WO2010065287A1 - Process for producing trichlorosilane and tetrachlorosilane - Google Patents

Process for producing trichlorosilane and tetrachlorosilane Download PDF

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Publication number
WO2010065287A1
WO2010065287A1 PCT/US2009/064721 US2009064721W WO2010065287A1 WO 2010065287 A1 WO2010065287 A1 WO 2010065287A1 US 2009064721 W US2009064721 W US 2009064721W WO 2010065287 A1 WO2010065287 A1 WO 2010065287A1
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WIPO (PCT)
Prior art keywords
mixture
distillation apparatus
solids
polychlorosiloxane
polychlorosilane
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Application number
PCT/US2009/064721
Other languages
French (fr)
Inventor
Patrick James Harder
Arthur James Tselepis
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Dow Corning Corporation
Hemlock Semiconductor Corporation
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Filing date
Publication date
Application filed by Dow Corning Corporation, Hemlock Semiconductor Corporation filed Critical Dow Corning Corporation
Priority to RU2011118231/04A priority Critical patent/RU2499801C2/en
Priority to CN2009801483478A priority patent/CN102232080A/en
Priority to EP09752997A priority patent/EP2367832A1/en
Priority to US13/127,987 priority patent/US20110250116A1/en
Priority to CA2743246A priority patent/CA2743246A1/en
Publication of WO2010065287A1 publication Critical patent/WO2010065287A1/en

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    • 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

