WO2017100404A1 - Systèmes réacteurs comportant des équilibreurs de pression externes - Google Patents

Systèmes réacteurs comportant des équilibreurs de pression externes Download PDF

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Publication number
WO2017100404A1
WO2017100404A1 PCT/US2016/065526 US2016065526W WO2017100404A1 WO 2017100404 A1 WO2017100404 A1 WO 2017100404A1 US 2016065526 W US2016065526 W US 2016065526W WO 2017100404 A1 WO2017100404 A1 WO 2017100404A1
Authority
WO
WIPO (PCT)
Prior art keywords
expansion joint
chamber
set forth
pressure balancer
reactor
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/US2016/065526
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English (en)
Inventor
Lee Frederick CHUSAK
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.)
SunEdison Inc
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SunEdison Inc
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 SunEdison Inc filed Critical SunEdison Inc
Publication of WO2017100404A1 publication Critical patent/WO2017100404A1/fr
Anticipated expiration legal-status Critical
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/03Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • B01J3/046Pressure-balanced vessels
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/021Preparation
    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/021Preparation
    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/029Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/021Preparation
    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/03Preparation 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

Definitions

  • the field of the disclosure relates to reactor systems having an external pressure balancer to counter-balance the hydrostatic end force of one or more system chambers .
  • Polycrystalline silicon may be produced economically and at relatively large scale by pyrolysis of thermally decomposable silicon-containing compounds (e.g., silane, trichlorosilane , dichlorosilane or
  • Such polycrystalline silicon may be used for production of solar cells or may be further processed according to the so-called Czochralski method to produce electronic grade single crystal silicon.
  • the reactor system includes a reactor liner defining a reaction chamber therein for receiving reaction components.
  • An outer shell is around the reactor liner.
  • An annular chamber is formed between the reactor liner and the outer shell.
  • the system includes a seal plate for sealing the annular chamber and the reaction chamber.
  • the system includes a clamping assembly for securing the seal plate so that the components in the reaction chamber are separate from the annular chamber.
  • a pressure balancer is in fluid communication with at least one of the annular chamber and the reaction chamber.
  • the pressure balancer includes an inner expansion joint defining an inner chamber therein and an outer expansion joint around the inner expansion joint.
  • the inner expansion joint and outer expansion joint define an annular chamber between the inner expansion joint and the outer expansion joint.
  • Figure 1 is a perspective view of a reactor system having a pressure balancer
  • Figure 2 is a perspective cross-section view of the reactor system
  • Figure 3 is a perspective cross-section view of another embodiment of the reactor system having two pressure balancer expansion joints
  • Figure 4 is a perspective cross-section view of another embodiment of the reactor system having three pressure balancer expansion joints.
  • the reactor system 5 includes a reactor liner 17 (Fig. 2) that defines a reaction chamber 15 therein for receiving reaction components.
  • the liner 17 may include a number of separate sections joined by gaskets to seal the various sections.
  • An outer shell 20 surrounds the reaction liner 17 and an annular chamber 12 is formed between the reaction liner 17 and the outer shell 20.
  • a seal plate 11 or reactor “head” seals the reaction chamber 15 and the annular chamber 12 to separate the fluids in each chamber.
  • a clamping assembly 29 (Fig. 1) secures the seal plate 11 by applying a clamping force between the seal plate 11 and the liner 17 and outer shell 20.
  • the clamping assembly 29 generally resists the hydraulic end force from the reaction chamber 15 or annular chamber 12.
  • the clamping assembly 29 adds additional force to the liner 17 to create a seal between the seal plate 11 and the liner 17.
  • the hydraulic end force is balanced by one or more expansion joints discussed below.
  • the clamping assembly 29 is a number of powered cylinders (e.g., hydraulic or pneumatic cylinders) .
  • the cylinders 29 are attached to the seal plate 11 and a clamping ring 31 that extends from the outer shell 20.
  • the clamping assembly 29 includes a number of springs, weights, screw jacks or counterbalances to seal the annular chamber and the reaction chamber.
  • the reactor system 5 includes a pressure balancer 10 to counteract changes in the reaction chamber 15 pressure and/or annular chamber 12 pressure.
  • the balancer 10 is external to the reactor components (e.g., external to the reaction chamber and/or the shell) .
  • the pressure balancer 10 includes a balancer top head 8 and a bottom head 18.
  • An expansion joint 48 extends between the top head 8 and the bottom head 18.
  • the expansion joint 48 has a flexible construction to allow for its expansion and contraction.
  • expansion joint 48 (and additional expansion joints of other embodiments described below) is a bellows. Suitable bellows include formed bellows and edge welded bellows.
  • the expansion joints may alternatively be composed of a material that stretches such as rubber.
