EP2222401A2 - Katalysator und verfahren zur dismutierung von wasserstoff enthaltenden halogensilanen - Google Patents

Katalysator und verfahren zur dismutierung von wasserstoff enthaltenden halogensilanen

Info

Publication number
EP2222401A2
EP2222401A2 EP08856913A EP08856913A EP2222401A2 EP 2222401 A2 EP2222401 A2 EP 2222401A2 EP 08856913 A EP08856913 A EP 08856913A EP 08856913 A EP08856913 A EP 08856913A EP 2222401 A2 EP2222401 A2 EP 2222401A2
Authority
EP
European Patent Office
Prior art keywords
catalyst
iso
propyl
butyl
column
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Withdrawn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
EP08856913A
Other languages
German (de)
English (en)
French (fr)
Inventor
Hartwig Rauleder
Ekkehard MÜH
Reinhold Schork
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
Priority to EP13154517.0A priority Critical patent/EP2591856A1/de
Publication of EP2222401A2 publication Critical patent/EP2222401A2/de
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/12—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides
    • B01J31/123—Organometallic polymers, e.g. comprising C-Si bonds in the main chain or in subunits grafted to the main chain
    • B01J31/124—Silicones or siloxanes or comprising such units
    • B01J31/127—Silicones or siloxanes or comprising such units the siloxane units, e.g. silsesquioxane units, being grafted onto other polymers or inorganic supports, e.g. via an organic linker
    • 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
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
    • B01J31/0235—Nitrogen containing compounds
    • B01J31/0254—Nitrogen containing compounds on mineral substrates
    • 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
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/0272—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing elements other than those covered by B01J31/0201 - B01J31/0255
    • B01J31/0274—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing elements other than those covered by B01J31/0201 - B01J31/0255 containing 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
    • C01B33/10773—Halogenated silanes obtained by disproportionation and molecular rearrangement of halogenated silanes

