JP5639047B2 - ハロゲン化ポリシラン及びその製造のための熱処理 - Google Patents
ハロゲン化ポリシラン及びその製造のための熱処理 Download PDFInfo
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- JP5639047B2 JP5639047B2 JP2011510824A JP2011510824A JP5639047B2 JP 5639047 B2 JP5639047 B2 JP 5639047B2 JP 2011510824 A JP2011510824 A JP 2011510824A JP 2011510824 A JP2011510824 A JP 2011510824A JP 5639047 B2 JP5639047 B2 JP 5639047B2
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- polysilane
- chlorinated
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
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Description
DE 10 2005 024 041 A1、DE 10 2006 034 061 A1、WO 2008/031427 A2、WO 81/03168、US 2005/0142046 A1、M. Schmeisser, P. Voss "Ueber das Siliciumdichlorid [SiCl2]x" [Concerning silicon dichloride [SiCl2]x], Z. anorg. allg. Chem. (1964) 334, 50〜56頁、US2007/0078252A1、DE 31 26 240 C2、GB 702,349、R. Schwarz and H. Meckbach "Ueber ein Siliciumchlorid der Formel Si10Cl22" [Concerning a silicon chloride of the formula Si10Cl22], Z. anorg. allg. Chem. (1937) 232, 241〜248頁。
PCSは、例えばM. Schmeisser, P. Voss "Ueber das Siliciumdichlorid [SiCl2]x", Z. anorg. allg. Chem. (1964) 334, 50〜56頁 (Schmeisser 1964)に記載されているように、純粋な熱反応によって生成できる一方、還元剤(Si, H2)とともに揮発性のハロシランを比較的高温(700°Cより大きい)に加熱することで生成可能である。得られたハロゲン化ポリシランはわずかに緑がかった黄色で、ガラス質の高分子である。さらに、前記文献の混合物は、その生成に起因し、AlCl3で強烈に汚染されている。
1.ナトリウムで還元され、その後、HCl/AlCl3芳香族で分裂されるべきハロゲン化アリルオリゴシラン
2.アリル化H-シランの遷移金属触媒による脱水素重合及びこの後のHCl/AlCl3での脱アリル化
3.TBAF (Bu4NF)での(SiCl2)5の陰イオン触媒による開環重合(ROP)
4.TBAF 又は Ph3SiKでの(SiAr2)5のROP及びこの後のHCl/AlCl3での脱アリル化
Claims (12)
- 少なくとも一つの直接Si-Si結合を有し、その置換基が塩素からなり、且つ、成分中、置換基:シリコンの原子比が少なくとも1:1である純粋化合物又は化合物の混合物としての塩素化ポリシランにおいて、
前記ポリシランは、高比率の分枝部位を備えた環式且つ鎖式からなり、
前記分岐部位が総生産混合物を基準に1%より大きいとともに、1よりも小さいI100/I132のラマン分子振動スペクトルを有し、ここで、
I100は100 cm-1でのラマン強度を示し、
I132は132 cm-1でのラマン強度を示し、
29Si NMR スペクトルにて、その重要な生産物信号が+23 ppm 〜 -13 ppm, -18 ppm 〜 -33 ppm 及び -73 ppm 〜 -93 ppmの化学シフト領域中にあることを特徴とする塩素化ポリシラン。 - 主に分枝鎖を含むことを特徴とする請求項1の塩素化ポリシラン。
- 置換基が塩素のみから成っていることを特徴とする請求項1又は2の塩素化ポリシラン。
- 塩素化ポリシランの生成されたままの混合物の平均鎖長はn = 3〜9に相当することを特徴とする請求項1〜3のいずれかの塩素化ポリシラン。
- 粘性に関しては油性であることを特徴とする請求項1〜4のいずれかの塩素化ポリシラン。
- わずかな黄色から強いオレンジ又は赤褐色を有していることを特徴とする請求項1〜5のいずれかの塩素化ポリシラン。
- 不活性溶媒中に容易に溶けることを特徴とする請求項1〜6のいずれかの塩素化ポリシラン。
- 水素置換基を含んでいないことを特徴とする請求項1,2、又は4〜7のいずれかの塩素化ポリシラン。
- 塩素化シランは700°Cを超える温度でシリコンと反応し、この反応が形成されたジクロロシリレン(SiCl 2 )に対して過剰な塩素化シランのもとで実行されることを特徴とする請求項1〜8のいずれかの塩素化ポリシランの製造方法。
- 使用されたシリコン充填ベッド中の塩素化シランの保持時間がシリコンの粒度で調節されることを特徴とする請求項9の方法。
- 0.1〜1000 hPaの圧力範囲で実行されることを特徴とする請求項9又は請求項10の方法。
- 塩素化ポリシランが沈殿すべき反応器部分の温度が-70°C 〜 300°Cに維持されていることを特徴とする請求項9〜11のいずれかの方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102008025260A DE102008025260B4 (de) | 2008-05-27 | 2008-05-27 | Halogeniertes Polysilan und thermisches Verfahren zu dessen Herstellung |
DE102008025260.3 | 2008-05-27 | ||
PCT/DE2009/000727 WO2009143824A1 (de) | 2008-05-27 | 2009-05-27 | Halogeniertes polysilan und thermisches verfahren zu dessen herstellung |
Publications (2)
Publication Number | Publication Date |
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JP2011523926A JP2011523926A (ja) | 2011-08-25 |
JP5639047B2 true JP5639047B2 (ja) | 2014-12-10 |