  • the expansion joint 48 defines an inner chamber 52 within the expansion joint 48.
  • the inner chamber 52 is in fluid communication with the reaction chamber 15 through piping conduit 57 that extends through an inner chamber outlet formed in the bottom head 18.
  • the pressure balancer 10 is rigidly attached to the seal plate 11 by supports 72. In other embodiments, the supports 72 are eliminated and the pressure balancer 10 is attached directly to the seal plate 11. In such embodiments, the bottom head 18 of the pressure balancer 10 may also be eliminated and the expansion joint 48 may be attached directly to the seal plate 11.
  • the seal plate 11 may include additional openings (not shown) and/or fittings for removing or adding the process gases in the reaction chamber 15 and/or annular chamber 12.
  • the pressure balancer head 8 is also fixed with respect to the outer shell 20 by rigidly attaching the head 8 to the clamping ring 31 by tie-rods 76.
  • the balancer head 8 may be fixed relative to the shell 20 by fixing both the shell 20 and the head 8 to external structures such as the building structure in which the reactor is located.
  • the reactor system 5 includes an outer shell expansion joint 81 to allow for differential expansion of at least one of the reaction liner 17 and the outer shell 20.
  • the expansion joint 48 may be sized to provide equal effective areas pushing up and down on the seal plate 11 for the reaction chamber 15.
  • the differential between the pressure of the reaction chamber 15 and the pressure of the annular chamber annular chamber 12 helps provide the clamping force between the seal plate 11 and the liner 17 and outer shell 20.
  • FIG. 3 Another embodiment of the pressure balancer 10 is shown in Figure 3.
  • the expansion joint 48 of the balancer 10 is an "outer" expansion joint and the balancer 10 also includes an inner expansion joint 40 that extends between the top head 8 and the bottom head 18.
  • the inner expansion joint 40 defines an inner chamber 52 within the expansion joint 40.
  • the inner chamber 52 is in fluid communication with the reaction chamber 15 through piping conduit 57 that extends through an inner chamber outlet formed in the bottom head 18.
  • the inner expansion joint 40 and outer expansion joint 48 form an annular chamber 54 (Fig. 3) .
  • the annular chamber 54 is in fluid communication with the annular chamber 12 formed between the reaction liner 17 and the outer shell 20 by piping conduit 59 that extends through an inner chamber outlet formed in the bottom head 18.
  • the chambers 52, 54 may be fluidly connected by use of additional conduits (not shown) .
  • the pressure balancer 10 is attached directly to the seal plate 11 and supports 72 are eliminated.
  • the bottom head 18 of the pressure balancer 10 may also be eliminated and the expansion joints 40, 48 may be attached directly to the seal plate 11.
  • the seal plate 11 of the balancer 10 of Figure 3 may include additional openings and fittings (not shown) .
  • the inner expansion joint 40 acts as the division between the reaction chamber 15 and the annular chamber 12 and should be designed for both internal and external pressure.
  • the inner expansion joint 40 may be sized to provide an equal effective areas pushing up and down on the seal plate 11 for the reaction chamber 15.
  • the outer expansion 48 acts as the outer boundary to the annular chamber 12 and should be designed for internal pressure (or external pressure as in vacuum applications)
  • the outer expansion joint 48 may be sized to provide equal effective areas pushing up and down on the seal plate 11 for the annular chamber 12. While the reactor system 5 may be generally described herein with reference to positive reaction chamber and/or annular chamber pressures, the reactor system 5 may also be used in vacuum pressure applications .
  • the pressure balancer 10 includes a core expansion joint 84 defining a core chamber 88.
  • a piping conduit 57 extends through the core chamber 88 and through the seal plate 11.
  • the piping conduit 57 is in fluid communication with the reaction chamber 15 or, as in other embodiments, the annular chamber 12.
  • the inner expansion joint 40 and core expansion joint 84 define the inner chamber 52.
  • the core expansion joint 84 should be designed for external pressure (or internal pressure as in vacuum applications).
  • the pressure balancer 10 is attached directly to the seal plate 11 and supports 72 are eliminated.
  • the seal plate 11 of the balancer of Figure 4 may include additional openings (not shown) and/or fittings for removing or adding the process gases in the reaction chamber 15 and/or annular chamber 12.
  • the reactor system 5 may be operated by reacting reactor fluids in the reaction chamber 15.
  • a second fluid may be present in the annular chamber 12 to prevent the reaction chamber from being contaminated.
  • the reaction fluid in the annular chamber 12 is generally inert to the reaction components within the reaction chamber 15.
  • the fluids in the reaction chamber 15 and annular chamber 12 are both gases .
  • the annular chamber 12 may be operated at a pressure greater than the reaction chamber 15 such as at least about 0.01 bar greater or at least about 0.05 bar, at least about 0.1 bar, at least about 0.5 bar, at least about 1 bar or at least about 2 bar greater (e.g., from about 0.1 bar to about 5 bar, from about 0.1 bar to about 2 bar or from about 0.1 bar to about 0.9 bar greater) .
