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WO2025015627A1 - Appareil et procédé de production combinée de méthode à lit fluidisé et méthode de siemens améliorée - Google Patents

Appareil et procédé de production combinée de méthode à lit fluidisé et méthode de siemens améliorée Download PDF

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Publication number
WO2025015627A1
WO2025015627A1 PCT/CN2023/109153 CN2023109153W WO2025015627A1 WO 2025015627 A1 WO2025015627 A1 WO 2025015627A1 CN 2023109153 W CN2023109153 W CN 2023109153W WO 2025015627 A1 WO2025015627 A1 WO 2025015627A1
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Prior art keywords
fluidized bed
tcs
disproportionation
improved siemens
hydrochlorination
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Pending
Application number
PCT/CN2023/109153
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English (en)
Chinese (zh)
Inventor
兰天石
朱共山
蒋立民
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Jiangsu Zhongneng Polysilicon Technology Development Co Ltd
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Jiangsu Zhongneng Polysilicon Technology Development Co Ltd
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Publication of WO2025015627A1 publication Critical patent/WO2025015627A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • 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
    • C01B33/029—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane
    • 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
    • C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
    • 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
    • C01B33/04—Hydrides of silicon
    • C01B33/043—Monosilane
    • 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
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • 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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/10778—Purification
    • C01B33/10784—Purification by adsorption
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
    • C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases

