EP2526055A1 - Procédé en "circuit fermé" pour la préparation de trichlorosilane à partir de silicium métallique - Google Patents

Procédé en "circuit fermé" pour la préparation de trichlorosilane à partir de silicium métallique

Info

Publication number
EP2526055A1
EP2526055A1 EP10788097A EP10788097A EP2526055A1 EP 2526055 A1 EP2526055 A1 EP 2526055A1 EP 10788097 A EP10788097 A EP 10788097A EP 10788097 A EP10788097 A EP 10788097A EP 2526055 A1 EP2526055 A1 EP 2526055A1
Authority
EP
European Patent Office
Prior art keywords
hydrogen
silicon tetrachloride
stream
heat exchanger
trichlorosilane
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.)
Withdrawn
Application number
EP10788097A
Other languages
German (de)
English (en)
Inventor
Yücel ÖNAL
Rainer Malzkorn
Ingo Pauli
Ingrid Lunt-Rieg
Guido Stochniol
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.)
Evonik Operations GmbH
Original Assignee
Evonik Degussa GmbH
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 Evonik Degussa GmbH filed Critical Evonik Degussa GmbH
Publication of EP2526055A1 publication Critical patent/EP2526055A1/fr
Withdrawn legal-status Critical Current

Links

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
    • 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
    • C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
    • C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
    • C01B33/10763—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane from silicon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • 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
    • C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
    • 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
    • C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
    • C01B33/10747—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of tetrachloride
    • C01B33/10752—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of tetrachloride from 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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
    • C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
    • 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
    • C01B33/10773—Halogenated silanes obtained by disproportionation and molecular rearrangement of halogenated silanes
    • 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
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Definitions

