffer tank 90, a reverse disproportionation rear separation tower 100, a mixer 110 and a reverse disproportionation reactor 120; the raw material buffer tank 10, the raw material adsorption tower 20, the coarse separation tower 30, the light and heavy removal tower are sequentially connected through pipelines.
The column side of the rough separation column 30 is connected to the light ends column by a pipe, and relatively pure Trichlorosilane (TCS) extracted from the side line is fed into the light ends column to further remove Light Impurities (LI). The lower tower kettle of the light component removal tower is connected to the heavy component removal tower through a pipeline to further remove heavy component (HI). Qualified trichlorosilane products are extracted from the top of the upper tower of the heavy-removal tower through a pipeline.
The top and bottom of the coarse separation column 30, the top of the light component removal column, and the bottom of the heavy component removal column are connected to the feed buffer tank 90 of the separation column after the reverse disproportionation through extraction pipelines respectively, and the cut raw material impurities are completely recovered.
The feed buffer tank 90 of the separation tower after the reverse disproportionation and the separation tower 100 after the reverse disproportionation are connected in sequence through pipelines; the top and the bottom of the separation tower 100 are respectively connected to the mixer 110 through a production line, dichlorosilane (DCS) is produced from the top of the separation tower, and Silicon Tetrachloride (STC) is produced from the bottom of the separation tower. The column side of the separation column 100 after the reverse disproportionation is reconnected to the raw material buffer tank 10 through a withdrawal line, and the withdrawn Trichlorosilane (TCS) is reused as a raw material for rectification and impurity removal. The mixer 110 and the anti-disproportionation reactor 120 are connected in sequence through a pipeline, and SiH mainly occurs in the anti-disproportionation reactor 120 2 Cl 2 +SiCl 4 →SiHCl 3 This reaction, the Trichlorosilane (TCS) produced by the reaction, as well as the unreacted Dichlorosilane (DCS) and Silicon Tetrachloride (STC), is returned again for separation via the withdrawal line to the post-disproportionation separation column feed buffer tank 90.
The content of dichlorosilane in raw material chlorosilane is higher than that of silicon tetrachloride, and the anti-disproportionation reaction ensures the complete consumption of dichlorosilane. Therefore, a silicon tetrachloride feed pipe 1101 is also connected to the feed side of the mixer 110, and Dichlorosilane (DCS) is fully reacted as much as possible by feeding sufficient Silicon Tetrachloride (STC).
The coarse separation tower 30 is a baffle tower, a coarse separation tower top reflux pipe 301 is arranged at the tower top, a condenser and a coarse separation tower top extraction pipe 304 are arranged on the coarse separation tower top reflux pipe 301, and Light Impurities (LI) and Dichlorosilane (DCS) at the tower top are extracted by setting reflux ratio. The reflux pipe 301 of the top of the rough separation tower is a gas phase pipe positioned at the front section of the condenser, a liquid phase pipe positioned at the rear section of the condenser, the gas phase discharged from the top of the rough separation tower is condensed into a liquid phase through the condenser, one part of the liquid phase is circulated into the rough separation tower 30, and the other part of the liquid phase is extracted from the extraction pipe 304 of the top of the rough separation tower. The lower tower kettle of the rough separation tower 30 is provided with a rough separation tower kettle return pipe 302, and the rough separation tower kettle return pipe 302 is provided with a reboiler and a rough separation tower kettle extraction pipe 305 to extract Heavy Impurities (HI) and Silicon Tetrachloride (STC) from the tower kettle. The reflux pipe 302 of the crude separation tower kettle is positioned at the front section of the reboiler and is a liquid phase pipe, the back section of the reboiler is a gas phase pipe, one part of liquid phase from the crude separation tower kettle is sent into the reboiler through the reboiler to be gasified and then returned to the crude separation tower 30 again, and the other part of liquid phase is extracted from the extraction pipe 305 of the crude separation tower kettle. The column side of the crude separation column 30 is provided with a crude separation column middle side line extraction pipe 303 for extracting purer Trichlorosilane (TCS), and is connected to the light component removal column through the crude separation column middle side line extraction pipe 303.
