EP3230206A1 - Verfahren zur gewinnung von hexachlordisilan aus in prozessabgasströmen enthaltenen gemischen von chlorsilanen - Google Patents
Verfahren zur gewinnung von hexachlordisilan aus in prozessabgasströmen enthaltenen gemischen von chlorsilanenInfo
- Publication number
- EP3230206A1 EP3230206A1 EP15825916.8A EP15825916A EP3230206A1 EP 3230206 A1 EP3230206 A1 EP 3230206A1 EP 15825916 A EP15825916 A EP 15825916A EP 3230206 A1 EP3230206 A1 EP 3230206A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- ring size
- general formula
- hexachlorodisilane
- mixture
- hydrogen
- 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- Withdrawn
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
- C01B33/10773—Halogenated silanes obtained by disproportionation and molecular rearrangement of halogenated silanes
-
- 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
- B01J31/0237—Amines
-
- 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
- B01J31/0239—Quaternary ammonium compounds
-
- 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
- C01B33/10778—Purification
Definitions
- Siemens process as well as other CVD processes of microelectronics using chlorosilanes, the hydrogenation of silicon tetrachloride to produce trichlorosilane or the trichlorosilane synthesis of metallurgical silicon, for example, produce such process gases.
- the low-boiling components are used in one or more distillation steps
- Chlorosilane mixture with components having a boiling point> 57 ° C (b ei 1013.25 mbar).
- This chlorosilane mixture contains Si 2 Cl 6 (hexachlorodisilane) and further partially hydrogenated chlorodisilanes having the general formula
- Hexachlorodisilane is an important starting material in microelectronics.
- the compound is, inter alia, precursor in CVD deposition for high-purity silicon nitride, silicon oxide or silicon carbide layers.
- Hexachlorodisilane plays an important role in transistor fabrication in memory chips. Low-temperature epitaxy becomes epitaxial silicon layers
- Another method describes the reaction with chlorine gas, which leads, according to EP 2036859 B1, to cleavage of the silicon-silicon bond and thus the high-quality disilanes having the general formula Si x HyCl 2 x + 2 y, where x is 2 and y equal to 1-5 is to be destroyed.
- the aim of this reaction is to convert the disilane to silicon tetrachloride and return it back to the material cycle in order to increase the material yield.
- Pentachlorodisilane mixtures of organotitrogen or phosphorus compounds described The objective of the applicants is complete decomposition of the listed disilanes to trichlorosilane, silicon tetrachloride and solid polychlorosilane.
- the present invention is therefore based on the object to provide a method which is a separation of Hexachlordisilans with high yields from the described chlorosilane mixtures, which in the thermal reaction of hydrogen with monosilanes of the general formula Si x HyCl 2 x + 2-y, where x equals 1 and y equals 0 - 2, is available.
- the object is achieved by a method for obtaining
- the reaction is carried out in a batch or in a continuous process.
- a further advantageous embodiment of the method is that the catalyst to inorganic, such as Al 2 0 3 , Si0 2 or organic, such as co-polymer of styrene and divinylbenzene, solids immobilized, dispersed or in a mixture of
- Chlorosilanes dissolved is used.
- Quaternary amines / ammonium salts of general formula II :
- the organic radicals may be linear or branched
- the chlorosilane mixture is mixed with silicon tetrachloride, which advantageously leads to an increase in yield.
- a further embodiment is characterized in that after the catalytic conversion of the chlorosilane mixture, the distillative separation of the
- Reaction mixture takes place or the catalytic reaction takes place during a reactive distillation.
- the advantages here are in particular the lower equipment costs and the better energy balance. Increase the temperature, then catalytically
- alkylated or arylated tertiary amines such as trimethylamine
- alkylated or arylated tertiary amines which have groupings such as dimethylamino groups, heterocyclic nitrogen compounds (azines), pyridine groups or nitriles or quaternary amines, with trimethylammonium chloride groups on one
- organic carrier material such as e.g. a copolymer of styrene and divinylbenzene or on an inorganic support material, e.g. Silica, are immobilized.