Definitions

  • This invention relates to a method for cracking high boiling polymers to improve yield and minimize waste in a process for making trichlorosilane (HSiCl 3 ).
  • the polymers include tetrachlorodisiloxane (H 2 Si 2 OCl 4 ), pentachlorodisiloxane (HSi 2 OCIs), hexachlorodisiloxane (Si 2 OCIo), and hexachlorodisilane (Si 2 CIo).
  • the cracking process produces additional HSiCl 3 and/or tetrachlorosilane (SiCl 4 ) useful in process for producing polycrystalline silicon.
  • SiCl 4 is a by-product produced when silicon is deposited on a substrate in a chemical deposition (CVD) reactor that uses a feed gas stream comprising HSiCl 3 and hydrogen (H 2 ). It is desirable to convert the SiCl 4 back to HSiCl 3 to be used in the feed gas stream.
  • CVD chemical deposition
  • One process for converting SiCl 4 back to HSiCl 3 comprises feeding H 2 and SiCl 4 to a fluidized bed reactor (FBR) having silicon particles therein.
  • the FBR operates at high pressure and temperature where the following reaction occurs.
  • Residue typically comprises polychlorosilanes and/or polychlorosiloxanes exemplified by partially hydrogenated species, including tetrachlorodisiloxane (H 2 Si 2 OCl 4 ) and pentachlorodisiloxane (HSi 2 OCIs); and other high boiling species, including hexachlorodisiloxane (Si 2 OCIo) and hexachlorodisilane (Si 2 CIo). Residue further comprises silicon particulates, which must periodically be removed. The residue is periodically pumped out and disposed of.
  • partially hydrogenated species including tetrachlorodisiloxane (H 2 Si 2 OCl 4 ) and pentachlorodisiloxane (HSi 2 OCIs); and other high boiling species, including hexachlorodisiloxane (Si 2 OCIo) and hexachlorodisilane (Si 2 CIo).
  • a process for cracking polychlorosilanes and/or polychlorosiloxanes comprises: recycling a clean mixture comprising polychlorosilanes and/or polychlorosiloxanes to a distillation apparatus; thereby producing trichlorosilane, tetrachlorosilane, or a combination thereof.
  • Figure 1 is a process flow diagram showing a process of this invention.
  • Reference Numerals
  • a process for cracking polychlorosilanes and/or polychlorosiloxanes is described herein.
  • the process may comprise: a. producing a mixture comprising a polychlorosilane and/or a polychlorosiloxane; optionally b. removing solids from the mixture to form a clean mixture; c. recycling the clean mixture to a distillation apparatus; thereby producing trichlorosilane, tetrachlorosilane, or a combination thereof.
  • Figure 1 shows a process flow diagram of an exemplary process for preparing HSiCl 3 . SiCl 4 is fed through line 101, and H 2 is fed through line 102, into a FBR 103.
  • Silicon particles are fed into the FBR through line 105 and form a fluidized bed in the FBR 103.
  • a crude product stream comprising HSiCl 3 , SiCl 4 , silicon solids, and H 2 is drawn off the top of the FBR 103 through line 107.
  • the silicon solids may be removed with a dust removing apparatus 108 such as a cyclone, and returned to the FBR 103 through line 109.
  • the resulting effluent mixture is fed to the sump 111 of a distillation column 110 through line 113.
  • the sump 111 of the distillation column 110 may contain a catalyst that facilitates cracking of the polychlorosiloxane and polychlorosilane species.
  • Some catalysts may inherently form in the sump 111 of the distillation column 110 resulting from impurities such as tin, titanium, or aluminum. Examples such catalysts include, but are not limited to, titanium dichloride, titanium trichloride, titanium tetrachloride, tin tetrachloride, tin dichloride, iron chloride, AlCl 3, and a combination thereof.
  • the amount of such catalyst depends on various factors including how frequently the residue is removed from the distillation apparatus 110 and the level of the catalyst present in the effluent mixture from the FBR 103.
  • a catalyst can be added to the sump 111.
  • Platinum group metal catalysts such as platinum, palladium, osmium, iridium, or heterogeneous compounds thereof can be used.
  • the platinum group metal catalysts may optionally be supported on substrates such as carbon or alumina.
  • the amount of catalyst may vary depending on the type of catalyst and the factors described above, however, the amount may range from 0 to 20 %, alternatively 0 to 10 % of the residue.