The light component removing tower is a serial tower and comprises a light component removing tower upper tower 40 and a light component removing tower lower tower 50 which are sequentially connected in series; the top of the upper light component removing tower 40 is provided with an upper light component removing tower top reflux pipe 401; a condenser and a top extraction pipe 403 are arranged on the top reflux pipe 401 of the light component removal tower, and the light component (LI) at the top of the tower and the Dichlorosilane (DCS) mixed therein are extracted by setting reflux ratio. The overhead reflux pipe 401 of the light component removal tower is a gas phase pipe positioned at the front section of the condenser, a liquid phase pipe positioned at the rear section of the condenser, the gas phase discharged from the top of the tower is condensed into a liquid phase by the condenser, one part of the liquid phase is circulated into the overhead 40 of the light component removal tower, and the other part of the liquid phase is extracted from the extraction pipe 403 of the overhead of the light component removal tower. The bottom of the upper light ends column 40 is connected to the lower light ends column 50 by an upper light ends column bottom draw line 402.
The top of the lower light component removing tower 50 is provided with a lower light component removing tower top gas phase pipe 501, and is reconnected to the upper light component removing tower 40 through the lower light component removing tower top gas phase pipe 501; the bottom of the lower light component removing tower 50 is provided with a lower light component removing tower kettle reflux pipe 502, the lower light component removing tower kettle reflux pipe 502 is provided with a reboiler and a lower light component removing tower kettle extraction pipe 503, and the lower light component removing tower kettle extraction pipe 503 is connected to a heavy component removing tower for further heavy component removing. The reflux pipe 502 of the lower tower kettle of the light component removing tower is positioned at the front section of the reboiler and is a liquid phase pipe, the rear section of the reboiler is a gas phase pipe, one part of liquid phase from the lower tower kettle of the light component removing tower is sent into the reboiler for gasification and then returns to the lower tower 50 of the light component removing tower again through the reboiler, and the other part of liquid phase is extracted from the extraction pipe 503 of the lower tower kettle of the light component removing tower and is sent into the heavy component removing tower.
The weight removing tower is also a serial tower and comprises a lower weight removing tower 60 and an upper weight removing tower 70 which are sequentially connected in series; the top of the lower de-weight tower 60 is provided with a lower de-weight tower top gas phase pipe 601, and the lower de-weight tower top gas phase pipe 601 is connected to the upper de-weight tower 70; the bottom of the lower tower 60 of the weight removing tower is provided with a reflux pipe 602 of the lower tower kettle of the weight removing tower, the reflux pipe 602 of the lower tower kettle of the weight removing tower is provided with a reboiler and a recovery pipe 603 of the lower tower kettle of the weight removing tower, and Heavy Impurities (HI) of the tower kettle and Silicon Tetrachloride (STC) mixed in the reflux pipe are recovered.
The top of the upper tower 70 of the weight removing tower is provided with an upper tower top reflux pipe 701 of the weight removing tower, the upper tower top reflux pipe 701 of the weight removing tower is provided with a condenser and an upper tower top extraction pipe 703 of the weight removing tower, and qualified trichlorosilane products are extracted through the upper tower top extraction pipe 703 of the weight removing tower; the bottom of the upper de-weight tower 70 is provided with a bottom extraction pipe 702 of the upper de-weight tower, and the bottom extraction pipe 702 of the upper de-weight tower is reconnected to the lower de-weight tower 60.
The front end of the feed side of the reverse disproportionation rear separation column feed buffer tank 90 is provided with a recycle material adsorption column 80 which acts the same as the raw material adsorption column 20 for removing phosphorus, boron and metal impurities in the raw material. The top and bottom of the rough separation column 30, the top of the light component removal column, and the bottom of the heavy component removal column are connected to the recovery adsorption column 80 through extraction pipelines.
