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WO2012017053A1 - Installation de production de monosilane - Google Patents

Installation de production de monosilane Download PDF

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Publication number
WO2012017053A1
WO2012017053A1 PCT/EP2011/063484 EP2011063484W WO2012017053A1 WO 2012017053 A1 WO2012017053 A1 WO 2012017053A1 EP 2011063484 W EP2011063484 W EP 2011063484W WO 2012017053 A1 WO2012017053 A1 WO 2012017053A1
Authority
WO
WIPO (PCT)
Prior art keywords
column
tubes
tube
segment
monosilane
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/EP2011/063484
Other languages
German (de)
English (en)
Inventor
Adolf Petrik
Christian Schmid
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.)
Schmid Silicon Technology GmbH
Original Assignee
Schmid Silicon Technology 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 Schmid Silicon Technology GmbH filed Critical Schmid Silicon Technology GmbH
Publication of WO2012017053A1 publication Critical patent/WO2012017053A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • 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
    • C01B33/10773—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

Definitions

  • the present invention relates to a plant for the preparation of monosilane (SiH 4 ) by catalytic disproportionation of trichlorosilane (SiHCIs) with a columnar reaction column with a feed for trichlorosilane, a sequence for accumulating silicon tetrachloride (SiCl 4 ) and a heating region, preferably at the lower end of the column, and a condenser through which monosilane produced can be removed from the column.
  • SiHCIs trichlorosilane
  • High purity silicon is typically produced in a multi-stage process starting from metallurgical silicon, which may have a relatively high level of impurities.
  • this can be converted, for example, into a trihalosilane, such as trichlorosilane (SiHCIs), which is subsequently thermally decomposed to give highly pure silicon.
  • SiHCIs trichlorosilane
  • Such a procedure is known for example from DE 29 19 086.
  • Monosilane can be obtained in particular by disproportionation of trichlorosilane.
  • the latter can in turn be produced, for example, by reacting metallurgical silicon with silicon tetrachloride and hydrogen.
  • catalysts can be used.
  • Basic catalysts have proved particularly suitable, for example the amine compounds and derivatives known from DE 25 07 864. These are preferably used in bonded form, as described for example in DE 33 1 1 650. Bound to solid supports - - dene catalysts are easily separable from liquid or gaseous reaction mixtures. In the case of amine compounds, an entry of contaminating amines into the silane / chlorosilane mixture can thus be avoided. Because of the associated advantage, in the technical disproportionation of trichlorosilane, only amine carriers immobilized or incorporated into crosslinked polymers are used today.
  • a plant according to the invention serves in accordance with the above. Purpose of the production of monosilane by catalytic disproportionation of trichlorosilane. Like many generic systems, it comprises a columnar reaction column with an inlet for trichlorosilane and a discharge of silicon tetrachloride. Furthermore, the plant comprises a heating area and a main condenser, can be removed from the column via the produced monosilane.
  • the reaction column has at least one segment which contains a catalytically active solid.
  • the at least one segment preferably comprises a tube or a tube bundle of two or more tubes, which are filled with the catalytically active solid.
  • this tube or tubes with the catalytically active solid form catalytic cells in which the disproportionation reaction takes place.
  • the principle of reactive distillation has already been mentioned at the beginning. Also in the reaction column of a plant according to the invention for the production of monosilane this principle is used. Thus, a reaction takes place in the one or more tubes with continuous discharge of the low boilers. These may then be transferred to a downstream reactive / distillative reaction zone (e.g., another catalytic cell).
  • the reaction column of a system according to the invention is usually oriented vertically.
  • the tube or tubes of the bundle are preferably arranged vertically and in particular parallel to one another within the column segment.
  • catalysis of chlorosilanes takes place in parallel in all tubes.
  • Tubes on a substantially cylindrical geometry can also have a polygonal cross section, for example a hexagonal cross section.
  • the tube bundle preferably comprises between 2 and 100 tubes, in particular between 5 and 50 tubes, which are each filled with the catalytically active solid.
  • the heating region can be integrated into the columnar reaction column, in particular at the lower end of the column.
  • the system according to the invention can also have an external sump heater.
  • the column segment comprises a heat exchange space through which the tube or the tubes of the tube bundle are guided.
  • a cavity can be formed, which is traversed by a heat exchange medium.
  • the segment may have an inlet and an outlet for the heat exchange medium.
  • the tube or tube bundle can be tempered so targeted to keep the catalytic solid inside in operation at certain suitable for the catalytic disproportionation temperatures.
  • the reaction column of a plant according to the invention preferably has a plurality of column segments which contain the mentioned catalytically active solid.
  • the system according to the invention preferably has a plurality of column segments with the mentioned tube or the tube bundle from the two or more tubes. These segments are particularly preferably arranged one above the other within the column. - -
  • Such superimposed segments of the reaction column correspond to a certain extent catalytic reactors, which are functionally connected in series.
  • the disproportionation of trichlorosilane can be carried out according to the principle of reactive distillation.
  • Both the segments and the tube bundles and tubes arranged therein each have identical dimensions and an identical construction in preferred embodiments.
  • the tube or tube bundles are preferably arranged within the reaction column or within the segments such that each tube in a higher-level segment is assigned a tube in an adjacent, lower-lying segment into which condensate can drip or drain out of the higher-lying tube.
