WO2020103799A1 - Dispositif et méthode d'élimination du méthyldichlorosilane du trichlorosilane par distillation réactive - Google Patents

Dispositif et méthode d'élimination du méthyldichlorosilane du trichlorosilane par distillation réactive

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Publication number
WO2020103799A1
WO2020103799A1 PCT/CN2019/119208 CN2019119208W WO2020103799A1 WO 2020103799 A1 WO2020103799 A1 WO 2020103799A1 CN 2019119208 W CN2019119208 W CN 2019119208W WO 2020103799 A1 WO2020103799 A1 WO 2020103799A1
Authority
WO
WIPO (PCT)
Prior art keywords
methyldichlorosilane
silicon tetrachloride
trichlorosilane
reaction
pretreatment device
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.)
Ceased
Application number
PCT/CN2019/119208
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English (en)
Chinese (zh)
Inventor
王红星
陈锦溢
华超
刘洋
李飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin University of Science and Technology
Original Assignee
Tianjin University of Science and Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tianjin University of Science and Technology filed Critical Tianjin University of Science and Technology
Publication of WO2020103799A1 publication Critical patent/WO2020103799A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • 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

Definitions

  • the invention relates to the technical field of reactive distillation, in particular to a method for removing methyldichlorosilane in trichlorosilane by reactive distillation using a chlorine atom redistribution reaction in the production process of polycrystalline silicon.
  • Carbon is one of the main impurities of semiconductor materials, which seriously affects the electrical properties of products and reduces the breakdown voltage of silicon devices.
  • carbon and oxygen work together to complicate the impact of impurities on the performance of materials and devices, resulting in a shortened service life.
  • high concentration of carbon in polysilicon will promote the formation of oxygen precipitates, which will induce dislocations, stacking faults, etc. Secondary defects, these defects will increase the silicon device leakage current, reducing the yield.
  • Polysilicon as a raw material for semiconductors if its carbon content exceeds the standard, it cannot be removed in the subsequent processing process, so the carbon content needs to be strictly controlled in the production of polysilicon.
  • adsorption technology is used to remove methyldichlorosilane in trichlorosilane.
  • This technology can reduce the content of methyldichlorosilane to less than 0.1 ppmw, and has a good removal effect. But limited by the adsorption capacity of the adsorbent, it is mainly used to remove trace impurities.
  • the use of adsorption technology will make the adsorbent very easy to adsorb and saturate, the use period will become shorter, and replacement and regeneration will produce a lot of work. Therefore, how to effectively dispose of materials with high content of methyldichlorosilane in trichlorosilane is a very urgent problem to be solved.
  • the present invention proposes a process for removing methyldichlorosilane in trichlorosilane by reactive distillation.
  • the silicon tetrachloride and methyldichlorosilane after pretreatment are respectively carried out in a reactive distillation tower Chlorine atom redistribution reaction, the reaction product trichlorosilane is recovered from the top of the tower, and the excess silicon tetrachloride and methyltrichlorosilane recovered from the tower kettle are sent to the silicon tetrachloride recycling device.
  • the invention provides a device and a method for removing methyldichlorosilane in trichlorosilane by reactive rectification.
  • the multi-stage rectification device discharges trichlorosilane containing high concentration of methyldichlorosilane as a raw material, and uses reactive rectification Technology, after pretreatment, rectification of chlorine atom redistribution reaction, and separation of silicon tetrachloride, methyldichlorosilane is converted into easily removable methyltrichlorosilane, and trichlorosilane is generated at the same time.
  • the chlorine atom redistribution reaction involved in the present invention is:
  • the raw materials of trichlorosilane containing methyldichlorosilane and silicon tetrachloride without silicon powder are respectively pretreated and sent to the rectification tower of chlorine atom redistribution reaction to carry out the above-mentioned chlorine atom redistribution reaction and use
  • the reaction product trichlorosilane is recovered from the top of the tower, and the excess silicon tetrachloride and reaction product methyltrichlorosilane recovered from the tower kettle are sent to the silicon tetrachloride recycling device.
  • the device for reactive distillation of the present invention to remove methyldichlorosilane in trichlorosilane is a device for reactive distillation of the present invention to remove methyldichlorosilane in trichlorosilane:
  • the main equipment of the silicon tetrachloride pretreatment device (A) is an adsorption column, which is filled with a granular or sheet-shaped adsorbent, and the adsorbent includes modified activated carbon and resin.