  • the present invention relates to a process for the production of trichlorosilane and silicon tetrachloride from metallurgical silicon. It is a multi-stage process, in a first step trichlorosilane and
  • Silicon tetrachloride is produced from metallurgical silicon and in a second step, the silicon tetrachloride to the final product trichlorosilane
  • the present invention further relates to a plant in which such processes can be performed integrated.
  • Trichlorosilane can z. B. can be used to produce high purity silicon. In this case, trichlorosilane is thermally decomposed to high-purity silicon.
  • Trichlorosilane in turn can be made of metallurgical silicon in one
  • the present invention is therefore based on the object to provide an optimized technical solution for the production of trichlorosilane from metallurgical silicon, which in view of the problems mentioned also the
  • the task is thus to network the product and heat flows within a multi-stage plant in such a way that the educts and energy quantities used there are used as efficiently as possible for the production of the end product trichlorosilane. This object is achieved by the partial and
  • the invention relates in particular to a process for the preparation of trichlorosilane from silicon tetrachloride by hydrodechlorination with hydrogen, wherein at least one educt stream containing silicon tetrachloride and at least one hydrogen-containing educt stream is passed into a hydrodechlorination reactor and wherein in the hydrodechlorination reactor the thermodynamic
  • Hydrodechlorination reactor is led out, characterized in that cooled by means of a heat exchanger, the product stream and preheated by the same heat exchanger guided silicon tetrachloride Eduktstrom and / or the hydrogen-containing Eduktstrom.
  • the product stream can be
  • the equilibrium reaction in the hydrodechlorination reactor is typically at 700 ° C to 1, 000 ° C, preferably 850 ° C to 950 ° C and at a pressure in the range between 1 and 10 bar, preferably between 3 and 8 bar, more preferably between 4 and 6 bar performed.
  • the cooled product stream leave the heat exchanger and in at least one
  • Downstream unit can be performed, in the subsystem of the Product stream silicon tetrachloride and / or trichlorosilane and / or hydrogen and / or HCl can be separated.
  • the at least one subsystem just described may also be an arrangement of several subsystems, in each of which one or more of the said products silicon tetrachloride, trichlorosilane, hydrogen and / or HCl can be separated and passed on as stream.
  • the "products" silicon tetrachloride and hydrogen can also be unreacted educts.
  • Silicon tetrachloride as a current in the silicon tetrachloride Eduktstrom out and / or that separated hydrogen can be passed as a stream in the hydrogen-containing Eduktstrom, each independently preferably upstream of the heat exchanger can be done. It is also contemplated that separated trichlorosilane may be withdrawn as the final product stream and / or that separated HCl may be supplied as a stream of hydrochlorination of silicon. It is particularly preferred that all four above-mentioned separated streams are passed accordingly and thus utilized.
  • the process is preferably a process for the production of trichlorosilane from metallurgical silicon, characterized
  • the at least one silicon tetrachloride-containing educt stream and the at least one hydrogen-containing educt stream originate from an upstream hydrochlorination process, the hydrochlorination process comprising the reaction of metallurgical silicon with HCl.
  • At least some of the HCl used in the preceding hydrochlorination process can originate from the HCl stream which was separated off in the partial unit downstream of the heat exchanger.
  • at least part of the coupled product hydrogen can be separated off in a condenser and at least silicon tetrachloride and trichlorosilane can be separated from the remaining product mixture in a distillation plant.
  • the hydrogen separated in the condenser and / or the silicon tetrachloride separated off in the distillation plant be passed into the hydrodechlorination reactor, more preferably the separated hydrogen via the at least one hydrogen-containing reactant stream and / or the separated silicon tetrachloride via the at least a silicon tetrachloride-containing reactant stream is fed into the Hydrodechlor mecanicsreaktor.
  • Hydrodechlorination reactor is typically carried out via a boiler room in which the Hydrodechlor michsreaktor is arranged.
  • the arrangement of boiler room and hydrodechlorination reactor may look like one or more
  • Reactor tubes are arranged in the heating chamber, wherein the heating chamber is preferably heated by an electrical resistance heater or wherein the heating chamber is a combustion chamber, which is operated with fuel gas and combustion air.
  • the method according to the invention can preferably be extended such that the flue gas flowing out of the combustion chamber is connected downstream
  • Recuperator is used to preheat the combustion air.
  • the flue gas flowing out of the recuperator can additionally be used to generate steam.
  • Heat exchangers are guided, wherein the heat exchanger
  • the ceramic material for the heat exchanger elements is preferably selected from Al 2 O 3, AlN, Si 3 N 4 , SiCN or SiC, more preferably selected from Si-infiltrated SiC, isostatically pressed SiC, hot isostatically pressed SiC or non-pressure sintered SiC (SSiC).
  • the silicon tetrachloride-containing educt stream and the hydrogen-containing educt stream can also be conducted as a common stream through the heat exchanger.
  • the pressure differences in the heat exchanger between the different streams should not be more than 10 bar, preferably not more than 5 bar, more preferably not more than 1 bar, particularly preferably not more than 0.2 bar, measured at the inputs and outputs of the product gas. and reactant gas streams.
  • Hydrodechlorierungsreaktors are, preferably the pressures of the
  • Hydrodechlorination reactor should be the same.
  • the pressure at the outlet of the hydrodechlorination reactor is typically in the range between 1 and 10 bar, preferably in the range between 4 and 6 bar.
  • the heat exchanger is preferably a shell-and-tube heat exchanger.
  • the invention is also a plant for the implementation of
  • Silicon tetrachloride with hydrogen to form trichlorosilane comprising:
  • a heat exchanger which is preferably a shell-and-tube heat exchanger, through which the product gas line and at least one silicon tetrachloride line and / or the at least one hydrogen line are guided so that a heat transfer from the product gas line into the at least one
  • Silicon tetrachloride line and / or the at least one hydrogen line is possible, wherein optionally the heat exchanger may comprise heat exchanger elements made of ceramic material;
  • Silicon tetrachloride trichlorosilane, hydrogen and HCl
  • Silicon tetrachloride line can lead, preferably upstream of the heat exchanger
  • End product removal can be supplied;
  • Hydrochlorination of silicon can be supplied.
  • the plant according to the invention described above can be expanded such that the plant is a plant for the production of trichlorosilane from metallurgical silicon, characterized in that the plant additionally comprises:
  • a capacitor for separating at least a portion of the coupling product hydrogen, which originates from the reaction in the Hydrochlor michsstrom, said hydrogen via the hydrogen line in the Hydrodechlorierungsreaktor or the arrangement of one or more reactor tubes is performed;
  • Silicon tetrachloride line in the Hydrodechlor mecanicsreaktor or in the arrangement of one or more reactor tubes can be performed;
  • recuperator for preheating the for the combustion chamber
  • FIG. 1 shows, by way of example and schematically, a plant according to the invention for the production of toluene silane from metallurgical silicon, including a subplant for the hydrochlorination of metallurgical silicon, including important material streams.
  • FIG. 2 schematically shows a plant variant according to the invention comprising two distillation lines including important material streams, typically particularly suitable for the hydrochlorination of silicon in the fluidized-bed reactor.
  • FIG. 3 schematically shows a plant variant according to the invention comprising two distillation lines including important material streams, typically particularly suitable for the hydrochlorination of silicon in the fixed bed reactor.
  • FIG. 4 schematically shows a plant variant according to the invention comprising a distillation line including important material streams, typically particularly suitable for the hydrochlorination of silicon in the fluidized-bed reactor.
  • FIG. 5 schematically shows a plant variant according to the invention comprising a distillation line including important material streams, typically particularly suitable in the hydrochlorination of silicon in the fixed bed reactor.
  • the plant according to the invention shown in FIG. 1 comprises one in one
  • Combustion chamber 15 arranged Hydrodechlor michsreaktor 3, a line 1 for silicon tetrachloride-containing gas and a line 2 for hydrogen-containing gas, both of which lead into the Hydrodechlor effetsreaktor 3, one of the
  • the plant further comprises a unit 7 for separating silicon tetrachloride 8, of Tnchlorsilan 9, of hydrogen 10 and HCl 11.
  • the separated silicon tetrachloride is passed through line 8 in the silicon tetrachloride line 1, the separated Tnchlorsilan through the line 9 a Supplied end product removal, the separated hydrogen passed through line 10 in the hydrogen line 2 and fed the separated HCl through line 11 to a plant 12 for the hydrochlorination of silicon.
  • the system also includes a
  • Hydrodechlorination reactor 3 is performed. Shown is also a distillation unit 14 for separating silicon tetrachloride 1 and Tnchlorsilan (TCS) and
  • the plant also comprises a recuperator 16, which preheats the combustion air 19 provided for the combustion chamber 15 with the flue gas 20 flowing out of the combustion chamber 15, and a plant 17 for generating steam with the aid of the flue gas 20 flowing out of the recuperator 16.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Heat-Exchange Devices With Radiators And Conduit Assemblies (AREA)