Definitions

  • the invention relates to a catalyst, its use as well as a process for the dismutation of hydrogen-containing halosilanes, in particular hydrogen-containing chlorosilanes.
  • the dismutation reaction is used, for example, to prepare monosilane (SiH 4 ), monochlorosilane (CISiH 3 ) and also dichlorosilane (DCS, H 2 SiCl 2 ) from trichlorosilane (TCS, HSiCb) to form the coupling product silicon tetrachloride (STC, SiCl 4 ).
  • the dismutation reaction to produce low chlorinated silanes such as monosilane, monochlorosilane or dichlorosilane, from higher chlorinated silanes, generally trichlorosilane, is performed to more rapidly adjust the chemical balance in the presence of catalysts.
  • an exchange of hydrogen and chlorine atoms between two silane molecules is generally carried out according to the general reaction equation (1) in a so-called dismutation or disproportionation reaction.
  • x can assume the values 1 to 3.
  • the majority of the catalysts used are secondary and tertiary amines or quaternary ammonium salts (cf DE-AS 21 62 537). Thereby, to the
  • reaction according to equation (1) is the preparation of dichlorosilane from trichlorosilane according to EP 0 285 937 A1.
  • a process for the preparation of dichlorosilane by disproportionation of trichlorosilane is disclosed on a fixed catalyst bed in which gaseous dichlorosilane is removed and recovered under pressures between 0.8 and 1.2 bar and reactor temperatures between 10 0 C and the boiling point of the resulting reaction mixture; Portions of trichlorosilane are condensed and recycled to the reactor, the liquid reaction phase is partially withdrawn from the reactor and separated into tetrachlorosilane and trichlorosilane to be recycled to the reactor.
  • catalysts for dismutation also usually ion exchangers are used, for.
  • divinylbenzene crosslinked polystyrene resin having tertiary amine groups which is prepared by direct aminomethylation of a styrene-divinylbenzene copolymer (DE 100 57 521 A1), on solids which are attached to a scaffold made of polystyrene, crosslinked with divinylbenzene, amino or Alkylenamino groups, for example, dimethylamino groups (DE 100 61 680 A1, DE 100 17 168 A1), on anion-exchange resins based catalysts with tertiary amino groups or quaternary ammonium groups (DE 33 11 650 A1 ), amine-functionalized inorganic supports (DE 37 11 444) or according to DE 39 25 357 organopolysiloxane catalysts, such as N [(CH 2 ) 3Si ⁇ 3 / 2].
  • the catalyst in the catalyst bed may correspond to a structured fabric packing or packing of tissue, alternatively, the catalyst bed may also contain packing or internals of catalytically active material.
  • reaction and material separation offer the reactive rectification, because the dismutation reaction is a reaction limited by the chemical equilibrium in the conversion. This fact necessitates the separation of reaction products from the unreacted starting materials in order ultimately to complete the conversion in the overall process.
  • the energetically ideal apparatus would be an infinitely high distillation column, in which on each tray or on each theoretical stage by a suitable catalyst or any length of time
  • Apparatus would have the lowest possible energy consumption and thus the lowest possible operating costs [cf. Figure 6 and Sundmacher &
  • Catalysts on inorganic supports for the production of dichlorosilane (DCS) from trichlorosilane by dismutation The listed catalysts (CH 3 CH 2 O) 3 Si (CH 2 ) 3 N (octyl) 2 and (CH 3 O) 3 Si (CH 2 ) SN (C 2 Hs) 2 have no high activity, so that the catalyst is used in relatively high amounts got to.
  • the object of the present invention is to provide a catalyst system for dismutating hydrogen halosilanes which does not have the mentioned disadvantages and enables a more economical process for the preparation of higher hydrogenated hydrogen halosilanes.
  • a catalyst according to the invention for the dismutation of hydrogen and halogen-containing silicon compounds comprising a support material and at least one linear, cyclic, branched and / or crosslinked aminoalkyl-functional siloxane and / or silanol, wherein at least one siloxane or silanol in an idealized form corresponds to general formula II,
  • A is an aminoalkyl radical - (CH 2 ) 3 -N (R 1 ) 2
  • R 1 is the same or different and iso-butyl, n-butyl, tert-butyl and / or a cyclohexyl group
  • R 2 independently of one another hydrogen, a methyl, ethyl, n-propyl, iso-propyl
  • the catalyst according to the invention has at least one siloxane or silanol with an aminoalkyl radical selected from 3- (N, N-di-n-butylamino), and a> 1 for a silanol ) propyl, 3- (N 1 N-di-tert-butylamino) propyl and / or 3- (N, N-di-iso-butylamino) propyl radical on.
  • siloxane bonds (-O-Si-O-), for example, have been formed by condensation of at least two of the original groups -OR 2 , R 3 and / or R 4 .
  • these catalysts allow a considerably faster adjustment of the equilibrium position in the dismutation reactions.
  • a catalyst In order to produce and recover high purity or ultrahigh purity silicon compounds, a catalyst must be completely anhydrous and / or free of alcohols. High-purity silicon compounds are those whose degree of contamination in the ppb
  • Ultrapure purity means impurities in the ppt range and below.
  • Metal compounds should be at most in the ppb range up to the ppt range, preferably in the ppt range.
  • the required purity can be determined by means of GC, IR, NMR,