  • the main equipment of the methyl dichlorosilane raw material pretreatment device (B) is an adsorption column, which is filled with a granular or sheet-shaped adsorbent, and the adsorbent includes modified activated carbon and resin.
  • the reaction section in the middle of the reaction rectification tower (C) is filled with structured catalyst, and the filling height of the structured catalyst is not less than 12m; the rectification section in the upper part of the tower and the stripping section in the lower part are respectively filled with metal high-efficiency structured packing and rectification
  • the number of theoretical plates in the section is not less than 10, and the number of theoretical plates in the stripping section is not less than 10.
  • the said structured catalyst is to fill the chlorine atom redistribution catalyst in the corrosion-resistant cloth strip which is divided into small cloth bags, and then stacked into a block structure filler in the manner of a layer of wire mesh and a layer of cloth strip.
  • the catalyst of this structure is packed in a reaction rectification tower, the redistribution catalyst serves as a catalytic reaction, and the cloth strip and wire mesh serve as a separation medium.
  • the silicon tetrachloride material after the silicon powder is removed is first sent to the silicon tetrachloride pretreatment device (A), and the impurities that are likely to cause catalyst poisoning are adsorbed and removed by the adsorption device, and then enters the top of the reaction section of the reaction rectification tower (C) .
  • the multi-stage rectification device discharges raw materials containing trichlorosilane with high concentration of methyldichlorosilane through the methyldichlorosilane raw material pretreatment device (B), which is also used to remove impurities that easily lead to catalyst poisoning.
  • the adsorbed materials enter The bottom of the reaction section of the reactive distillation column (C).
  • reaction rectification tower In the reaction rectification tower (C), the redistribution of chlorine atoms of silicon tetrachloride and methyldichlorosilane and the separation of the reaction products are simultaneously carried out.
  • the reaction product trichlorosilane is taken from the top of the tower and sent to trichlorosilane. Distillation device, excess silicon tetrachloride and reaction product methyltrichlorosilane are withdrawn from the tower kettle and sent to the silicon tetrachloride recycling device.
  • 1- silicon tetrachloride raw material 2-trichlorosilane containing methyldichlorosilane raw material; 3-trichlorosilane; 4-tetrachlorosilane and methyl trichlorosilane mixture.
  • the reaction section in the middle of the reaction rectification tower (C) is filled with structured catalyst, and the filling height of the structured catalyst is not less than 12m; the rectification section in the upper part of the tower and the stripping section in the lower part are respectively filled with metal high-efficiency structured packing and rectification
  • the number of theoretical plates in the section is not less than 10, and the number of theoretical plates in the stripping section is not less than 10.
  • the structured catalyst is to fill the chlorine atom redistribution catalyst in the cloth strips which are divided into small cloth bags which are resistant to corrosion, and then stacked into a block structure according to a layer of wire mesh and a layer of cloth strips.
  • the catalyst of this structure is packed in a reaction rectification tower, the redistribution catalyst serves as a catalytic reaction, and the cloth strip and wire mesh serve as a separation medium.
  • the calculation is based on the industrial application scale of the raw material with methyl dichlorosilane content of 5% in trichlorosilane and the processing capacity of 500kg / h.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un dispositif et une méthode pour éliminer le méthyldichlorosilane du trichlorosilane au moyen d'une distillation réactive, le dispositif étant composé d'un dispositif de prétraitement de tétrachlorure de silicium (A), d'un dispositif de prétraitement de matière première de trichlorosilane contenant du méthyldichlorosilane (B), et d'une colonne de distillation réactive (C). Du tétrachlorure de silicium prétraité et des matières premières de trichlorosilane contenant du méthyldichlorosilane subissent une réaction de redistribution d'atome de chlore dans la colonne de distillation réactive, et au moyen de l'action de séparation de distillation réactive, un produit de réaction de trichlorosilane est extrait de la partie supérieure de la colonne, et le tétrachlorure de silicium en excès et le méthyltrichlorosilane généré sont extraits d'une chaudière de colonne. Afin d'assurer la conversion complète du méthyldichlorosilane, une quantité excessive appropriée de tétrachlorure de silicium est utilisée. Le procédé est simple et le taux de conversion du méthyldichlorosilane est élevé.
PCT/CN2019/119208 2018-11-19 2019-11-18 Dispositif et méthode d'élimination du méthyldichlorosilane du trichlorosilane par distillation réactive Ceased WO2020103799A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201811381032.5A CN109179426A (zh) 2018-11-19 2018-11-19 一种反应精馏去除三氯氢硅中甲基二氯硅烷的装置和方法
CN201811381032.5 2018-11-19