  • One skilled in the art would recognize that different catalysts have different catalytic activities and would be able to select an appropriate catalyst and amount thereof based on the process conditions in the distillation apparatus 110 and the sump 111.
  • a mixture including SiCl 4 , HSiCl 3 , and H 2 is removed from the top of the distillation column 110 through line 115.
  • the SiCl 4 and H 2 may be recovered and fed back to the FBR 103, as described above.
  • the HSiCl 3 may optionally be used as a feed gas for a CVD reactor (not shown) for the production of polycrystalline silicon.
  • Residue is generated in the FBR 103 along with the intended product HSiCl 3 . Residue, which is heavier than SiCl 4 , accumulates in the sump 111. The residue is periodically removed through line 117.
  • Residue typically comprises a polychlorosilane and/or a polychlorosiloxane.
  • Such polychlorosilanes and polychlorosiloxanes are exemplified by partially hydrogenated species, including tetrachlorodisiloxane (H 2 Si 2 OCl 4 ) and pentachlorodisiloxane (HSi 2 OCIs); and other high boiling species, including hexachlorodisiloxane (Si 2 OCIo) and hexachlorodisilane (Si 2 CIo).
  • the exact amount of each species of polychlorosilane and polychlorosiloxane in the residue may vary depending on the process chemistry and conditions that produce the residue.
  • residue may contain 0 to 15 % H 2 Si 2 OCl 4 , 5 % to 35 % HSi 2 OCl 5 , 15 % to 25 % Si 2 OCl 6 , and 35 % to 75 % Si 2 Cl 6 , based on the combined weights of the polychlorosilanes and polychlorosiloxanes in the residue.
  • Residue may further comprise solids, which are insoluble in the species described above.
  • the solids may be polychlorosiloxanes having 4 or more silicon atoms and higher order polychlorosilanes.
  • the solids may further comprise silicon particulates, which may optionally be recovered as described below and optionally recycled to the FBR 103.
  • the residue may be fed to a solids removing apparatus 119.
  • the solids may be removed through line 121.
  • the clean mixture i.e., the mixture comprising tetrachlorodisiloxane, pentachlorodisiloxane, hexachlorodisiloxane, and hexachlorodisilane with the solids removed
  • Figure 1 is intended to illustrate the invention to one of ordinary skill in the art and should not be interpreted to limit the scope of the invention set forth in the claims. Modifications may be made to Figure 1 by one of ordinary skill in the art and still embody the invention.
  • cyclone 108 is optional and that one or more of the feeds in lines 101, 102, and 105 may optionally be combined before being fed into the FBR 103.
  • the distillation column 110 can have a different configuration than that shown in Figure 1, e.g., a separate reboiler into which gas from line 113 is fed may be used instead of the sump 111. The residue would then accumulate in the reboiler.
  • an alternative process for producing HSiCl 3 may be used, for example, an alternative FBR 103 that produces HSiCl 3 from HCl and particulate silicon.
  • Cracking reactions of the polychlorosilane and/or polychlorosiloxane species in the clean mixture can form monomeric chlorosilane species (HSiCl 3 and SiCl 4 ) and higher order silane and siloxane polymers with each successive reaction of the species in the clean mixture.
  • the siloxane polymers become large enough to form solids at approximately 4 units long.
  • polychlorosilanes undergo cracking reactions, similarly.
  • the partially hydrogenated species described above exhibit equilibria with HSiCl 3
  • the other (not hydrogenated) species described above exhibit equilibria with SiCl 4 according to the following reactions:
  • H n Si 2 OCIo-Ii ⁇ H n-1 Si 3 O 2 CIg-Ii + HSiCl 3 where subscript n represents the number of hydrogen atoms, e.g., 1 or 2, Si 2 OCl 6 ⁇ Si 3 O 2 Cl 8 + SiCl 4 .
  • n represents the number of hydrogen atoms, e.g., 1 or 2, Si 2 OCl 6 ⁇ Si 3 O 2 Cl 8 + SiCl 4 .
  • the sump 111 may operate at 130 0 C to 280 0 C, alternatively to 180 0 C to 240 0 C, and alternatively 200 0 C to 220 0 C, for a residence time ranging from 10 days to 1 hour at a pressure ranging from 25 bar to 40 bar.
  • the residence time selected depends on various factors including the temperature and the presence or absence of a catalyst.
  • the pressure may be selected based on practical limitations. Increasing pressure will increase the boiling temperatures in the distillation apparatus. The range of pressures enable the reaction to occur at the appropriate temperatures, and therefore at sufficient rate.