  • any porous or microporous material is suitable as the carrier material (Y), preferably silicon dioxide (SiO 2 ) or else zeolites, which are used may additionally contain aluminum, iron, titanium, potassium, sodium, calcium and / or magnesium.
  • the silica may have an acidic, neutral or basic character.
  • the carrier material is particulate and can be used, for example, in the form of shaped articles, such as spheres, pellets, rings, extruded rod-shaped bodies, trilopes, tubes, honeycomb, etc. or in the form of granules, granules or powders, spheres or pellets being preferred.
  • the supported catalyst is preferably based on a microporous support having a pore volume of 100 to 1,000 mm 3 / g and a BET surface area of 10 to 500 nrvVg, preferably 50 to 400 nrvVg, particularly preferably 100 to 200 nrvVg.
  • the expert can determine the pore volume and the BET surface area by means of methods known per se.
  • the support material preferably has a geometric surface area of 100 to 2,000 m 2 / m 3 or a bulk volume of 0.1 to 2 kg / l, preferably of 0.2 to 1 kg / l, particularly preferably 0.4 to 0.9 kg / l, up.
  • the ready-to-use, supported catalyst should be absolutely free of water, solvents, and oxygen, and should not release these materials on heating.
  • the content of aminoalkylalkoxysilane compound used for modifying or impregnating the support material in the preparation of the catalyst is preferably from 0.1 to 40% by weight, based on the amount of support. Levels of from 1 to 25% by weight, more preferably from 10 to 20% by weight, based on the support material, are preferred.
  • aminoalkyl-functional siloxane or silanol of the general formula (II) deposited on the carrier or condensed with the carrier material and advantageously covalently bound thereto via Y-O-Si
  • the aminoalkyl-functional siloxane or silanol may also be deposited as an ammonium salt from a solvent, for example as a hydrohalide such as hydrochloride. In another alternative, it may also be deposited with a carboxylate or sulfate as the counterion.
  • the invention furthermore relates to a process for the preparation of the catalysts according to the invention and to catalysts obtainable by the process in which a support material and at least one alkoxysilane of the general formula I
  • A is an aminoalkyl radical - (CH 2 ) 3 -N (R 1 ) 2 and R 1 is identical or different and iso-butyl, n-butyl, tert-butyl and / or cyclohexyl group
  • R 2 is hydrogen, methyl, ethyl, n-propyl or iso-propyl group
  • R 3 and R 4 are independently a hydroxy, methoxy, ethoxy, n-propoxy, iso-propoxy , Methyl, ethyl, n-propyl and / or iso-propyl group
  • aqueous alcohols for hydrolysis these are, for example, methanol, ethanol, isopropanol with a water content which is in particular in the range from 0.5 to 30% by weight, preferably from 0.5 to 10% by weight. %, more preferably between 1 to 5 wt .-%, is located.
  • 0.5 to 50 mol of water in particular 1 to 20 mol of water, are advantageously used, ie added during the hydrolysis.
  • all solvents are suitable in which the compound of formula I and / or the process product are soluble.
  • Particular preference is given to hydrolyzing and / or condensing in aqueous ethanolic solution.
  • the reaction may be carried out at temperatures between 0 and 150 0 C, under atmospheric pressure or reduced pressure, preferably at 1 to 1 000 mbar, more preferably at 50 to 800 mbar, in particular at 100 to 500 mbar, wherein the reaction is preferably in the boiling heat he follows.
  • At least one alkoxysilane is selected from the group 3- (N, N-di-n-butylamino) propyltrimethoxysilane, 3- (N, N-di-n-butylamino) propyltriethoxysilane, 3- (N, N-di-) tert-butylamino) propylthmethoxysilan, 3- (N, N-di-tert-butylamino) - propyltriethoxysilane, 3- (N, N-di-iso-butylamino) propylthmethoxysilan or 3- (N 1 N-di- iso-butylamino ) Propyltriethoxysilane reacted in the presence of a carrier material, wherein the carrier material is preferably based on silica particles.
  • alkoxysilanes of the general formula (I) may have the following substituents, where R 1 is an isobutyl, n-butyl or tert-butyl group, R 2 is a methyl, ethyl, n-propyl or isobutyl Propyl group and R 4 and R 3 of a methoxy, ethoxy, n-propoxy and / or iso-propoxy group correspond.
  • the ready-to-use catalyst according to the invention for the production of highly pure or ultrahigh-purity silicon compounds must be absolutely anhydrous and / or free of alcohols.
  • the coated catalyst support is advantageously dried to constant weight.
  • the catalyst according to the invention is used in the dismutation of hydrogen and halogen-containing silicon compounds, in particular of 10
  • Halosilanes such as trichlorosilane, which can react to dichlorosilane, monosilane, monochlorosilane and tetrachlorosilane.
  • the invention also provides a process for the dismutation of hydrogen and halogen-containing silicon compounds on the aminoalkyl-functional catalyst according to the invention, which is located in a reactor, wherein the
  • Halogen-containing silicon compound is brought into contact, wherein at least one siloxane or silanol in an idealized form of the general formula II,
  • A is an aminoalkyl radical - (CH 2 ) 3 -N (R 1 ) 2
  • R 1 is identical or different and iso-butyl, n-butyl, tert-butyl and / or cyclohexyl