  • the pressure in the annular chamber 12 is less than the pressure in the reaction chamber 15 such as at least about 0.01 bar less or at least about 0.05 bar, at least about 0.1 bar, at least about 0.5 bar, at least about 1 bar or at least about 2 bar less (e.g., from about 0.1 bar to about 5 bar, from about 0.1 bar to about 2 bar or from about 0.1 bar to about 0.9 bar less) .
  • the annular chamber 12 may include a heater (not shown) therein to heat the reactor components in the reaction chamber 15.
  • the reactor system 5 is used to produce polycrystalline silicon.
  • a silicon feed gas comprising a silicon-containing compound is introduced into the reaction chamber 15.
  • the silicon feed gas may be introduced with a carrier gas such as hydrogen, argon, helium, silicon tetrachloride or combinations thereof.
  • Silicon particles e.g., seed particles
  • the reaction chamber 15 may be maintained at a pressure of at least about -0.5 barg, at least about 0 barg, at least about 0.5 barg, at least about 1 barg, at least about 3 barg, at least about 5 barg or at least about 10 barg (e.g., from about -0.5 barg to about 25 barg, from about 3 barg to about 25 barg or from about 3 barg to about 10 barg) .
  • Incoming gases may be pre-heated to a temperature of at least about 200°C (e.g., from about 200°C to about 500°C of from about 200 °C to about 350 °C) .
  • the reactor chamber 15 may be maintained at a temperature of at least about 600°C (e.g., 600°C to about 900°C or from about 600°C to about 750 °C) by use of external heating means such as induction heating or use of resistive heating elements positioned in the annular chamber 12.
  • the gas velocity through the fluidized bed reactor 30 may be generally maintained at a velocity of from about 1 to about 8 times the minimum fluidization velocity necessary to fluidize the particles within the fluidized bed.
  • the mean diameter of the particulate polycrystalline silicon that is withdrawn from the reactor 30 may be at least about 600 ⁇ (e.g., from about 600 ⁇ to about 1500 ⁇ or from about 800 ⁇ to about 1200 ⁇ ) .
  • the mean diameter of the silicon seed particles introduced into the reactor may be less than about 600 ⁇ (e.g., from about 100 ⁇ to about 600 ⁇ ) .
  • Quench gases may be introduced into the reactor 30 (e.g., at a freeboard region of the reactor) to reduce the temperature of the effluent gas 39 before being discharged from the reactor to suppress formation of silicon dust.
  • Inert gas may be introduced into the annular chamber 15 and maintained at a pressure below or above the pressure of the process gases of the reaction chamber 15 as noted above to chemically isolate the reaction chamber.
  • the thermally decomposable gases may be directed to the core region of the reactor and carrier gas (e.g., hydrogen) may be directed to the peripheral portion of the reactor near the reactor walls to reduce the deposition of silicon on the walls of the reactor as disclosed in U.S. Pat. No. 8,906,313 and U.S. Pat. Pub. No. 2011/0158888, both of which are incorporated herein by reference for all relevant and consistent purposes.
  • the reactor may be operated in accordance with the reaction conditions disclosed in U.S. Patent Publication No. 2013/0084233, which is incorporated herein by reference for all relevant and consistent purposes.
  • U.S. Patent Publication No. 2013/0084233 which is incorporated herein by reference for all relevant and consistent purposes.
  • dichlorosilane is used as the thermally decomposable compound
  • the reactor may be operated in accordance with the reaction conditions disclosed in U.S. Patent
  • the reactor may be operated in accordance with the reaction conditions disclosed in U.S. Patent Publication No. 2012/0100059, which is incorporated herein by reference for all relevant and consistent purposes.
  • the pressure balancer 10 responds to changes in the pressure of the reaction chamber 15. As the pressure increases, the pressure in the inner chamber 52 (Fig. 2) within the expansion joint 48 increases causing the expansion joint to exert a higher pressure and increase the clamping force applied to the seal plate 11 and the liner 17.
  • the pressure balance 10 includes a two or more pressure balancers (Figs. 3 and 4) the pressure balancer 10 can respond to a change in pressure in the annular chamber 12 to exert a force on the shell 20.
  • the pressure balancer 10 may vary the clamping force of the seal plate 11 based on changes in the pressure in the reaction chamber 15 and/or annular chamber 12. This allows the clamping assembly 29 to be simplified (e.g., a passive system may be used) as the clamping force of the apparatus is a function of gasket pressure and expansion joint 81 expansion/contraction.
  • the pressure balancer 10 of Figures 3 and 4 operates in the event the reactor rupture disk (not shown) ruptures allowing the system to remain pressure balanced (i.e., a sudden decrease in reaction chamber 15 and/or annular chamber 12 pressure is counteracted by a sudden decrease in force applied by balancer 10) .
  • concentrations, temperatures or other physical or chemical properties or characteristics is meant to cover variations that may exist in the upper and/or lower limits of the ranges of the properties or characteristics, including, for example, variations resulting from rounding, measurement methodology or other statistical variation.
  • the articles "a”, “an”, “the” and “said” are intended to mean that there are one or more of the elements.
  • the terms “comprising,” “including,” “containing” and “having” are intended to be inclusive and mean that there may be additional elements other than the listed elements.
  • the use of terms indicating a particular orientation is for convenience of description and does not require any particular orientation of the item described .