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

Abstract

A process for reducing waste and increasing yield of chlorosilane monomers is performed by cracking polychlorosiloxane and polychlorosilane by-products generated during production of trichlorosilane useful for the manufacture of polycrystalline silicon.

Description

PROCESS FOR PRODUCING TRICHLOROS ILANE AND TETRACHLOROS ILANE
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Patent Application No. 61/119,391 filed on 3 December 2008. U.S. Provisional Patent Application No. 61/119,391 is hereby incorporated by reference.
STATEMENT REGARDING FEDERALLY FUNDED RESEARCH [0002] None.
BACKGROUND Technical Field
[0003] This invention relates to a method for cracking high boiling polymers to improve yield and minimize waste in a process for making trichlorosilane (HSiCl3). The polymers include tetrachlorodisiloxane (H2Si2OCl4), pentachlorodisiloxane (HSi2OCIs), hexachlorodisiloxane (Si2OCIo), and hexachlorodisilane (Si2CIo). The cracking process produces additional HSiCl3 and/or tetrachlorosilane (SiCl4) useful in process for producing polycrystalline silicon.
Problem to be Solved
[0004] SiCl4 is a by-product produced when silicon is deposited on a substrate in a chemical deposition (CVD) reactor that uses a feed gas stream comprising HSiCl3 and hydrogen (H2). It is desirable to convert the SiCl4 back to HSiCl3 to be used in the feed gas stream. One process for converting SiCl4 back to HSiCl3 comprises feeding H2 and SiCl4 to a fluidized bed reactor (FBR) having silicon particles therein. The FBR operates at high pressure and temperature where the following reaction occurs.
3 SiCl4 + 2 H2 + Si ^ 4 HSiCl3 [0005] Partial conversion of the H2 and SiCl4 to HSiCl3 is achieved due to equilibrium limitations. H2 is separated from the chlorosilanes and is recycled back to the feed. Likewise, unconverted SiCl4 is distilled from the product HSiCl3 and is recycled. Product HSiCl3 may be further distilled to remove impurities. [0006] Residue is generated in the FBR along with the intended product HSiCl3. Residue, which is heavier than SiCl4, accumulates in the bottoms from the distillation apparatus. Residue typically comprises polychlorosilanes and/or polychlorosiloxanes exemplified by partially hydrogenated species, including tetrachlorodisiloxane (H2Si2OCl4) and pentachlorodisiloxane (HSi2OCIs); and other high boiling species, including hexachlorodisiloxane (Si2OCIo) and hexachlorodisilane (Si2CIo). Residue further comprises silicon particulates, which must periodically be removed. The residue is periodically pumped out and disposed of.
[0007] One approach for converting polychlorosilanes and polychlorosiloxanes has been proposed in which these species are fed back to the FBR for making HSiCl3. However, it is thought that this process may not be industrially desirable because of limitations presented by reaction kinetics at typical reactor temperatures unless considerable recycle passes are undertaken. This process is also complicated by the interference of the recycle stream with hydrodynamics in the reactor and the intended HSiCl3 generating reaction itself.
SUMMARY
[0008] A process for cracking polychlorosilanes and/or polychlorosiloxanes comprises: recycling a clean mixture comprising polychlorosilanes and/or polychlorosiloxanes to a distillation apparatus; thereby producing trichlorosilane, tetrachlorosilane, or a combination thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] Figure 1 is a process flow diagram showing a process of this invention. Reference Numerals
101 SiCl4 feed line 111 sump
102 H2 feed line 113 distillation feed line
103 fluidized bed reactor 115 overheads mixture removal line
105 silicon particle feed line 117 residue removal line
107 crude product line 119 solids removing apparatus
108 dust removing apparatus 121 solids removal line
109 silicon particle recycle line 123 clean mixture line
110 distillation column DETAILED DESCRIPTION
[0010] A process for cracking polychlorosilanes and/or polychlorosiloxanes is described herein. The process may comprise: a. producing a mixture comprising a polychlorosilane and/or a polychlorosiloxane; optionally b. removing solids from the mixture to form a clean mixture; c. recycling the clean mixture to a distillation apparatus; thereby producing trichlorosilane, tetrachlorosilane, or a combination thereof. [0011] Figure 1 shows a process flow diagram of an exemplary process for preparing HSiCl3. SiCl4 is fed through line 101, and H2 is fed through line 102, into a FBR 103. Silicon particles are fed into the FBR through line 105 and form a fluidized bed in the FBR 103. A crude product stream comprising HSiCl3, SiCl4, silicon solids, and H2 is drawn off the top of the FBR 103 through line 107. The silicon solids may be removed with a dust removing apparatus 108 such as a cyclone, and returned to the FBR 103 through line 109. The resulting effluent mixture is fed to the sump 111 of a distillation column 110 through line 113.
