EP2429673A1 - Distillation de silane à utilisation d'énergie réduite - Google Patents

Distillation de silane à utilisation d'énergie réduite

Info

Publication number
EP2429673A1
EP2429673A1 EP10722027A EP10722027A EP2429673A1 EP 2429673 A1 EP2429673 A1 EP 2429673A1 EP 10722027 A EP10722027 A EP 10722027A EP 10722027 A EP10722027 A EP 10722027A EP 2429673 A1 EP2429673 A1 EP 2429673A1
Authority
EP
European Patent Office
Prior art keywords
heat
distillation apparatus
vapors
column
distillation
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Withdrawn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
EP10722027A
Other languages
German (de)
English (en)
Inventor
Peter Nürnberg
Birgit FRÖBEL
Michael Hallmann
Christian Kaltenmarkner
Benedikt Postberg
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.)
Wacker Chemie AG
Original Assignee
Wacker Chemie AG
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 Wacker Chemie AG filed Critical Wacker Chemie AG
Publication of EP2429673A1 publication Critical patent/EP2429673A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/143Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/146Multiple effect distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/143Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/148Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/12Organo silicon halides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/20Purification, separation

Definitions

  • the invention relates to a process for the distillation of silane mixtures f in the heat for heating the distillation apparatus of vapors of another
  • the difficulty of silane distillation is in particular their high purity requirements, for example, is dimethyldichlorosilane with very low levels of
  • Methyltrichlorosilane and Ethyldichlorsilan required, the contents of the latter components vary greatly in the silane mixture to be distilled. These boundary conditions require an extremely stable adjustment of the operating parameters of the distillation network as well as a variable adaptation of the operating parameters to the changing silane compositions.
  • the invention relates to a process for the thermal separation of silane mixtures containing silanes selected from alkylchlorosilanes and hydrogenchlorosilanes in a distillation apparatus in which at least a portion of the heat for heating the distillation apparatus is transferred from vapors of a v / eiteren distillation apparatus and wherein a Silane product is obtained with impurities of not more than 200 ppm.
  • the energy content of the vapor stream is utilized, which has been previously discharged via heat transfer to the environment.
  • the process can save up to 85% of energy compared to conventional distillation. Surprisingly, despite this energy saving, the distillation of highly pure alkylchlorosilane and hydrogenchlorosilanes succeeds.
  • the vapors are condensed and the
  • the distillation device consists of one or more columns.
  • the further distillation device consists of one or more columns.
  • At least 20% by weight / in particular at least 50% by weight of the vapors of the further distillation apparatus give off heat for heating the distillation apparatus.
  • At least 10%, in particular at least 20%, of the heat for heating the distillation apparatus is transferred from vapors to a further distillation apparatus.
  • heat of the vapors of the further distillation apparatus is discharged to a heat exchanger to a heat carrier and this heat carrier used to heat the distillation apparatus.
  • heat of the vapors of the further distillation apparatus is discharged by condensation to a heat exchanger.
  • the heat of the vapors of the further distillation apparatus is used as a heat source in a cyclic process used.
  • the heat of the vapors of the further distillation apparatus is passed through a heat pump.
  • the vapors of the further distillation apparatus are used to heat the bottom of the distillation apparatus.
  • the distillation device is a column.
  • the vapors accumulating at the top of a column are compressed and thereby heated. Heat is then transferred to a heat carrier in a heat exchanger and this heat carrier is used to heat the bottom of this column.
  • the distillation apparatus and the further distillation apparatus are identical.
  • FIG. 1 A further preferred embodiment is illustrated by FIG. 1:
  • silane mixture (A1) is distilled.
  • the vapor withdrawn at the top (B1) is condensed in a heat exchanger (W1) and gives off heat to a heat transfer medium.
  • the heat carrier heats the sump of the column (K2).
  • the heat carrier can be additionally heated in a further heat exchanger (W2).
  • the column (K2) is fed to silane mixture (A2) and distilled.
  • the at the top of the column (K2) withdrawn vapors (B2) are condensed in a heat exchanger (W3) and give off heat to a heat carrier.
  • the bottom (C2) is discharged at the bottom of the column (K2).
  • the produced silane product is obtained with impurities of at most 200 ppm at the bottom of the distillation apparatus.
  • Silane mixtures containing silanes selected from alkylchlorosilanes and hydrogenchlorosilanes are preferably also separated in the further distillation apparatus.
  • Silanprod ⁇ kt with impurities of at most 200 ppm are preferably also produced in the further distillation device.
  • the alkylchlorosilane and / or hydrogenchlorosilanes to be separated preferably correspond to the general formula (D
  • R 1 is a hydrocarbon radical having 1-10 carbon atoms, a is 0, 1, 2, 3 or 4 and b is 0, 1, 2 or 3.
  • Particularly preferred hydrocarbon radicals R 1 are the alkyl radicals having 1 to 6 carbon atoms, in particular the methyl and ethyl radicals.
  • the silane product produced contains impurities of at most 100 ppm, particularly preferably at most 50 ppm, in particular at most 20 ppm.
  • the proportion of a single compound in the impurities is preferably at most 100 ppm, particularly preferably at most 60 ppm, in particular at most 15 ppm.
  • dimethyldichlorosilane is obtained, which preferably contains in each case at most 100 ppm, more preferably at most 60 ppm, in particular at most 15 ppm methyltrichlorosilane and ethyldichlorosilane.
  • mixtures are used, in addition to
  • the top product (B) consists of 18% dimethyldichlorosilane, 58% methyltrichlorosilane, 16% trimethylchlorosilane and 8% methylhydrogen dichlorosilane.
  • the bottom product (C) consists of 100% dimethyldichlorosilane.
  • the dimethyldichlorosilane can be distilled as needed with less than 80 ppm, with less than 20 ppm and in particular with 10-15 ppm methyltrichlorosilane impurities.
  • Vapor from other columns (K3) and (K4) give 1.5 MW condensation heat to a heat pump ⁇ columns (K3) and (K4) and the heat pump not shown in Figure 1). This heats with the addition of another 0.8 MW heat exchanger (Wl) the bottom of the column (K2). The energy saving is 65%.