Definitions

  • the present invention belongs to the field of new energy material preparation, and specifically relates to a combined production process and device of an improved Siemens method and a fluidized bed method.
  • Polysilicon is one of the main raw materials for solar photovoltaic power generation.
  • the mainstream technologies for polysilicon production are the modified Siemens method using trichlorosilane as raw material and the fluidized bed method using silane as raw material.
  • the purity of the raw material trichlorosilane needs to be controlled to produce 99.9999%-99.9999999% high-purity polysilicon that meets the needs of photovoltaic power generation, so as to grow polysilicon rods that meet the requirements.
  • the characteristic of the fluidized bed method is that in a fluidized bed reactor (FBR), small-size granular polysilicon is used as a deposition carrier (seed), the reaction temperature is 500-1200°C, and the reaction medium is silane or chlorosilane and hydrogen, which drives the seed to float and tumble in the reaction medium gas.
  • the raw material undergoes thermal decomposition reaction or reduction reaction on the surface of the seed to generate elemental silicon, and the generated elemental silicon is deposited on the surface of the granular silicon seed crystal.
  • the particle size of the granular silicon seed crystal gradually increases until it reaches the specified size, and is finally extracted in the form of millimeter-level granular polysilicon.
  • Waste gas is mainly generated in silane production and separation, silicon tetrachloride cold hydrogenation, silane purification and other sections.
  • the production process waste gas mainly contains chlorosilane, silane, SiCl 4 , HCl, H 2 , N 2 , etc.
  • Granular silicon and polysilicon photovoltaic manufacturing are the core raw materials, and are accelerators to help achieve the "dual carbon" goal.
  • electricity energy consumption is one of the important costs of high-purity crystalline silicon and silicon wafer pulling manufacturing.
  • the comprehensive power consumption in the polysilicon production process accounts for more than 35% of the manufacturing cost.
  • the existing technology has not yet disclosed a technology that combines the two processes and devices of the modified Siemens method and the FBR fluidized bed method to produce electronic-grade polysilicon and granular silicon, and significantly reduces energy consumption through material and heat circulation.
  • the technical problem to be solved by the present invention is to overcome the defects of the prior art and provide a granular silicon production method and system that combines an improved Siemens method and a fluidized bed method, wherein the process can recycle reaction by-products and improve the utilization rate of raw materials.
  • TCS refining and purification The TCS prepared in step (1) is purified by adsorption and distillation to remove impurities;
  • TCS reduction reaction The TCS (SiHCl 3 ) prepared in step (2) is introduced into a modified Siemens reduction furnace.
  • the disproportionation reaction produces silane SiH 4 ;
  • step (6) The silane prepared in step (5) and the hydrogen recovered in step (4) are introduced into the FBR fluidized bed reactor as raw gas to generate product granular silicon by heterogeneous deposition.
  • the STC and DCS purified by the TCS refining and purification device in step (2) can be circulated to the hydrochlorination fluidized bed and the disproportionation device respectively.
  • the hydrogen purified in step (4) is recycled to the hydrochlorination reactor and/or the fluidized bed reactor for recycling.
  • the resulting hydrogen is recycled to the hydrochlorination reactor for the production of trichlorosilane.
  • DCS and TCS can be used for the disproportionation reaction in step (5) to produce silane.
  • the reduction tail gas in step (3) can be recycled to the hydrochlorination reactor after recovery and purification of silicon tetrachloride.
  • the steam produced as a by-product of the reduction furnace in step (3) is circulated to the disproportionation reaction device in step (5) and used for heating the silane gas production device.
  • the steam produced as a byproduct in the FBR fluidized bed reactor in step (6) is circulated to step (1)
  • the hydrochlorination unit is used for heating.
  • the raw material for the disproportionation reaction in step (5) can also be TCS (SiHCl 3 ) prepared in step (1);
  • the disproportionation reaction in step (5) prepares silane, which can be compressed to obtain high-pressure silane gas for sale.
  • step (4) the tail gas (including silicon tetrachloride, unreacted trichlorosilane, dichlorosilane and high molecular weight silane polymer, etc.) is reduced.
  • a certain proportion of dichlorosilane is configured in trichlorosilane and hydrogen as a raw material, which is beneficial to improving the yield of silane gas in the disproportionation device.
  • the present invention also relates to a combined production device of improved Siemens process and fluidized bed process, the device comprising a hydrochlorination fluidized bed, a TCS refining and purification device, an improved Siemens reduction furnace, a reduction tail gas recovery and purification device, a disproportionation device, an FBR reactor, and a gas-solid separation device;
  • the discharge of the hydrochlorination fluidized bed first enters the TCS refining and purification device for purification, and the purified high-purity TCS enters the improved Siemens reduction furnace to participate in the preparation of polysilicon; the reduction tail gas generated by the improved Siemens reduction furnace is separated and purified by the reduction tail gas recovery and purification device, and TCS and DCS enter the disproportionation device to react and produce SiH4 ; the SiH4 enters the FBR reactor to generate product granular silicon.
  • the reduction tail gas generated by the improved Siemens reduction furnace is separated and purified by the reduction tail gas recovery and purification device, and then H2 is circulated to the FBR reactor and/or the hydrochlorination fluidized bed, and the STC is circulated to the hydrochlorination fluidized bed.
  • STC and DCS purified by the TCS refining and purification device can be circulated to the hydrochlorination fluidized bed and the disproportionation device respectively.
  • the tail gas of the FBR reactor passes through a gas-solid separation device to separate silicon powder and H 2 , and the H 2 can be recycled.
  • the disproportionation device is connected to the feed port of the hydrochlorination fluidized bed, so as to circulate the STC produced as a by-product in the disproportionation device to the hydrochlorination fluidized bed for reaction.
  • the high-purity TCS purified by the TCS refining and purification device can also be directly introduced into the disproportionation device for reaction.
  • the disproportionation device is preferably a reactive disproportionation distillation tower to achieve coupling of disproportionation and distillation.
  • the gas-solid separation device is a cyclone separator or a membrane separation device
  • the membrane is a ceramic membrane
  • the improved Siemens process and fluidized bed process combined production device described in the present invention is also provided with a steam thermal energy circulation system.
  • the steam thermal energy circulation system can circulate the by-product steam of the improved Siemens reduction furnace to the disproportionation device for reaction heating, and circulate the by-product steam of the FBR reactor to the hydrochlorination fluidized bed for reaction heating.
  • the purity of polysilicon and granular silicon produced by the combined production process of the present invention can reach ⁇ 99.99999999999%.
  • the present invention provides a combined production process and device of an improved Siemens method and a fluidized bed method, which can recycle reaction byproducts and greatly improve the utilization rate of raw materials.