  • the temperature preferably drops from bottom to top, so that a higher column segments is usually operated at a lower temperature than a lower arranged.
  • the lowest-lying segment in the reaction column accordingly usually has the highest operating temperature.
  • an intermediate capacitor may be arranged between the stacked column segments. This serves for the separation / restraint of low-volatility chlorosilanes and optionally relieves downstream condensers, in particular the main capacitor.
  • downstream main condenser is integrated in the top of the reaction column.
  • the segments as well as the mentioned capacitor units can be units which are firmly connected to one another - - Also around modular units, which are connected by detachable connections.
  • a system according to the invention is characterized in that the tube or tubes in the segments are each closed at their lower end with a grid and / or a net.
  • the mesh size of the grid and / or the network is expediently chosen so that the catalytically active solid contained in the tubes, which is preferably present in the form of particles, can not escape from the tubes in an uncontrolled manner.
  • the grids and / or the nets form a conical lower tube termination with a conical tip pointing downwards and a cone angle ⁇ 90 ° C, preferably between 30 ° C and 60 °.
  • This serves, in particular, for focusing condensate from the tube or tubes, which can drip off or flow away via the cone tip into a deeper-lying column segment, in particular into a corresponding tube arranged there.
  • the upper ends of the tube or tubes are preferably open.
  • the tube or tubes open at the top in preferably cylindrical cavities, which are bounded to the sides by the inner walls of the columnar reaction column.
  • the walls of the reaction column can be pierced in this area by closable maintenance openings, via which the tube or the two or more tubes of the tube bundle can be filled with catalyst.
  • catalytically active solid based on vinyl pyridine or a vinylpyridine derivative in the reaction column of a plant according to the invention.
  • a suitable catalytically active vinylpyridine-divinylbenzene copolymer is described, for example, in US 4,613,489. - -
  • At least one of the segments of the reaction column of a plant according to the invention contains a catalytically active solid based on styrene or a styrene derivative, in particular based on a styrene-divinylbenzene copolymer.
  • Suitable Ciopolymere can be obtained by various methods, each leading to formulas identical products (see Ullmann's Encyclopedia of Industrial Chemistry, 4th Edition, Volume 13, Weinheim 1997, page 301 -303).
  • a plant according to the invention has a reaction column in accordance with the above statements in particularly preferred embodiments,
  • the segment containing the catalytically active solid based on vinylpyridine or the vinylpyridine derivative is preferably arranged below the segment with the catalytically active solid based on styrene or the styrene derivative.
  • both a reaction and a continuous, distillative separation of low-boiling components ie in particular the monosilane-containing fraction
  • the low boilers can then be converted into downstream segments, so that usually the concentration of - -
  • Monosilane in a column increases towards the top.
  • the silane-containing product mixture is then fed to a condenser, the main condenser mentioned, which is usually operated so that either only monosilane or a monosilane-containing fraction with the lowest possible Shares in other volatile components can happen.
  • Chlorine-containing silanes should, if possible, be retained by the main condenser in the reaction column.
  • the main condenser is integrated in the top of the reaction column. In principle, however, it is also possible to use a separate condenser connected downstream of the column. The chlorosilanes separated in such a condenser can be returned to the reaction column via a recycle line.
  • the operating temperature of the main capacitor is preferably in the range between -20 ° C and -100 ° C.
  • a plant according to the invention characterized in that the diameter of the tube or all tubes of the tube bundle by a factor of 50 to 300 is greater than the mitllere grain size of the catalyst (preferably obtained from the sieve analysis, it corresponds to the at a 50% throughput associated grain diameter).
  • the latter preferably moves in the range between 1 mm and 6 mm.
  • the length of the tube (s) in the tubes contained in segments exceeds its diameter by a factor of 10 to 20.
  • a process for the preparation of monosilane (SiH 4 ) by catalytic disproportionation of trichlorosilane (SiHCIs) is also the subject of the present invention.
  • the method is characterized in that - - It is carried out in a plant, as described above, in particular using the described catalytically active solids.
  • FIG. 1 shows schematically the structure of a preferred embodiment of a system according to the invention (representation in longitudinal section).
  • the illustrated preferred embodiment of a plant according to the invention comprises the reaction column 101 with the feed 102 for Tnchlorsilan, the discharge 103 for silicon tetrachloride and the heating region 104, in which the Tnchlorsilan can be evaporated.
  • the heating area 104 Above the heating area 104, three segments 106, 107 and 108 are arranged, each of which has a tube bundle comprising a plurality of tubes (which each have identically formed tubes 109, 110 and 111). The latter are filled with a catalytically active solid.
  • Each of the column segments includes a heat exchange 112 (shown hatched) through which the tubes 109, 110 and 111 are routed.
  • heat exchange media can be conducted into these heat exchange spaces 112, so that it is possible to precisely determine the temperature at which the catalyzed reactions in the individual segments 106, 107 and 108 are to take place.
  • the tubes of the tube bundle are each closed with a net.
  • the nets taper downwards and form conical bottom tube ends.
  • the cone angle is less than 90 °.
  • the tubes 109, 110 and 111 can be filled via feed openings 118 in the reactor wall.
  • the main condenser 105 which is integrated as a modular segment in the reaction column 101.
  • the condenser coolant can be supplied.
  • Monosilane produced in the reaction column 101 can escape via the outlet 121.