[0012] The sump 111 of the distillation column 110 may contain a catalyst that facilitates cracking of the polychlorosiloxane and polychlorosilane species. Some catalysts may inherently form in the sump 111 of the distillation column 110 resulting from impurities such as tin, titanium, or aluminum. Examples such catalysts include, but are not limited to, titanium dichloride, titanium trichloride, titanium tetrachloride, tin tetrachloride, tin dichloride, iron chloride, AlCl3, and a combination thereof. The amount of such catalyst depends on various factors including how frequently the residue is removed from the distillation apparatus 110 and the level of the catalyst present in the effluent mixture from the FBR 103. Alternatively, a catalyst can be added to the sump 111. Platinum group metal catalysts such as platinum, palladium, osmium, iridium, or heterogeneous compounds thereof can be used. The platinum group metal catalysts may optionally be supported on substrates such as carbon or alumina. The amount of catalyst may vary depending on the type of catalyst and the factors described above, however, the amount may range from 0 to 20 %, alternatively 0 to 10 % of the residue. One skilled in the art would recognize that different catalysts have different catalytic activities and would be able to select an appropriate catalyst and amount thereof based on the process conditions in the distillation apparatus 110 and the sump 111. [0013] A mixture including SiCl4, HSiCl3, and H2 is removed from the top of the distillation column 110 through line 115. The SiCl4 and H2 may be recovered and fed back to the FBR 103, as described above. The HSiCl3 may optionally be used as a feed gas for a CVD reactor (not shown) for the production of polycrystalline silicon. [0014] Residue is generated in the FBR 103 along with the intended product HSiCl3. Residue, which is heavier than SiCl4, accumulates in the sump 111. The residue is periodically removed through line 117. Residue typically comprises a polychlorosilane and/or a polychlorosiloxane. Such polychlorosilanes and polychlorosiloxanes are exemplified by partially hydrogenated species, including tetrachlorodisiloxane (H2Si2OCl4) and pentachlorodisiloxane (HSi2OCIs); and other high boiling species, including hexachlorodisiloxane (Si2OCIo) and hexachlorodisilane (Si2CIo). The exact amount of each species of polychlorosilane and polychlorosiloxane in the residue may vary depending on the process chemistry and conditions that produce the residue.
However, residue may contain 0 to 15 % H2Si2OCl4, 5 % to 35 % HSi2OCl5, 15 % to 25 % Si2OCl6, and 35 % to 75 % Si2Cl6, based on the combined weights of the polychlorosilanes and polychlorosiloxanes in the residue. Residue may further comprise solids, which are insoluble in the species described above. For example, the solids may be polychlorosiloxanes having 4 or more silicon atoms and higher order polychlorosilanes. The solids may further comprise silicon particulates, which may optionally be recovered as described below and optionally recycled to the FBR 103. [0015] The residue may be fed to a solids removing apparatus 119. The solids may be removed through line 121. The clean mixture (i.e., the mixture comprising tetrachlorodisiloxane, pentachlorodisiloxane, hexachlorodisiloxane, and hexachlorodisilane with the solids removed) may be sent through line 123 back to the sump 111.
[0016] Figure 1 is intended to illustrate the invention to one of ordinary skill in the art and should not be interpreted to limit the scope of the invention set forth in the claims. Modifications may be made to Figure 1 by one of ordinary skill in the art and still embody the invention. For example, one skilled in the art would recognize that cyclone 108 is optional and that one or more of the feeds in lines 101, 102, and 105 may optionally be combined before being fed into the FBR 103. One skilled in the art would recognize that the distillation column 110 can have a different configuration than that shown in Figure 1, e.g., a separate reboiler into which gas from line 113 is fed may be used instead of the sump 111. The residue would then accumulate in the reboiler.
Furthermore, an alternative process for producing HSiCl3 may be used, for example, an alternative FBR 103 that produces HSiCl3 from HCl and particulate silicon. [0017] Cracking reactions of the polychlorosilane and/or polychlorosiloxane species in the clean mixture can form monomeric chlorosilane species (HSiCl3 and SiCl4) and higher order silane and siloxane polymers with each successive reaction of the species in the clean mixture. The siloxane polymers become large enough to form solids at approximately 4 units long. Under the conditions in the distillation apparatus, polychlorosilanes undergo cracking reactions, similarly. The partially hydrogenated species described above exhibit equilibria with HSiCl3, and the other (not hydrogenated) species described above, exhibit equilibria with SiCl4 according to the following reactions:
HnSi2OCIo-Ii <→ Hn-1Si3O2CIg-Ii + HSiCl3, where subscript n represents the number of hydrogen atoms, e.g., 1 or 2, Si2OCl6 <→ Si3O2Cl8 + SiCl4. When the polychlorosiloxanes reach a degree of polymerization of 4 or greater, a solid may form and the reaction may become irreversible, as illustrated below: HnSi3O2Cl8-D → Hn-i Si4O3Cl10-D(SoHd) + HSiCl3, and Si3O2Cl8 → Si4O3Cl10(SoHd) + SiCl4. Based on the kinetic data, the reactions above all occur at different rates in the sump 111 to permit the above equilibria to be reached within the residence time for the species in the sump 111 when the clean mixture is recycled. The sump 111 may operate at 130 0C to 280 0C, alternatively to 180 0C to 240 0C, and alternatively 200 0C to 220 0C, for a residence time ranging from 10 days to 1 hour at a pressure ranging from 25 bar to 40 bar. One skilled in the art would recognize that the residence time selected depends on various factors including the temperature and the presence or absence of a catalyst. The pressure may be selected based on practical limitations. Increasing pressure will increase the boiling temperatures in the distillation apparatus. The range of pressures enable the reaction to occur at the appropriate temperatures, and therefore at sufficient rate.
Industrial Applicability
[0018] The process described herein reduces waste and improves yield of chlorosilane monomers (HSiCl3 and SiCl4) useful for the production of polycrystalline silicon. Polychlorosilanes and polychlorosiloxanes that otherwise would have been disposed of as waste are cracked to form useful HSiCl3 and SiCl4.