Abstract

La présente invention concerne un procédé à plusieurs étapes pour la préparation de trichlorosilane et de tétrachlorure de silicium à partir de silicium métallique, où dans une première étape du trichlorosilane et du tétrachlorure de silicium sont préparés à partir de silicium métallique et dans une deuxième étape le tétrachlorure de silicium est transformé vers le produit final du trichlorosilane. La présente invention concerne en outre une installation, dans laquelle de tels procédés peuvent être réalisés de façon intégrée.
EP10788097A 2010-01-18 2010-12-16 Procédé en "circuit fermé" pour la préparation de trichlorosilane à partir de silicium métallique Withdrawn EP2526055A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102010000981A DE102010000981A1 (de) 2010-01-18 2010-01-18 Closed loop-Verfahren zur Herstellung von Trichlorsilan aus metallurgischem Silicium
PCT/EP2010/069944 WO2011085902A1 (fr) 2010-01-18 2010-12-16 Procédé en "circuit fermé" pour la préparation de trichlorosilane à partir de silicium métallique

Publications (1)

Publication Number Publication Date
EP2526055A1 true EP2526055A1 (fr) 2012-11-28

Family

ID=43608103

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10788097A Withdrawn EP2526055A1 (fr) 2010-01-18 2010-12-16 Procédé en "circuit fermé" pour la préparation de trichlorosilane à partir de silicium métallique

Country Status (9)

Country Link
US (1) US20130095026A1 (fr)
EP (1) EP2526055A1 (fr)
JP (1) JP2013517210A (fr)
KR (1) KR20120127414A (fr)
CN (1) CN102753477A (fr)
CA (1) CA2786422A1 (fr)
DE (1) DE102010000981A1 (fr)
TW (1) TW201139275A (fr)
WO (1) WO2011085902A1 (fr)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2135844A1 (fr) 2008-06-17 2009-12-23 Evonik Degussa GmbH Procédé de fabrication d'hydridosilanes plus élevés
DE102008002537A1 (de) * 2008-06-19 2009-12-24 Evonik Degussa Gmbh Verfahren zur Entfernung von Bor enthaltenden Verunreinigungen aus Halogensilanen sowie Anlage zur Durchführung des Verfahrens
DE102008043422B3 (de) 2008-11-03 2010-01-07 Evonik Degussa Gmbh Verfahren zur Aufreinigung niedermolekularer Hydridosilane
DE102009048087A1 (de) 2009-10-02 2011-04-07 Evonik Degussa Gmbh Verfahren zur Herstellung höherer Hydridosilane
DE102010000980A1 (de) * 2010-01-18 2011-07-21 Evonik Degussa GmbH, 45128 Katalytische Systeme zur kontinuierlichen Umsetzung von Siliciumtetrachlorid zu Trichlorsilan
DE102010039267A1 (de) * 2010-08-12 2012-02-16 Evonik Degussa Gmbh Verwendung eines Reaktors mit integriertem Wärmetauscher in einem Verfahren zur Hydrodechlorierung von Siliziumtetrachlorid
EP2630081B1 (fr) * 2010-10-22 2016-04-20 MEMC Electronic Materials, Inc. Production de silicium polycristallin dans des procédés et des systèmes à boucle fermée
US8449848B2 (en) 2010-10-22 2013-05-28 Memc Electronic Materials, Inc. Production of polycrystalline silicon in substantially closed-loop systems
US20120100061A1 (en) 2010-10-22 2012-04-26 Memc Electronic Materials, Inc. Production of Polycrystalline Silicon in Substantially Closed-loop Processes
DE102011002749A1 (de) 2011-01-17 2012-07-19 Wacker Chemie Ag Verfahren und Vorrichtung zur Konvertierung von Siliciumtetrachlorid in Trichlorsilan

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Also Published As

Publication number Publication date
WO2011085902A1 (fr) 2011-07-21
US20130095026A1 (en) 2013-04-18
CA2786422A1 (fr) 2011-07-21
CN102753477A (zh) 2012-10-24
JP2013517210A (ja) 2013-05-16
TW201139275A (en) 2011-11-16
DE102010000981A1 (de) 2011-07-21
KR20120127414A (ko) 2012-11-21

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