The top of the separation column 100 after the reverse disproportionation is provided with a reflux pipe 1001 at the top of the separation column after the reverse disproportionation, the reflux pipe 1001 at the top of the separation column after the reverse disproportionation is provided with a condenser and a recovery pipe 1004 at the top of the separation column after the reverse disproportionation, and Dichlorosilane (DCS) is recovered by setting a reflux ratio. The lower tower kettle of the separation tower 100 after the anti-disproportionation is provided with a reflux pipe 1002 of the separation tower kettle after the anti-disproportionation, and the reflux pipe 1002 of the separation tower kettle after the anti-disproportionation is provided with a reboiler and a extraction pipe 1005 of the separation tower kettle after the anti-disproportionation so as to extract Silicon Tetrachloride (STC). The column side of the post-disproportionation separation column 100 is provided with a post-disproportionation separation column middle side offtake pipe 1003 for discharging Trichlorosilane (TCS), and is reconnected to the raw material buffer tank 10 through the post-disproportionation separation column middle side offtake pipe 1003. The post-disproportionation separation tower top extraction pipe 1004 and the post-disproportionation separation tower bottom extraction pipe 1005 are connected to the mixer 110 together, and the extracted Dichlorosilane (DCS) and Silicon Tetrachloride (STC) are mixed and then fed into the post-disproportionation reactor 120 for reaction, wherein the reaction formula is as follows: siH (SiH) 2 Cl 2 +SiCl 4 →SiHCl 3 。
The bottom of the anti-disproportionation reactor 120 is provided with an anti-disproportionation reactor extraction pipe 1201, and the anti-disproportionation reactor extraction pipe 1201 is reconnected to the feeding buffer tank 90 of the separation tower after the anti-disproportionation to separate the Trichlorosilane (TCS) generated by the reaction, the unreacted Dichlorosilane (DCS) and the Silicon Tetrachloride (STC) again.
The chlorosilane rectifying and impurity removing process flow in the polysilicon production of the invention mainly comprises the following steps:
upstream raw material chlorosilane is fed into the raw material buffer tank 10 through the chlorosilane raw material guide pipe 101, and then most of phosphorus, boron and metal impurities in raw material chlorosilane are removed through the raw material adsorption tower 20 first through the chlorosilane raw material conveying pipe 102. And the raw materials enter a rough separation tower 30 (a baffle tower), the rough separation tower 30 can cut off dichlorosilane and light impurities from the tower top at the same time, cut off silicon tetrachloride and heavy impurities from the tower kettle, and extract 99.99% of trichlorosilane from the middle side line of the tower, so that the light and heavy removal functions of the front two-stage tower in the traditional polysilicon synthesis material rectification flow are achieved, and the boron and phosphorus contents in the side line of the extracted trichlorosilane can be less than 10ppbw. The side-line extracted trichlorosilane enters a light component removing tower (stringing tower), the upper tower 40 of the light component removing tower mainly removes light components, the lower tower 50 of the light component removing tower extracts materials enter a heavy component removing tower (stringing tower), and the lower tower 60 of the heavy component removing tower mainly removes heavy components. Qualified trichlorosilane products are extracted from the upper tower 70 of the heavy-duty removal tower.
All the towers are cut off and recycled, the recycle material adsorption tower 80 is used for recycling the adsorption tower for impurity removal treatment, and the treated chlorosilane (containing dichlorosilane, trichlorosilane and silicon tetrachloride) is sent to a reverse disproportionation rear separation tower 100 (baffle tower) for component separation after passing through a reverse disproportionation feeding buffer tank 90. The dichlorosilane is extracted from the top of the separation tower 100 after the anti-disproportionation, the silicon tetrachloride is fully recycled from the bottom of the separation tower 100 after the anti-disproportionation, and the dichlorosilane and the silicon tetrachloride with a certain proportion are subjected to the anti-disproportionation reaction (reaction type: siH) in the anti-disproportionation reactor 120 after passing through the mixer 110 2 Cl 2 +SiCl 4 →SiHCl 3 ) Trichlorosilane is generated, the part of trichlorosilane is used for rectifying trichlorosilane raw materials, and because the proportion of Dichlorosilane (DCS) is large, fresh silicon tetrachloride STC is additionally supplemented through a silicon tetrachloride supplementing pipe 1101 when necessary, so that the Dichlorosilane (DCS) is reacted completely as much as possible to generate the trichlorosilaneSilicon chloride (TCS). The anti-disproportionation reaction is carried out in a catalyst bed, the reaction proportion of STC/DCS is 3-5, the reaction temperature is generally controlled between 40-50 ℃, and the reaction pressure is controlled to be about 0.2Mpa.