Landscapes

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

Abstract

L'invention concerne une installation de production de monosilane (SiH4) par disproportionation catalytique de trichlorosilane (SiHCI3), comportant une colonne de réaction (101) de forme cylindrique comprenant une amenée (102) pour le trichlorosilane, une évacuation (103) pour le tétrachlorure de silicium (SiCI4) généré et une zone chauffante (104), de préférence à l'extrémité inférieure de la colonne, ainsi qu'un condenseur (105) par l'intermédiaire duquel le monosilane produit peut être évacué de la colonne (101), la colonne (101) comportant un segment (106; 107; 108) dans lequel est contenu un solide à action catalytique et le segment (106; 107; 108) de colonne comportant un tube ou un faisceau de tubes composés de deux ou de plus de deux tubes (109; 110; 111), lequel ou lesquels sont remplis du solide à action catalytique.
PCT/EP2011/063484 2010-08-06 2011-08-04 Installation de production de monosilane Ceased WO2012017053A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102010034469A DE102010034469A1 (de) 2010-08-06 2010-08-06 Anlage zur Herstellung von Monosilan
DE102010034469.9 2010-08-06

Publications (1)

Publication Number Publication Date
WO2012017053A1 true WO2012017053A1 (fr) 2012-02-09

Family

ID=44512854

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2011/063484 Ceased WO2012017053A1 (fr) 2010-08-06 2011-08-04 Installation de production de monosilane

Country Status (2)

Country Link
DE (1) DE102010034469A1 (fr)
WO (1) WO2012017053A1 (fr)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2507864A1 (de) 1974-02-25 1975-08-28 Union Carbide Corp Verfahren zur herstellung von silan
DE2919086A1 (de) 1978-08-18 1980-03-06 Schumacher Co J C Verfahren zur herstellung von polykristallinem silizium
DE3311650A1 (de) 1982-03-31 1983-10-13 Union Carbide Corp., 06817 Danbury, Conn. Verfahren zur herstellung von hoch reinem silan sowie hoch reinem polykristallinem und einkristallinem silicium fuer solarzellen und halbleiter
US4613489A (en) 1983-08-10 1986-09-23 Osaka Titanium Co., Ltd. Process for the disproportionation of chlorosilanes
DE19860146A1 (de) 1998-12-24 2000-06-29 Bayer Ag Verfahren und Anlage zur Herstellung von Silan
WO2007039326A1 (fr) * 2005-09-27 2007-04-12 Evonik Degussa Gmbh Procede de fabrication de monosilane

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0218303A (ja) * 1988-07-07 1990-01-22 Mitsubishi Gas Chem Co Inc 炭化水素の改質反応器および改質方法
DE10057522B4 (de) * 2000-11-21 2009-04-16 Evonik Degussa Gmbh Verfahren zur Herstellung von Silanen
DE102008017304A1 (de) * 2008-03-31 2009-10-01 Schmid Silicon Technology Gmbh Verfahren und Anlage zur Herstellung von Reinstsilizium

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2507864A1 (de) 1974-02-25 1975-08-28 Union Carbide Corp Verfahren zur herstellung von silan
DE2919086A1 (de) 1978-08-18 1980-03-06 Schumacher Co J C Verfahren zur herstellung von polykristallinem silizium
DE3311650A1 (de) 1982-03-31 1983-10-13 Union Carbide Corp., 06817 Danbury, Conn. Verfahren zur herstellung von hoch reinem silan sowie hoch reinem polykristallinem und einkristallinem silicium fuer solarzellen und halbleiter
US4613489A (en) 1983-08-10 1986-09-23 Osaka Titanium Co., Ltd. Process for the disproportionation of chlorosilanes
DE19860146A1 (de) 1998-12-24 2000-06-29 Bayer Ag Verfahren und Anlage zur Herstellung von Silan
WO2007039326A1 (fr) * 2005-09-27 2007-04-12 Evonik Degussa Gmbh Procede de fabrication de monosilane

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Ullmanns Enzyklopädie der technischen Chemie", vol. 13, 1997, pages: 301 - 303

Also Published As

Publication number Publication date
DE102010034469A1 (de) 2012-02-09

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