- the heterogeneous catalyst is used in the form of pellets containing a
- the catalyst still has sufficient stability at at least 100 ° C., is insoluble and substantially does not tend to split off the amine.
- the catalytically active functional groups are easily accessible.
- tertiary alkylamines such as:
- Trimethylamine which are soluble in the system one and have a significantly lower boiling point than that of hexachlorodisilane, so that a good separation is guaranteed.
- chlorosilane mixtures having proportions of chlorosilanes of the general formula Si x HyCl 2X + 2 .y, where x is 2 and y is 0-5, of
- the catalytic conversion of the chlorosilane mixture leads mainly to the formation of hexachlorodisilane and higher boiling silicon compounds, which a particularly clean separation of Hexachlordisilan allows.
- hexachlorodisilane can be separated from the exhaust gases of the processes described with low equipment costs and low costs, without additional safety risks, in high purity. This is achieved by means of the selective catalytic reaction of partially hydrogenated chlorodisilane moieties in the chlorosilane mixture, having the general formula Si x HyCl 2 x + 2 -y- where x is 2 and y is 0-5.
- Hexachlorodisilane from mixtures of chlorosilanes in a process exhaust gas 1 process exhaust gases, after conversion into the liquid phase by
- a fraction 7.2 contains the target product hexachlorodisilane Si 2 Cl 6 and the distillation bottom 7.3 contains a mixture of higher-boiling silicon compounds having> 2 silicon atoms in the
- the chlorosilane mixture from the separation region 4 is catalytically reacted during the distillation by means of a reactive distillation 6.
- fraction 6.1 which contains mainly trichlorosilane
- the catalyst must be separated from the liquid phase prior to further distillation in order then to obtain silicon tetrachloride as a separate fraction 6.2 and hexachlorodisilane as fraction 6.3.
- a distillation bottoms 6.4 remains from higher-boiling silicon compounds having> 2 silicon atoms in the molecule.
- Embodiment 1 (Comparative Example)
- Exemplary embodiment 2 (according to FIG. 1, implementation 5)
- Embodiment 3 (according to FIG. 1, implementation 5)
- HCDS hexachlorodisilane
- HSS higher boiling silicon compounds
- Exemplary embodiment 5 (according to FIG. 1, implementation 5)
- HCDS hexachlorodisilane
- HSS higher boiling silicon compounds
- Exemplary embodiment 6 (according to FIG. 1, implementation 5)
- Hexachlorodisilane further higher-boiling silicon compounds.
- Exemplary embodiment 7 (according to FIG. 1, implementation 5)
- Diphenylphosphine-functionalized silica (catalyst) at 20 ° C After one week at room temperature, the composition was redetermined (Table 7). The catalyst was filtered off and the mixture was separated by distillation. Three fractions were taken. The third fraction or the bottom contained, in addition to hexachlorodisilane, further higher-boiling silicon compounds. Table 7.
- TCS trichlorosilane
- STC silicon tetrachloride
- TCDS tetrachlorodisilane
- PCDS pentachlorodisilane
- HCDS hexachlorodisilane
- HSS higher-boiling silicon compounds
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102014018435.8A DE102014018435A1 (de) | 2014-12-10 | 2014-12-10 | Verfahren zur Gewinnung von Hexachlordisilan aus in Prozessabgasströmen enthaltenen Gemischen von Chlorsilanen |
PCT/DE2015/000562 WO2016091240A1 (de) | 2014-12-10 | 2015-11-20 | Verfahren zur gewinnung von hexachlordisilan aus in prozessabgasströmen enthaltenen gemischen von chlorsilanen |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3230206A1 true EP3230206A1 (de) | 2017-10-18 |