  • the device can also reduce the investment in production heating devices through heat circulation between various reaction components, and reduce carbon dioxide emissions and energy consumption.
  • the present invention can realize the use of a steam heat energy circulation system to convert the steam in the polysilicon production process into high-temperature steam through a waste heat recovery device, meet the steam energy consumption required by the downstream granular silicon production process device, and reduce the investment in the heating device required for the downstream granular silicon production process; it can also convert the steam in the downstream FBR reactor granular silicon production process into high-temperature steam through a waste heat recovery device, and circulate it to the hydrochlorination fluidized bed for reaction heating.
  • the use of the device and process described in the present invention can greatly reduce the reaction materials and energy consumption.
  • the improved Siemens method and fluidized bed method combined production process described in the present invention can greatly reduce the loss of other materials and heat, and recycle them, so as to greatly reduce the overall production cost; the production process described in the present invention can reduce 130,000 tons of carbon dioxide emissions at the polysilicon raw material end for 1GW components, and the industrial chain can reduce carbon dioxide emissions by 47.7%.
  • FIG. 1 is a flow chart of a joint production process of polysilicon and granular silicon.
  • Embodiment 1 is a diagrammatic representation of Embodiment 1:
  • a combined production device of improved Siemens process and fluidized bed process comprising a hydrochlorination fluidized bed, a TCS refining and purification device, an improved Siemens reduction furnace, a reduction tail gas recovery and purification device, a disproportionation device, an FBR reactor, and a gas-solid separation device; the discharge of the hydrochlorination fluidized bed first enters the TCS refining and purification device for purification, and the purified high-purity TCS enters the improved Siemens reduction furnace to participate in the preparation of polysilicon; the reduction tail gas generated by the improved Siemens reduction furnace is subjected to a reduction reaction; After separation and purification by the tail gas recovery and purification device, TCS and DCS enter the disproportionation device to react and produce SiH4 ; the SiH4 enters the FBR reactor to generate product granular silicon.
  • H2 is circulated to the FBR reactor and/or the hydrochlorination fluidized bed
  • STC is circulated to the hydrochlorination fluidized bed
  • the STC and DCS purified by the TCS refining and purification device can be circulated to the hydrochlorination fluidized bed and the disproportionation device respectively.
  • the tail gas of the FBR reactor passes through the gas-solid separation device to separate silicon powder and H2 , and the H2 can be recycled.
  • the disproportionation device is connected to the feed port of the hydrochlorination fluidized bed to circulate the by-product STC in the disproportionation device to the hydrochlorination fluidized bed for reaction.
  • the high-purity TCS purified by the TCS refining and purification device can also be directly introduced into the disproportionation device for reaction.
  • the disproportionation device is preferably a reaction disproportionation distillation tower to achieve the coupling of disproportionation and distillation.
  • the improved Siemens process and fluidized bed process combined production device described in the present invention is also provided with a steam thermal energy circulation system.
  • the steam thermal energy circulation system can circulate the by-product steam of the improved Siemens reduction furnace to the disproportionation device for reaction heating, and circulate the by-product steam of the FBR reactor to the hydrochlorination fluidized bed for reaction heating.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1:
  • FIG1 The process flow of a combined production process of an improved Siemens process and a fluidized bed process of the present invention is shown in FIG1 .
  • a combined production process of an improved Siemens process and a fluidized bed process comprising the following steps:
  • Step (1) Hydrochlorination: using silicon powder, hydrogen chloride, silicon tetrachloride and hydrogen as raw materials, reacting to prepare TCS (SiHCl 3 );
  • the TCS prepared in step (1) is purified by adsorption and distillation to remove impurities;
  • the STC and DCS purified by the TCS refining and purification device can be circulated to the hydrochlorination fluidized bed and the disproportionation device respectively.
  • Step (4) recovering and purifying the reduction tail gas in the production process of the improved Siemens reduction furnace to recover DCS (SiH 2 Cl 2 ) and TCS, STC, HCl, and H 2 ; recovering the purified hydrogen to the hydrochlorination reactor or/and the fluidized bed reactor for recycling;
  • Step (5) passing the DCS (SiH 2 Cl 2 )/TCS recovered from the Siemens process in step (4) into a disproportionation device for disproportionation reaction to obtain silane SiH 4 ;
  • Step (6) The silane prepared in step (5) and the hydrogen recovered in step (4) are introduced into the FBR fluidized bed reactor as raw gas to generate product granular silicon by heterogeneous deposition. After the silicon powder is removed from the tail gas of the FBR fluidized bed reactor by a gas-solid separation device such as a cyclone, the obtained hydrogen is recovered to the hydrochlorination reactor for the production of trichlorosilane.
  • a gas-solid separation device such as a cyclone
  • the steam produced as a byproduct of the reduction furnace in step (3) is circulated to the disproportionation reaction device in step (5) and used for heating the silane gas production device.
  • the steam produced as a byproduct of the FBR fluidized bed reactor in step (6) is circulated to the hydrochlorination device in step (1) for heating.
  • the power consumption of fluidized bed granular silicon deposition using this method is less than 3kWh/kg; the comprehensive power consumption is less than 15kWh/kg; the purity of polycrystalline silicon and granular silicon produced by the combined production process of the present invention can reach ⁇ 99.99999999999%, and the total metal impurity content is less than 1ppbw.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un appareil et un procédé de production combinée de méthode à lit fluidisé et méthode de Siemens améliorée. Selon le procédé, des sous-produits de réaction peuvent être recyclés, de telle sorte que le taux d'utilisation de matières premières peut être considérablement augmenté. Au moyen d'un système de circulation d'énergie thermique à la vapeur, de la vapeur dans un procédé de production de silicium polycristallin peut générer de la vapeur à haute température à travers un appareil de récupération de chaleur perdue, répondant à la consommation d'énergie de vapeur requise par un appareil dans un procédé de production de silicium granulaire en aval, et réduisant l'investissement dans l'appareil d'alimentation en chaleur requis par le procédé de production de silicium granulaire en aval ; de la vapeur dans le procédé de production de silicium granulaire d'un réacteur à lit fluidisé en aval (FBR) peut également générer de la vapeur à haute température à travers l'appareil de récupération de chaleur perdue, et la vapeur à haute température circule dans un lit fluidisé d'hydrochloration pour le chauffage de réaction. Par comparaison avec la construction indépendante et séparée des projets de productivité de silicium granulaire et de silicium polycristallin à la même échelle, l'utilisation de l'appareil et du procédé peut réduire considérablement les matériaux de réaction et la consommation d'énergie.
PCT/CN2023/109153 2023-07-20 2023-07-25 Appareil et procédé de production combinée de méthode à lit fluidisé et méthode de siemens améliorée Pending WO2025015627A1 (fr)