In the invention, the upstream raw material chlorosilane is dichlorosilane SiH 2 Cl 2 Trichlorosilane SiHCl 3 Silicon tetrachloride SiCl 4 And mixtures of impurities. The chlorosilane raw material comprises the following components in parts by mass: DCS-3%, TCS-96%, STC-1%, and the components slightly fluctuate during the production process. The impurities such as boron, phosphorus and the like are BCl 3 、PCl 3 、BCl 5 、PH 3 、B 2 H 6 Other metal impurities such as methyldichlorosilane and dimethylmonochlorosilane. The light component removing tower and heavy component removing tower are serial towers, and are divided into upper tower and lower tower, the tower reboiler and condenser are only one, and its auxiliary equipment is equipped quantity of single tower, and the upper tower and lower tower are connected with a reflux pipe by means of a gas phase pipe so as to implement energy transfer. By adopting the impurity removal process and the impurity removal system, the equipment investment of the same capacity can be reduced by more than 20%, and the production energy consumption is effectively reduced; closed circulation of the rectification system is realized, and material recycling is realized; stable quality of trichlorosilane and meets the production requirement of electronic grade polysilicon.
Example 1
The trichlorosilane raw material is pumped to the coarse separation tower through a feeding pump at the flow rate of 50t/h, and the content of the feeding impurity, the process impurity and the product impurity is detected, so that the content of the trichlorosilane product impurity meets the production requirement of electronic grade polysilicon in the data and actual production process, and specific data are shown in the process chlorosilane impurity detection data of table 1.
TABLE 1 Process chlorosilane impurity detection data
Example 2
The method comprises the steps of (1) introducing Dichlorosilane (DCS) and Silicon Tetrachloride (STC) into an anti-disproportionation reactor for reaction at a reaction mass ratio of 1:3, a reaction temperature and a reaction pressure of 0.2Mpa and a reaction temperature of 45 ℃, and detecting process operation data at a flow rate of 5 t/h. Through data detection, the DCS conversion rate can reach more than 90%, so that the recycling of DCS is effectively solved, and the discharge component data of the anti-disproportionation reactor are shown in Table 2.
TABLE 2 data on the discharge components of the anti-disproportionation reactor
The invention provides a chlorosilane rectifying impurity-removing process and a system thought and a method in polysilicon production, and particularly the method and the method for realizing the technical scheme are numerous, the above is only a preferred embodiment of the invention, and it should be pointed out that a plurality of improvements and modifications can be made by those skilled in the art without departing from the principle of the invention, and the improvements and modifications are also considered as the protection scope of the invention. The components not explicitly described in this embodiment can be implemented by using the prior art.
Claims (12)
1. The chlorosilane rectifying and impurity-removing process in the production of polysilicon is characterized by comprising the following steps of:
introducing upstream raw material chlorosilane into a raw material adsorption tower to remove impurities;
the chlorsilane after impurity removal is sent to a rough separation tower, and the rough separation tower is provided with at least three outlets of a tower top extraction pipe of the rough separation tower, a tower bottom extraction pipe of the rough separation tower and a side extraction pipe of the middle line of the rough separation tower;
the materials extracted from the side extraction pipe in the coarse separation tower are sent into a light component removal tower and a heavy component removal tower, and the light component removal tower is at least provided with two outlets of an upper tower top extraction pipe and a lower tower bottom extraction pipe of the light component removal tower; the materials extracted from the extraction pipe at the lower tower kettle of the light component removing tower are sent into the heavy component removing tower; the heavy impurity is removed from the lower tower kettle of the heavy removal tower, and the qualified trichlorosilane product is produced from the upper tower top extraction pipe of the heavy removal tower;
the materials extracted from the top extraction pipe of the coarse separation tower, the extraction pipe of the bottom extraction pipe of the coarse separation tower, the upper top of the light component removal tower and the bottom extraction pipe of the heavy component removal tower are sent into the reverse disproportionation separation tower for component separation; the anti-disproportionation separation tower is configured to be provided with at least three outlets of an anti-disproportionation separation tower top extraction pipe, an anti-disproportionation separation tower kettle extraction pipe and a anti-disproportionation separation tower middle side extraction pipe, wherein the anti-disproportionation separation tower top extraction pipe and the anti-disproportionation separation tower kettle extraction pipe are used for feeding materials extracted from the anti-disproportionation separation tower kettle extraction pipe into an anti-disproportionation reactor for anti-disproportionation reaction, and then feeding the materials into the anti-disproportionation separation tower again;
and the materials extracted from the side extraction pipe in the separation tower after the reverse disproportionation and the upstream raw material chlorosilane are sent into the raw material adsorption tower again.