  • R 2 and R 4 independently of one another are hydroxyl, methoxy, ethoxy, n-propoxy, R 2 and R 4 are each independently of the other hydrogen, a methyl, ethyl, n-propyl, isopropyl group or Y; iso-propoxy, methyl, ethyl, n-propyl, iso-propyl and / or -OY, where Y is the support, HW is an acid, where W is an inorganic or organic acid radical, with a> 1 for the silanol, a> 2 for the siloxane and w> 0, and wherein at least a portion of the resulting reaction mixture is worked up.
  • a preferred catalyst comprises siloxanes and / or silanols having at least one of the following aminoalkyl radicals A, 3- (N, N-di-n-butylamino) propyl, 3- (N, N-di-tert-butylamino) propyl -, and / or 3- (N, N-di-iso-butylamino) propyl groups, wherein the siloxanes and / or silanols in the presence of a carrier material, which is preferably based on the silica described above, were prepared. Depending on the reaction procedure and reactor, the most favorable form of carrier material can be selected. 1 1
  • the catalyst is continuously flown in a reactor with at least one silicon compound of the general formula III H n Si m X (2m + 2-n) to be disiloxane, where X independently of one another corresponds to fluorine, chlorine, bromine and / or iodine and 1 ⁇ n ⁇ (2m + 2) and 1 ⁇ m ⁇ 12, preferably 1 ⁇ m ⁇ 6, more preferably trichlorosilane is converted to dichlorosilane, monochlorosilane and monosilane, which are subsequently separated.
  • the silicon tetrachloride also formed is withdrawn from the chemical equilibrium discontinuously or continuously and can be purified separately.
  • the catalyst is preferably in a catalyst bed.
  • the separation of the halosilanes can take place by means of a column assigned to the reactor, which can be connected, for example, directly to the reactor.
  • a column assigned to the reactor which can be connected, for example, directly to the reactor.
  • higher hydrogenated silicon compounds can be recovered as low boilers at the top of the column and higher chlorinated silicon compounds are enriched as high boilers in a collecting vessel, while at least one unreacted silicon compound recovered as medium boilers on the column and again can be supplied to the associated reactor.
  • the catalyst in a catalyst bed in a reactor is assigned to a separating tray of a column, for example a rectification column.
  • This plant comprises an inventive
  • Catalyst comprising a support material with siloxanes and / or silanols based on the reaction of an aminoalkylalkoxysilane of the general formula I, in particular siloxanes and / or silanols according to the general formula II, wherein the system comprises at least one distillation column (1) with a 12
  • the starting or filling of the system with higher chlorinated silanes as reactant, in particular with trichlorosilane, and the Eduktzuschreib during operation of the system can be done for example via leads or taps of Eduktaufgabe (1.3) and / or on the column template (1.1).
  • a removal of products can be carried out via the top of the column (1.8), the removal point (1.5) and / or the column template (1.4).
  • the catalyst may be present in the catalyst bed (3) in the form of packing, which may be present, for example, as a bed or as a compressed mold body.
  • the plant can be advantageously equipped with a heated column bottom (1.6, 1.1) and a cryogenic cooling (1.7) in the column head (1.2).
  • the column (1) can be equipped with at least one column packing (8) and have at least one additional educt feed (1.3) or product removal (1.5). 13
  • the catalyst bed of a side reactor is preferably operated at a temperature from -80 to 120 0 C, with the reactor or catalyst bed temperature regulated advantageously of a cooling or heating jacket of the reactor or controlled (2.1) will can.
  • a sufficiently long residence time on the catalyst i. H. a sufficiently low catalyst loading is to ensure the approximate achievement of the chemical equilibrium
  • the reactor as conventional reactors for comparable product flows.
  • the usable reactors (2) should be dimensioned so that 80 to 98% of the equilibrium conversion can be achieved.
  • the silicon compounds dichlorosilane, monochlorosilane and / or monosilane prepared by the process according to the invention are highly pure to ultra-high purity and are especially suitable as precursors for the production of silicon nitride, silicon oxynitride, silicon carbide, silicon oxycarbide or silicon oxide and as precursors for generating epitaxial layers.
  • the SiO 2 balls were predried for one hour at a pressure of 300 to 30 mbar and a bath temperature of 110 to 120 0 C and then dried for 9.5 hours at ⁇ 1 mbar.
  • reaction mixture 150 m 2 / g, bulk density: 0.55 g / cm 3 ). The reaction mixture was
  • the comparative examples clearly demonstrate that the catalyst of the invention is able to adjust the desired short residence times of trichlorosilane on the catalyst. Short residence times are particularly desirable in continuous process control.
  • the catalyst prepared according to Example 3 was subjected to continuous operation over several months and checked its activity. In addition, the continuous operation was interrupted, the catalyst bed drained and put back into operation. The determination of the rates of dissolution showed a constant activity of the catalyst.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
EP08856913A 2007-12-06 2008-10-08 Katalysator und verfahren zur dismutierung von wasserstoff enthaltenden halogensilanen Withdrawn EP2222401A2 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP13154517.0A EP2591856A1 (de) 2007-12-06 2008-10-08 Anlage mit Katalysator zur Dismutierung von Wasserstoff enthaltenden Halogensilanen