Applications Claiming Priority (2)

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CN202310892907.2 2023-07-20
CN202310892907.2A CN116924410A (zh) 2023-07-20 2023-07-20 一种改良西门子法、流化床法联合生产工艺及装置

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5673617A (en) * 1979-11-17 1981-06-18 Osaka Titanium Seizo Kk Manufacture of trichlorosilane
CN101143723A (zh) * 2007-08-08 2008-03-19 徐州东南多晶硅材料研发有限公司 制备三氯氢硅和多晶硅的改进方法和装置
CN101487139A (zh) * 2008-01-14 2009-07-22 瓦克化学股份公司 沉积多晶硅的方法
CN102874817A (zh) * 2012-09-14 2013-01-16 浙江精功新材料技术有限公司 一种二氯二氢硅歧化制备硅烷的方法
CN108862281A (zh) * 2018-07-17 2018-11-23 亚洲硅业（青海）有限公司 一种棒状多晶硅和颗粒多晶硅的联合生产方法
CN114132933A (zh) * 2021-11-02 2022-03-04 江苏中能硅业科技发展有限公司 一种颗粒硅生产方法和系统
CN116216723A (zh) * 2023-03-16 2023-06-06 内蒙古鑫元硅材料科技有限公司 一种纳米硅和颗粒硅的联产工艺

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5673617A (en) * 1979-11-17 1981-06-18 Osaka Titanium Seizo Kk Manufacture of trichlorosilane
CN101143723A (zh) * 2007-08-08 2008-03-19 徐州东南多晶硅材料研发有限公司 制备三氯氢硅和多晶硅的改进方法和装置
WO2009018713A1 (fr) * 2007-08-08 2009-02-12 Xuzhou Southeast Polysilicon R & D Ltd Procédés et dispositifs améliorés servant à préparer trichloro-hydrosilicium et polysilicium
CN101487139A (zh) * 2008-01-14 2009-07-22 瓦克化学股份公司 沉积多晶硅的方法
CN102874817A (zh) * 2012-09-14 2013-01-16 浙江精功新材料技术有限公司 一种二氯二氢硅歧化制备硅烷的方法
CN108862281A (zh) * 2018-07-17 2018-11-23 亚洲硅业（青海）有限公司 一种棒状多晶硅和颗粒多晶硅的联合生产方法
CN114132933A (zh) * 2021-11-02 2022-03-04 江苏中能硅业科技发展有限公司 一种颗粒硅生产方法和系统
CN116216723A (zh) * 2023-03-16 2023-06-06 内蒙古鑫元硅材料科技有限公司 一种纳米硅和颗粒硅的联产工艺

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