Landscapes

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

Abstract

L'invention a pour objet un procédé de séparation thermique de mélanges de silane qui renferment le silane sélectionné à partir d'alkylchlorosilanes et d'hydrogénochlorosilanes, dans un dispositif de distillation, procédé caractérisé en ce qu'au moins une partie de la chaleur est transférée, pour le chauffage du dispositif de distillation, par les vapeurs d'échappement d'un autre dispositif de distillation, et en ce qu'un produit de silane est obtenu avec un maximum de 200 ppm d'impuretés.
EP10722027A 2009-05-15 2010-05-05 Distillation de silane à utilisation d'énergie réduite Withdrawn EP2429673A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102009003163A DE102009003163A1 (de) 2009-05-15 2009-05-15 Silandestillation mit reduziertem Energieeinsatz
PCT/EP2010/056090 WO2010130609A1 (fr) 2009-05-15 2010-05-05 Distillation de silane à utilisation d'énergie réduite

Publications (1)

Publication Number Publication Date
EP2429673A1 true EP2429673A1 (fr) 2012-03-21

Family

ID=42711796

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10722027A Withdrawn EP2429673A1 (fr) 2009-05-15 2010-05-05 Distillation de silane à utilisation d'énergie réduite

Country Status (7)

Country Link
US (1) US20120048719A1 (fr)
EP (1) EP2429673A1 (fr)
JP (1) JP2012526743A (fr)
KR (1) KR20120023768A (fr)
CN (1) CN102427864A (fr)
DE (1) DE102009003163A1 (fr)
WO (1) WO2010130609A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013207282A1 (de) 2013-04-22 2014-11-06 Wacker Chemie Ag Verfahren und Vorrichtung zur destillativen Trennung eines Drei- oder Mehrkomponentengemisches
EP3769830A1 (fr) * 2019-07-22 2021-01-27 Sulzer Management AG Procédé de distillation d'une composition brute dans une installation de rectification comprenant une pompe à chaleur indirecte

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3168542A (en) * 1957-05-15 1965-02-02 Union Carbide Corp Process for separating mixtures of chlorosilanes
US4402797A (en) * 1982-09-20 1983-09-06 Dow Corning Corporation Separation of chlorosilanes by extractive distillation
JP3501171B2 (ja) * 1994-03-30 2004-03-02 日本エア・リキード株式会社 超高純度モノシランの製造方法及び装置
US5735141A (en) * 1996-06-07 1998-04-07 The Boc Group, Inc. Method and apparatus for purifying a substance
DE19842154C2 (de) * 1998-09-15 2000-11-09 Aventis Res & Tech Gmbh & Co Verfahren zur Verbesserung der rektifikativen Trennung von Methyltrichlorsilan und Dimethyldichlorsilan
DE102004045245B4 (de) * 2004-09-17 2007-11-15 Degussa Gmbh Vorrichtung und Verfahren zur Herstellung von Silanen
DE102008000490A1 (de) 2008-03-03 2008-12-18 Wacker Chemie Ag Verfahren zur thermischen Trennung von Silanen
US20100061912A1 (en) * 2008-09-08 2010-03-11 Stephen Michael Lord Apparatus for high temperature hydrolysis of water reactive halosilanes and halides and process for making same
US8298490B2 (en) * 2009-11-06 2012-10-30 Gtat Corporation Systems and methods of producing trichlorosilane
KR101292545B1 (ko) * 2009-12-28 2013-08-12 주식회사 엘지화학 트리클로로실란의 정제 방법 및 정제 장치

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2010130609A1 *

Also Published As

Publication number Publication date
US20120048719A1 (en) 2012-03-01
CN102427864A (zh) 2012-04-25
KR20120023768A (ko) 2012-03-13
WO2010130609A1 (fr) 2010-11-18
DE102009003163A1 (de) 2010-11-25
JP2012526743A (ja) 2012-11-01

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