2. The process for rectifying and impurity-removing chlorosilane in polysilicon production according to claim 1, wherein the materials fed into the anti-disproportionation reactor are subjected to batching calculation before mixing, and silicon tetrachloride is fed from the outside to completely react dichlorosilane.
3. The chlorosilane rectifying and impurity-removing system in the production of polysilicon is characterized by comprising a raw material buffer tank (10), a coarse separation tower (30), a light removal tower, a heavy removal tower, a reverse disproportionation post-separation tower (100) and a reverse disproportionation reactor (120); the raw material buffer tank (10), the coarse separation tower (30), the light component removal tower and the heavy component removal tower are sequentially connected through pipelines;
the tower side of the rough separation tower (30) is connected to a light component removal tower through a pipeline, the lower tower kettle of the light component removal tower is connected to a heavy component removal tower through a pipeline, and the upper tower top of the heavy component removal tower is used for extracting qualified trichlorosilane products through a pipeline;
the top and the bottom of the coarse separation tower (30), the upper top of the light component removal tower and the lower bottom of the heavy component removal tower are respectively connected to the reverse disproportionation post-separation tower (100) together through a production pipeline; the top and the bottom of the separation tower (100) after the anti-disproportionation are respectively connected to an anti-disproportionation reactor (120) through a production pipeline; the side surface of the separation tower (100) is reconnected to the raw material buffer tank (10) through a extraction pipeline after the reverse disproportionation; the anti-disproportionation reactor (120) returns to the anti-disproportionation post-separation tower (100) through a extraction pipeline.
4. A chlorosilane rectifying and impurity removing system in the production of polysilicon according to claim 3, characterized in that a mixer (110) is arranged between the anti-disproportionation post-separation tower (100) and the anti-disproportionation reactor (120); the top and the bottom of the separation tower (100) after the anti-disproportionation are respectively connected to a mixer (110) through a extraction pipeline, and are mixed and then sent into an anti-disproportionation reactor (120).
5. The system for rectifying and impurity removing of chlorosilane in polysilicon production as claimed in claim 4, wherein a silicon tetrachloride feed pipe (1101) is further connected to the feed side of said mixer (110).
6. A chlorosilane rectifying and impurity removing system in the production of polysilicon as in claim 3, further comprising a reverse disproportionation post-separation column feed buffer tank (90); the feeding buffer tank (90) of the reverse disproportionation separation tower is arranged at the front end of the reverse disproportionation separation tower (100); the top and the bottom of the coarse separation tower (30), the upper top of the light component removal tower and the lower bottom of the heavy component removal tower are respectively connected to a feed buffer tank (90) of the separation tower after the reverse disproportionation together through a production pipeline, and then are sent to a separation tower (100) after the reverse disproportionation after the buffer tank is cached; the anti-disproportionation reactor (120) is connected to a feed buffer tank (90) of the anti-disproportionation post-separation tower through a production line.
7. The chlorosilane rectifying and impurity removing system in polysilicon production as claimed in claim 6, wherein a raw material adsorption tower (20) is arranged between the raw material buffer tank (10) and the rough separation tower (30); the front end of the feeding side of the feeding buffer tank (90) of the reverse disproportionation rear separation tower is provided with a recovery material adsorption tower (80); the top of the coarse separation tower (30), the tower kettle, the upper tower top of the light component removal tower and the lower tower kettle of the heavy component removal tower are respectively connected into a reclaimed material adsorption tower (80) together through a production pipeline.
8. The chlorosilane rectifying and impurity removing system in polysilicon production according to claim 3, wherein a crude separation tower top reflux pipe (301) is arranged at the top of the crude separation tower (30), and a condenser and a crude separation tower top extraction pipe (304) are arranged on the crude separation tower top reflux pipe (301); a coarse separation tower kettle return pipe (302) is arranged at the lower tower kettle of the coarse separation tower (30), and a reboiler and a coarse separation tower kettle extraction pipe (305) are arranged on the coarse separation tower kettle return pipe (302); the tower side of the coarse separation tower (30) is provided with a coarse separation tower middle side line extraction pipe (303), and the coarse separation tower middle side line extraction pipe (303) is connected to the light component removal tower.