Claims

1. A process comprises: step a) recycling a clean mixture comprising a polychlorosilane and/or a polychlorosiloxane to a distillation apparatus and cracking the polychlorosilane and/or polychlorosiloxane; thereby producing trichlorosilane, tetrachlorosilane, or a combination thereof.
2. The process of claim 1, where the clean mixture is obtained by a method comprising: b) producing a mixture comprising a polychlorosilane and/or a polychlorosiloxane; and optionally c) removing solids from the mixture to form the clean mixture.
3. The process of claim 1, where the clean mixture is recycled to a sump of the distillation apparatus.
4. The process of claim 1, where the clean mixture is recycled to a reboiler of a distillation apparatus.
5. The process of claim 1, where step c) is present, and the solids are recycled to a fluidized bed reactor for making trichlorosilane.
6. The process of claim 1, where the polychlorosilane is selected from the group consisting of hexachlorodisilane, pentachlorodisilane, tetrachlorodisilane, and a combination thereof.
7. The process of claim 1, where the polychlorosiloxane is selected from the group consisting of tetrachlorodisiloxane, pentachlorodisiloxane, hexachlorodisiloxane, and a combination thereof.
8. The process of claim 1, where the distillation apparatus operates at a temperature ranging from 130 0C to 280 0C when the residence time ranges from 10 days to 1 hour at a pressure ranging from 25 bar to 40 bar.
9. The process of claim 2, where the process further comprises: d) feeding an effluent from a fluidized bed reactor producing trichlorosilane to the distillation apparatus before step b).
10. The process of claim 9, where the effluent is a crude product stream comprising tetrachlorosilane, trichlorosilane, silicon solids, and hydrogen.
11. The process of claim 9, where the process further comprises: e) removing silicon solids from the effluent before step d).
12. The process of claim 1, where a catalyst is in the reboiler.
13. The process of claim 12, where the catalyst is selected from the group consisting of a chloride of titanium, tin, aluminum, or a combination thereof.
14. The process of claim 12, where the catalyst comprises a platinum group metal.
PCT/US2009/064721 2008-12-03 2009-11-17 Process for producing trichlorosilane and tetrachlorosilane WO2010065287A1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
RU2011118231/04A RU2499801C2 (en) 2008-12-03 2009-11-17 Method of producing trichlorosilane and tetrachlorosilane
CN2009801483478A CN102232080A (en) 2008-12-03 2009-11-17 Process for producing trichlorosilane and tetrachlorosilane
EP09752997A EP2367832A1 (en) 2008-12-03 2009-11-17 Process for producing trichlorosilane and tetrachlorosilane
US13/127,987 US20110250116A1 (en) 2008-12-03 2009-11-17 Process for Producing Trichlorosilane and Tetrachlorosilane
CA2743246A CA2743246A1 (en) 2008-12-03 2009-11-17 Process for producing trichlorosilane and tetrachlorosilane

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US11939108P 2008-12-03 2008-12-03
US61/119,391 2008-12-03

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EP (1) EP2367832A1 (en)
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CN (1) CN102232080A (en)
CA (1) CA2743246A1 (en)
RU (1) RU2499801C2 (en)
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