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102007059170A DE102007059170A1 (de) 2007-12-06 2007-12-06 Katalysator und Verfahren zur Dismutierung von Wasserstoff enthaltenden Halogensilanen
PCT/EP2008/063461 WO2009071358A2 (de) 2007-12-06 2008-10-08 Katalysator und verfahren zur dismutierung von wasserstoff enthaltenden halogensilanen

Publications (1)

Publication Number Publication Date
EP2222401A2 true EP2222401A2 (de) 2010-09-01

Family

ID=40210437

Family Applications (2)

Application Number Title Priority Date Filing Date
EP08856913A Withdrawn EP2222401A2 (de) 2007-12-06 2008-10-08 Katalysator und verfahren zur dismutierung von wasserstoff enthaltenden halogensilanen
EP13154517.0A Withdrawn EP2591856A1 (de) 2007-12-06 2008-10-08 Anlage mit Katalysator zur Dismutierung von Wasserstoff enthaltenden Halogensilanen

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP13154517.0A Withdrawn EP2591856A1 (de) 2007-12-06 2008-10-08 Anlage mit Katalysator zur Dismutierung von Wasserstoff enthaltenden Halogensilanen

Country Status (11)

Country Link
US (1) US20100296994A1 (enExample)
EP (2) EP2222401A2 (enExample)
JP (1) JP2011505246A (enExample)
KR (1) KR20100092478A (enExample)
CN (1) CN101450323A (enExample)
BR (1) BRPI0821154A2 (enExample)
CA (1) CA2706418A1 (enExample)
DE (1) DE102007059170A1 (enExample)
RU (1) RU2492924C9 (enExample)
UA (1) UA104851C2 (enExample)
WO (1) WO2009071358A2 (enExample)

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004037675A1 (de) * 2004-08-04 2006-03-16 Degussa Ag Verfahren und Vorrichtung zur Reinigung von Wasserstoffverbindungen enthaltendem Siliciumtetrachlorid oder Germaniumtetrachlorid
DE102005041137A1 (de) 2005-08-30 2007-03-01 Degussa Ag Reaktor, Anlage und großtechnisches Verfahren zur kontinuierlichen Herstellung von hochreinem Siliciumtetrachlorid oder hochreinem Germaniumtetrachlorid
DE102006003464A1 (de) * 2006-01-25 2007-07-26 Degussa Gmbh Verfahren zur Erzeugung einer Siliciumschicht auf einer Substratoberfläche durch Gasphasenabscheidung
DE102007007874A1 (de) 2007-02-14 2008-08-21 Evonik Degussa Gmbh Verfahren zur Herstellung höherer Silane
DE102007014107A1 (de) 2007-03-21 2008-09-25 Evonik Degussa Gmbh Aufarbeitung borhaltiger Chlorsilanströme
DE102007048937A1 (de) * 2007-10-12 2009-04-16 Evonik Degussa Gmbh Entfernung von polaren organischen Verbindungen und Fremdmetallen aus Organosilanen
DE102007050199A1 (de) * 2007-10-20 2009-04-23 Evonik Degussa Gmbh Entfernung von Fremdmetallen aus anorganischen Silanen
DE102007050573A1 (de) * 2007-10-23 2009-04-30 Evonik Degussa Gmbh Großgebinde zur Handhabung und für den Transport von hochreinen und ultra hochreinen Chemikalien
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
DE102008054537A1 (de) * 2008-12-11 2010-06-17 Evonik Degussa Gmbh Entfernung von Fremdmetallen aus Siliciumverbindungen durch Adsorption und/oder Filtration
DE102009027728A1 (de) * 2009-07-15 2011-01-20 Evonik Degussa Gmbh Verfahren zur Behandlung von Katalysator-Präkursoren
DE102009027730A1 (de) * 2009-07-15 2011-01-27 Evonik Degussa Gmbh Verahren und Verwendung von aminofunktionellen Harzen zur Dismutierung von Halogensilanen und zur Entfernung von Fremdmetallen
DE102009053804B3 (de) 2009-11-18 2011-03-17 Evonik Degussa Gmbh Verfahren zur Herstellung von Hydridosilanen
DE102010002342A1 (de) 2010-02-25 2011-08-25 Evonik Degussa GmbH, 45128 Verwendung der spezifischen Widerstandsmessung zur indirekten Bestimmung der Reinheit von Silanen und Germanen und ein entsprechendes Verfahren
DE102010043649A1 (de) 2010-11-09 2012-05-10 Evonik Degussa Gmbh Verfahren zur Spaltung höherer Silane
DE102010043648A1 (de) 2010-11-09 2012-05-10 Evonik Degussa Gmbh Verfahren zur selektiven Spaltung höherer Silane
DE102011002436A1 (de) * 2011-01-04 2012-07-05 Evonik Degussa Gmbh Hydrierung von Organochlorsilanen und Siliciumtetrachlorid
DE102011004058A1 (de) * 2011-02-14 2012-08-16 Evonik Degussa Gmbh Monochlorsilan, Verfahren und Vorrichtung zu dessen Herstellung
CN103241743B (zh) * 2013-05-22 2015-07-22 黄国强 三氯氢硅直接歧化制备硅烷的反应精馏方法及设备
CN103449449B (zh) * 2013-08-30 2015-09-09 中国恩菲工程技术有限公司 制备三氯氢硅的方法及其设备
EP3659964A1 (en) 2018-11-28 2020-06-03 Hysilabs, SAS Catalysed process of production of hydrogen from silylated derivatives as hydrogen carrier compounds
CN111659329B (zh) * 2019-03-07 2022-05-24 江西福特化工新材料有限公司 缩合反应装置
CN113651844B (zh) * 2021-08-20 2023-09-12 唐山偶联硅业有限公司 连续法制备二甲基氢氯硅烷的工艺