Family
ID=55174478
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP15825916.8A Withdrawn EP3230206A1 (de) | 2014-12-10 | 2015-11-20 | Verfahren zur gewinnung von hexachlordisilan aus in prozessabgasströmen enthaltenen gemischen von chlorsilanen |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP3230206A1 (de) |
KR (1) | KR20170091623A (de) |
CN (1) | CN107207267A (de) |
DE (1) | DE102014018435A1 (de) |
WO (1) | WO2016091240A1 (de) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
TWI791547B (zh) * | 2017-07-31 | 2023-02-11 | 中國大陸商南大光電半導體材料有限公司 | 製備五氯二矽烷之方法及包含五氯二矽烷之經純化的反應產物 |
WO2021164876A1 (de) | 2020-02-20 | 2021-08-26 | Wacker Chemie Ag | Verfahren zur gewinnung von hexachlordisilan durch umsetzung von mindestens einem teilhydrierten chlordisilan an einem festen, unfunktionalisierten adsorber |
CN112479212B (zh) * | 2020-12-16 | 2022-06-28 | 亚洲硅业(青海)股份有限公司 | 一种六氯乙硅烷提纯装置及方法 |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1142848B (de) | 1958-06-25 | 1963-01-31 | Wacker Chemie Gmbh | Verfahren zur Herstellung von hochreinem Siliciumhexachlorid |
DE3503262A1 (de) | 1985-01-31 | 1986-08-07 | Wacker-Chemitronic Gesellschaft für Elektronik-Grundstoffe mbH, 8263 Burghausen | Verfahren zum aufarbeiten von bei der siliciumherstellung anfallenden halogensilangemischen |
WO2002012122A1 (fr) * | 2000-08-02 | 2002-02-14 | Mitsubishi Materials Polycrystalline Silicon Corporation | Procédé de production d'hexachlorure de disilicium |
JP2006176357A (ja) * | 2004-12-22 | 2006-07-06 | Sumitomo Titanium Corp | ヘキサクロロジシランの製造方法 |
KR101341360B1 (ko) | 2006-03-07 | 2013-12-13 | 도아고세이가부시키가이샤 | Hcd 가스의 제해방법과 제해장치 |
WO2008051328A1 (en) * | 2006-10-24 | 2008-05-02 | Dow Corning Corporation | Composition comprising neopentasilane and method of preparing same |
JP4659797B2 (ja) | 2007-09-05 | 2011-03-30 | 信越化学工業株式会社 | 多結晶シリコンの製造方法 |
DE102007000841A1 (de) * | 2007-10-09 | 2009-04-16 | Wacker Chemie Ag | Verfahren zur Herstellung von hochreinem Hexachlordisilan |
EP2067745B1 (de) * | 2007-11-30 | 2017-07-12 | Mitsubishi Materials Corporation | Verfahren zum Trennen und Wiedergewinnen von Konvertierungsreaktionsgas |
DE102009053804B3 (de) * | 2009-11-18 | 2011-03-17 | Evonik Degussa Gmbh | Verfahren zur Herstellung von Hydridosilanen |
DE102010002812A1 (de) | 2010-03-12 | 2011-09-15 | Wacker Chemie Ag | Verfahren zur Entsorgung Hexachlordisilan-haltiger Dämpfe |
DE102010043648A1 (de) * | 2010-11-09 | 2012-05-10 | Evonik Degussa Gmbh | Verfahren zur selektiven Spaltung höherer Silane |
DE102010043649A1 (de) * | 2010-11-09 | 2012-05-10 | Evonik Degussa Gmbh | Verfahren zur Spaltung höherer Silane |
-
2014
- 2014-12-10 DE DE102014018435.8A patent/DE102014018435A1/de not_active Withdrawn
-
2015
- 2015-11-20 CN CN201580075776.2A patent/CN107207267A/zh active Pending
- 2015-11-20 KR KR1020177015427A patent/KR20170091623A/ko unknown
- 2015-11-20 WO PCT/DE2015/000562 patent/WO2016091240A1/de active Application Filing
- 2015-11-20 EP EP15825916.8A patent/EP3230206A1/de not_active Withdrawn
Non-Patent Citations (2)
Title |
---|
None * |
See also references of WO2016091240A1 * |
Also Published As
Publication number | Publication date |
---|---|
DE102014018435A1 (de) | 2016-06-16 |
WO2016091240A1 (de) | 2016-06-16 |
KR20170091623A (ko) | 2017-08-09 |
CN107207267A (zh) | 2017-09-26 |
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RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: SCHLEY, MICHAEL Inventor name: KATZ, MARTIN Inventor name: SCHAAFF, FRIEDRICH |
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