9. A chlorosilane rectifying and impurity-removing system in polysilicon production according to claim 3, wherein said light component removing tower comprises a light component removing tower upper tower (40) and a light component removing tower lower tower (50) which are sequentially connected in series; a reflux pipe (401) at the top of the upper tower (40) of the light component removing tower is arranged at the top of the upper tower of the light component removing tower; a condenser and a light component removal tower top extraction pipe (403) are arranged on the light component removal tower top return pipe (401); the bottom of the upper light component removing tower (40) is connected to the lower light component removing tower (50) through a bottom extraction pipe (402) of the upper light component removing tower;
the top of the lower light component removing tower (50) is provided with a lower light component removing tower top gas phase pipe (501), and the lower light component removing tower top gas phase pipe (501) is reconnected to the upper light component removing tower (40); the bottom of the light component removing tower lower tower (50) is provided with a light component removing tower lower tower kettle reflux pipe (502), the light component removing tower lower tower kettle reflux pipe (502) is provided with a reboiler and a light component removing tower lower tower kettle extraction pipe (503), and the light component removing tower lower tower kettle extraction pipe (503) is connected to the heavy component removing tower.
10. The system for rectifying and removing impurities from chlorosilane in polysilicon production according to claim 3, wherein the weight removing tower comprises a lower weight removing tower (60) and an upper weight removing tower (70) which are sequentially connected in series; the top of the lower de-weight tower (60) is provided with a lower de-weight tower top gas phase pipe (601), and the lower de-weight tower top gas phase pipe (601) is connected to an upper de-weight tower (70); a reflux pipe (602) of the lower tower kettle of the weight removing tower is arranged at the bottom of the lower tower (60) of the weight removing tower, and a reboiler and a extraction pipe (603) of the lower tower kettle of the weight removing tower are arranged on the reflux pipe (602) of the lower tower kettle of the weight removing tower;
a top reflux pipe (701) of the top of the heavy removal tower is arranged at the top of the top tower (70) of the heavy removal tower, a condenser and a top extraction pipe (703) of the top of the heavy removal tower are arranged on the top reflux pipe (701) of the top of the heavy removal tower, and qualified trichlorosilane products are extracted through the top extraction pipe (703) of the top of the heavy removal tower; the bottom of the upper tower (70) of the weight removing tower is provided with a bottom extraction pipe (702) of the upper tower kettle of the weight removing tower, and the bottom extraction pipe (702) of the upper tower kettle of the weight removing tower is connected to the lower tower (60) of the weight removing tower again.
11. The chlorosilane rectifying and impurity removing system in polysilicon production as claimed in claim 4, wherein a back flow pipe (1001) at the top of the back disproportionation separation tower is arranged at the top of the back disproportionation separation tower (100), and a condenser and a recovery pipe (1004) at the top of the back disproportionation separation tower are arranged on the back flow pipe (1001) at the top of the back disproportionation separation tower; the lower tower kettle of the anti-disproportionation separation tower (100) is provided with an anti-disproportionation separation tower kettle reflux pipe (1002), and the anti-disproportionation separation tower kettle reflux pipe (1002) is provided with a reboiler and an anti-disproportionation separation tower kettle extraction pipe (1005); the side of the anti-disproportionation separation tower (100) is provided with a side line extraction pipe (1003) in the anti-disproportionation separation tower, and the side line extraction pipe (1003) in the anti-disproportionation separation tower is reconnected to the raw material buffer tank (10); the post-disproportionation separation tower top extraction pipe (1004) and the post-disproportionation separation tower bottom extraction pipe (1005) are connected to the mixer (110) together.
12. The system for rectifying and impurity removing chlorosilane in polysilicon production as claimed in claim 6, wherein a bottom of said anti-disproportionation reactor (120) is provided with an anti-disproportionation reactor extraction pipe (1201), and is reconnected to a feed buffer tank (90) of a separation column after anti-disproportionation through the anti-disproportionation reactor extraction pipe (1201).
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