Family Cites Families (54)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2009A (en) * 1841-03-18 Improvement in machines for boring war-rockets
US403202A (en) * 1889-05-14 Xjohn s stewart macarthur
US358259A (en) * 1887-02-22 Halp to aaeon a- haepee
US2008A (en) * 1841-03-18 Gas-lamp eok conducting gas pkom ah elevated buhner to one below it
CA988275A (en) * 1970-12-17 1976-05-04 Carl J. Litteral Disproportionation of chlorosilicon hydrides
BE784818A (fr) * 1971-06-14 1972-12-13 Westinghouse Electric Corp Etalonnage du profil de deplacement de la position d'un entrainement par moteur
US3968199A (en) 1974-02-25 1976-07-06 Union Carbide Corporation Process for making silane
US4676967A (en) * 1978-08-23 1987-06-30 Union Carbide Corporation High purity silane and silicon production
KR860000661B1 (ko) * 1984-05-17 1986-05-29 한국과학기술원 염화실란의 불균등화 반응촉매의 제조방법
US4613491A (en) * 1984-05-17 1986-09-23 Korea Advanced Institute Of Science And Technology Redistribution catalyst and methods for its preparation and use to convert chlorosilicon hydrides to silane
DE3711444A1 (de) * 1987-04-04 1988-10-13 Huels Troisdorf Verfahren und vorrichtung zur herstellung von dichlorsilan
DE3712098A1 (de) * 1987-04-10 1988-10-20 Wacker Chemie Gmbh Verfahren zur herstellung von disproportionierungsprodukten von dichlormethylsilan in gegenwart eines katalysators
DE3828549A1 (de) * 1988-08-23 1990-03-08 Huels Chemische Werke Ag Verfahren zur entfernung von silanverbindungen aus silanhaltigen abgasen
US5417938A (en) 1988-09-02 1995-05-23 Sulzer Brothers Limited Device for carrying out catalyzed reactions
DE3925357C1 (enExample) * 1989-07-31 1991-04-25 Degussa Ag, 6000 Frankfurt, De
DE4323406C2 (de) * 1993-07-13 2001-02-15 Wacker Chemie Gmbh Verfahren zur Herstellung von Methylchlorsilanen aus Methylchlordisilanen
DE4419270A1 (de) * 1994-06-01 1995-12-07 Wacker Chemie Gmbh Verfahren zur Herstellung von Alkyl- oder Aryldichlorsilanen
EP0702017B1 (de) * 1994-09-14 2001-11-14 Degussa AG Verfahren zur Herstellung von chloridarmen bzw. chloridfreien aminofunktionellen Organosilanen
DE19516386A1 (de) * 1995-05-04 1996-11-07 Huels Chemische Werke Ag Verfahren zur Herstellung von an chlorfunktionellen Organosilanen armen bzw. freien aminofunktionellen Organosilanen
DE19520737C2 (de) * 1995-06-07 2003-04-24 Degussa Verfahren zur Herstellung von Alkylhydrogenchlorsilanen
DE19649023A1 (de) * 1996-11-27 1998-05-28 Huels Chemische Werke Ag Verfahren zur Entfernung von Restmengen an acidem Chlor in Carbonoyloxysilanen
DE19746862A1 (de) * 1997-10-23 1999-04-29 Huels Chemische Werke Ag Vorrichtung und Verfahren für Probenahme und IR-spektroskopische Analyse von hochreinen, hygroskopischen Flüssigkeiten
DE19847786A1 (de) * 1998-10-16 2000-04-20 Degussa Vorrichtung und Verfahren zum Befüllen und Entleeren eines mit brennbarem sowie aggressivem Gas beaufschlagten Behälters
DE19849196A1 (de) * 1998-10-26 2000-04-27 Degussa Verfahren zur Neutralisation und Minderung von Resthalogengehalten in Alkoxysilanen oder Alkoxysilan-basierenden Zusammensetzungen
ATE284406T1 (de) * 1998-11-06 2004-12-15 Degussa Verfahren zur herstellung von chloridarmen oder chloridfreien alkoxysilanen
DE19918115C2 (de) * 1999-04-22 2002-01-03 Degussa Verfahren zur Herstellung von Vinylchlorsilanen
DE19918114C2 (de) * 1999-04-22 2002-01-03 Degussa Verfahren und Vorrichtung zur Herstellung von Vinylchlorsilanen
DE19963433A1 (de) * 1999-12-28 2001-07-12 Degussa Verfahren zur Abscheidung von Chlorsilanen aus Gasströmen
DE10017168A1 (de) * 2000-04-07 2001-10-11 Bayer Ag Verfahren und Anlage zur Herstellung von Silan