Publications (1)

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WO2020103799A1 true WO2020103799A1 (fr) 2020-05-28

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CN (1) CN109179426A (fr)
WO (1) WO2020103799A1 (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109179426A (zh) * 2018-11-19 2019-01-11 天津科技大学 一种反应精馏去除三氯氢硅中甲基二氯硅烷的装置和方法
CN110078080B (zh) * 2019-04-26 2022-09-02 天津科技大学 一种结合渣浆处理与裂解反应的氯硅烷高沸物回收工艺
CN110980742A (zh) * 2019-12-31 2020-04-10 天津大学 一种去除氯硅烷中含碳杂质的反应精馏提纯方法及装置
US12391559B2 (en) * 2020-11-05 2025-08-19 Wacker Chemie Ag Process for removing an impurity from a chlorosilane mixture
CN114956092A (zh) * 2022-04-21 2022-08-30 新疆大全新能源股份有限公司 一种分离三氯氢硅中一甲基二氯硅烷杂质的方法
CN115490236B (zh) * 2022-09-20 2024-03-29 云南通威高纯晶硅有限公司 一种电子级多晶硅生产用三氯氢硅的制备方法
CN115650242A (zh) * 2022-11-21 2023-01-31 青海黄河上游水电开发有限责任公司新能源分公司 三氯氢硅除碳装置及三氯氢硅除碳方法
CN116407861A (zh) * 2023-03-16 2023-07-11 清电光伏科技有限公司 一种基于固定床的电子级多晶硅精馏除碳装置及方法
CN116730346A (zh) * 2023-06-15 2023-09-12 内蒙古鄂尔多斯多晶硅业有限公司 一种多晶硅中联合除碳杂质的方法
CN117899506A (zh) * 2023-09-11 2024-04-19 青海丽豪半导体材料有限公司 一种多晶硅精馏脱碳反应炉
CN117339230A (zh) * 2023-09-23 2024-01-05 青海丽豪半导体材料有限公司 多晶硅精馏产物的脱碳吸附系统及其应用方法

Citations (5)

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US20100266489A1 (en) * 2007-10-20 2010-10-21 Evonik Degussa Gmbh Removal of foreign metals from inorganic silanes
CN102791630A (zh) * 2010-03-10 2012-11-21 信越化学工业株式会社 三氯硅烷的制造方法
CN105073638A (zh) * 2013-02-13 2015-11-18 信越化学工业株式会社 三氯硅烷的制造方法
CN108516555A (zh) * 2018-07-10 2018-09-11 天津科技大学 一种电子级二氯二氢硅的制备方法及设备
CN109179426A (zh) * 2018-11-19 2019-01-11 天津科技大学 一种反应精馏去除三氯氢硅中甲基二氯硅烷的装置和方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100266489A1 (en) * 2007-10-20 2010-10-21 Evonik Degussa Gmbh Removal of foreign metals from inorganic silanes
CN102791630A (zh) * 2010-03-10 2012-11-21 信越化学工业株式会社 三氯硅烷的制造方法
CN105073638A (zh) * 2013-02-13 2015-11-18 信越化学工业株式会社 三氯硅烷的制造方法
CN108516555A (zh) * 2018-07-10 2018-09-11 天津科技大学 一种电子级二氯二氢硅的制备方法及设备
CN109179426A (zh) * 2018-11-19 2019-01-11 天津科技大学 一种反应精馏去除三氯氢硅中甲基二氯硅烷的装置和方法

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