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

L'invention concerne des systèmes réacteurs comportant un équilibreur de pression externe destiné à contrebalancer la force hydrostatique aux extrémités d'une ou de plusieurs chambres de système.
PCT/US2016/065526 2015-12-11 2016-12-08 Systèmes réacteurs comportant des équilibreurs de pression externes Ceased WO2017100404A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201562266377P 2015-12-11 2015-12-11
US62/266,377 2015-12-11

Publications (1)

Publication Number Publication Date
WO2017100404A1 true WO2017100404A1 (fr) 2017-06-15

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113351117A (zh) * 2021-08-11 2021-09-07 山东福尔特种设备有限公司 一种螺纹式快开高压釜盖自紧密封结构

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007094607A1 (fr) * 2006-02-14 2007-08-23 Korea Research Institute Of Chemical Technology Procédé de préparation de silicium polycristallin granulaire au moyen d'un réacteur à lit fluidisé
US20110117729A1 (en) * 2009-11-18 2011-05-19 Rec Silicon Inc Fluid bed reactor
US20110158888A1 (en) 2009-12-29 2011-06-30 Memc Electronic Materials, Inc. Methods for reducing the deposition of silicon on reactor walls using peripheral silicon tetrachloride
US20120100059A1 (en) 2010-10-22 2012-04-26 Memc Electronic Materials, Inc. Production of Polycrystalline Silicon By The Thermal Decomposition of Trichlorosilane In A Fluidized Bed Reactor
US20120164323A1 (en) 2010-12-23 2012-06-28 Memc Electronic Materials, Inc. Production of polycrystalline silicon by the thermal decomposition of dichlorosilane in a fluidized bed reactor
US20130084233A1 (en) 2011-09-30 2013-04-04 Memc Electronic Materials, Inc. Production of polycrystalline silicon by the thermal decomposition of silane in a fluidized bed reactor
US8906313B2 (en) 2008-06-30 2014-12-09 Sunedison, Inc. Fluidized bed reactor systems
WO2016183308A1 (fr) * 2015-05-12 2016-11-17 Sunedison, Inc. Ensemble de serrage pour un système de réacteur

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007094607A1 (fr) * 2006-02-14 2007-08-23 Korea Research Institute Of Chemical Technology Procédé de préparation de silicium polycristallin granulaire au moyen d'un réacteur à lit fluidisé
US8906313B2 (en) 2008-06-30 2014-12-09 Sunedison, Inc. Fluidized bed reactor systems
US20110117729A1 (en) * 2009-11-18 2011-05-19 Rec Silicon Inc Fluid bed reactor
US20110158888A1 (en) 2009-12-29 2011-06-30 Memc Electronic Materials, Inc. Methods for reducing the deposition of silicon on reactor walls using peripheral silicon tetrachloride
US20120100059A1 (en) 2010-10-22 2012-04-26 Memc Electronic Materials, Inc. Production of Polycrystalline Silicon By The Thermal Decomposition of Trichlorosilane In A Fluidized Bed Reactor
US20120164323A1 (en) 2010-12-23 2012-06-28 Memc Electronic Materials, Inc. Production of polycrystalline silicon by the thermal decomposition of dichlorosilane in a fluidized bed reactor
US20130084233A1 (en) 2011-09-30 2013-04-04 Memc Electronic Materials, Inc. Production of polycrystalline silicon by the thermal decomposition of silane in a fluidized bed reactor
WO2016183308A1 (fr) * 2015-05-12 2016-11-17 Sunedison, Inc. Ensemble de serrage pour un système de réacteur

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113351117A (zh) * 2021-08-11 2021-09-07 山东福尔特种设备有限公司 一种螺纹式快开高压釜盖自紧密封结构
CN113351117B (zh) * 2021-08-11 2021-10-22 山东福尔特种设备有限公司 一种螺纹式快开高压釜盖自紧密封结构

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