US6576588B2 (en) * 2000-04-07 2003-06-10 Catalytic Distillation Technologies Process for selective hydrogenation of alkynes and catalyst therefor
DE10057522B4 (de) * 2000-11-21 2009-04-16 Evonik Degussa Gmbh Verfahren zur Herstellung von Silanen
DE10057521B4 (de) 2000-11-21 2009-04-16 Evonik Degussa Gmbh Verfahren zur Herstellung von Silanen
DE10057519A1 (de) * 2000-11-21 2002-05-23 Solarworld Ag Verfahren zur Herstellung von Silanen
DE10061680A1 (de) 2000-12-11 2002-06-20 Solarworld Ag Verfahren zur Herstellung von Silan
DE10116007A1 (de) * 2001-03-30 2002-10-02 Degussa Vorrichtung und Verfahren zur Herstellung von im Wesentlichen halogenfreien Trialkoxysilanen
DE10330022A1 (de) * 2003-07-03 2005-01-20 Degussa Ag Verfahren zur Herstellung von Iow-k dielektrischen Filmen
DE102004008442A1 (de) * 2004-02-19 2005-09-15 Degussa Ag Siliciumverbindungen für die Erzeugung von SIO2-haltigen Isolierschichten auf Chips
DE102004025766A1 (de) * 2004-05-26 2005-12-22 Degussa Ag Herstellung von Organosilanestern
DE102004037675A1 (de) * 2004-08-04 2006-03-16 Degussa Ag Verfahren und Vorrichtung zur Reinigung von Wasserstoffverbindungen enthaltendem Siliciumtetrachlorid oder Germaniumtetrachlorid
DE102004045245B4 (de) 2004-09-17 2007-11-15 Degussa Gmbh Vorrichtung und Verfahren zur Herstellung von Silanen
EP1661628A1 (en) * 2004-11-25 2006-05-31 Total Petrochemicals Research Feluy Process for dispersing functional molecules on the surface of a support and support made by this process
RU2279403C1 (ru) * 2004-12-27 2006-07-10 Федеральное государственное унитарное предприятие "Государственный научно-исследовательский институт химии и технологии элементоорганических соединений" (ФГУП ГНИИХТЭОС) Способ получения моносилана высокой чистоты
DE102005041137A1 (de) * 2005-08-30 2007-03-01 Degussa Ag Reaktor, Anlage und großtechnisches Verfahren zur kontinuierlichen Herstellung von hochreinem Siliciumtetrachlorid oder hochreinem Germaniumtetrachlorid
UA13211U (en) * 2005-10-10 2006-03-15 Yurii Oleksandrovych Kasatkin A method for producing monosilane
DE102006003464A1 (de) * 2006-01-25 2007-07-26 Degussa Gmbh Verfahren zur Erzeugung einer Siliciumschicht auf einer Substratoberfläche durch Gasphasenabscheidung
DE102007023759A1 (de) * 2006-08-10 2008-02-14 Evonik Degussa Gmbh Anlage und Verfahren zur kontinuierlichen industriellen Herstellung von Fluoralkylchlorsilan
DE102007007874A1 (de) * 2007-02-14 2008-08-21 Evonik Degussa Gmbh Verfahren zur Herstellung höherer Silane
DE102007014107A1 (de) * 2007-03-21 2008-09-25 Evonik Degussa Gmbh Aufarbeitung borhaltiger Chlorsilanströme
DE102007048937A1 (de) * 2007-10-12 2009-04-16 Evonik Degussa Gmbh Entfernung von polaren organischen Verbindungen und Fremdmetallen aus Organosilanen
DE102007050199A1 (de) * 2007-10-20 2009-04-23 Evonik Degussa Gmbh Entfernung von Fremdmetallen aus anorganischen Silanen
DE102007050573A1 (de) * 2007-10-23 2009-04-30 Evonik Degussa Gmbh Großgebinde zur Handhabung und für den Transport von hochreinen und ultra hochreinen Chemikalien
DE102008004397A1 (de) * 2008-01-14 2009-07-16 Evonik Degussa Gmbh Verfahren zur Verminderung des Gehaltes von Elementen, wie Bor, in Halogensilanen sowie Anlage zur Durchführung des Verfahrens
US20090197014A1 (en) * 2008-02-04 2009-08-06 Atomic Energy Council - Institute Of Nuclear Energy Research Apparatus and method for coating diamond on work pieces via hot filament chemical vapor deposition
DE102009053804B3 (de) * 2009-11-18 2011-03-17 Evonik Degussa Gmbh Verfahren zur Herstellung von Hydridosilanen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2009071358A2 *

Also Published As

Publication number Publication date
US20100296994A1 (en) 2010-11-25
RU2492924C2 (ru) 2013-09-20
KR20100092478A (ko) 2010-08-20
WO2009071358A2 (de) 2009-06-11
CA2706418A1 (en) 2009-06-11
EP2591856A1 (de) 2013-05-15
WO2009071358A3 (de) 2009-08-13
DE102007059170A1 (de) 2009-06-10
CN101450323A (zh) 2009-06-10
JP2011505246A (ja) 2011-02-24
BRPI0821154A2 (pt) 2015-06-16
RU2010127424A (ru) 2012-01-20
UA104851C2 (uk) 2014-03-25
RU2492924C9 (ru) 2014-03-27

Similar Documents

Publication Publication Date Title
EP2222401A2 (de) Katalysator und verfahren zur dismutierung von wasserstoff enthaltenden halogensilanen
EP2294006B1 (de) Verfahren zur entfernung von bor enthaltenden verunreinigungen aus halogensilanen sowie anlage zur durchführung des verfahrens
EP2637968B1 (de) Verfahren zur selektiven spaltung höherer silane
EP2229342B1 (de) Verfahren zur verminderung des gehaltes von elementen, wie bor, in halogensilanen sowie anlage zur durchführung des verfahrens
WO2012062562A2 (de) Verfahren zur spaltung höherer silane
CN101466463B (zh) 生产甲硅烷的方法
DE102009027730A1 (de) Verahren und Verwendung von aminofunktionellen Harzen zur Dismutierung von Halogensilanen und zur Entfernung von Fremdmetallen
EP2454016A2 (de) Verfahren zur behandlung von aminofunktionellen, polymeren katalysator-präkursoren
DE102011110040B4 (de) Verfahren zur Herstellung von Chlorsilanen mittels hochsiedender Chlorsilane oder chlorsilanhaltiger Gemische
JP5317707B2 (ja) クロロシラン統合プラント内での高沸点化合物の再利用方法
DE10057482A1 (de) Verfahren zur Reinigung von Trichlorsilan
DE102010043646A1 (de) Verfahren zur Herstellung von Trichlorsilan
EP2956462B1 (de) Verfahren zur veresterung von siliziumhalogenverbindungen in einer kolonne und dafür geeignete vorrichtung
EP1316557A1 (de) Verfahren zur Herstellung von in 3-Stellung funktionalisierten Propylsilanen
KR101414694B1 (ko) 디실란의 변환 방법
DE10057521A1 (de) Verfahren zur Herstellung von Silanen
CN223069100U (zh) 一种降低多晶硅中施、受主杂质的氯硅烷原料提纯系统
DE102011082662A1 (de) Verwertung niedrigsiedender Verbindungen in Chlorsilan-Prozessen
DE2162537B2 (de) Verfahren zur herstellung von disproportionierungsprodukten von chlorsilanen

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20100519

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MT NL NO PL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: AL BA MK RS

DAX Request for extension of the european patent (deleted)
17Q First examination report despatched

Effective date: 20120809

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

INTG Intention to grant announced

Effective date: 20141215

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20150428