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JP2011510824A Expired - Fee Related JP5639047B2 (ja) | 2008-05-27 | 2009-05-27 | ハロゲン化ポリシラン及びその製造のための熱処理 |
Country Status (14)
Country | Link |
---|---|
US (1) | US9617391B2 (ja) |
EP (1) | EP2296804B1 (ja) |
JP (1) | JP5639047B2 (ja) |
KR (1) | KR101659098B1 (ja) |
CN (1) | CN102099104B (ja) |
AU (1) | AU2009253523B2 (ja) |
BR (1) | BRPI0912045B1 (ja) |
CA (1) | CA2725366C (ja) |
DE (1) | DE102008025260B4 (ja) |
IL (1) | IL209578A0 (ja) |
MX (1) | MX2010012992A (ja) |
RU (1) | RU2502554C2 (ja) |
UA (1) | UA102545C2 (ja) |
WO (1) | WO2009143824A1 (ja) |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
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DE102008042934A1 (de) * | 2008-10-17 | 2010-04-22 | Wacker Chemie Ag | Verfahren zur Herstellung von Neopentasilanen |
DE102009027194A1 (de) * | 2009-06-25 | 2010-12-30 | Wacker Chemie Ag | Verfahren zur Herstellung von Dodecahalogenneopentasilanen |
DE102009056436B4 (de) | 2009-12-02 | 2013-06-27 | Spawnt Private S.À.R.L. | Chloridhaltiges Silicium |
DE102009056438B4 (de) | 2009-12-02 | 2013-05-16 | Spawnt Private S.À.R.L. | Verfahren zur Herstellung von Hexachlordisilan |
DE102009056731A1 (de) * | 2009-12-04 | 2011-06-09 | Rev Renewable Energy Ventures, Inc. | Halogenierte Polysilane und Polygermane |
JP2013527831A (ja) | 2010-05-05 | 2013-07-04 | シュパウント プライベート ソシエテ ア レスポンサビリテ リミテ | 新規な前駆体から生成されたナノワイヤおよびその製造方法 |
DE102010045260A1 (de) * | 2010-09-14 | 2012-03-15 | Spawnt Private S.À.R.L. | Verfahren zur Herstellung von fluorierten Polysilanen |
DE102010043646A1 (de) * | 2010-11-09 | 2012-05-10 | Evonik Degussa Gmbh | Verfahren zur Herstellung von Trichlorsilan |
DE102014203810A1 (de) * | 2014-03-03 | 2015-09-03 | Evonik Degussa Gmbh | Verfahren zur Herstellung reiner Octachlortrisilane und Decachlortetrasilane |
DE102014007767A1 (de) | 2014-05-21 | 2015-11-26 | Psc Polysilane Chemicals Gmbh | Verfahren und Vorrichtung zur Herstellung halogenierter Oligosilane aus Silicium und Tetrachlorsilan |
DE102014007766A1 (de) | 2014-05-21 | 2015-11-26 | Psc Polysilane Chemicals Gmbh | Verfahren zur plasmachemischen Herstellung halogenierter Oligosilane aus Tetrachlorsilan |
DE102014109275A1 (de) | 2014-07-02 | 2016-01-07 | Spawnt Private S.À.R.L. | Verfahren zur Herstellung von Nanopartikeln, Nanopartikel und deren Verwendung |
KR20170035981A (ko) | 2014-07-22 | 2017-03-31 | 모멘티브 퍼포먼스 머티리얼즈 게엠베하 | 모노실란, 폴리실란, 및/또는 올리고실란에서 규소-규소 결합 및/또는 규소-염소 결합의 분해 방법 |
EP3088359B1 (de) * | 2015-04-28 | 2018-09-12 | Evonik Degussa GmbH | Verfahren zur herstellung von octachlortrisilan und höherer polychlorsilane unter verwertung von hexachlordisilan |
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2008
- 2008-05-27 DE DE102008025260A patent/DE102008025260B4/de not_active Expired - Fee Related
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- 2009-05-27 MX MX2010012992A patent/MX2010012992A/es active IP Right Grant
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- 2009-05-27 US US12/995,174 patent/US9617391B2/en not_active Expired - Fee Related
- 2009-05-27 KR KR1020107029330A patent/KR101659098B1/ko not_active Application Discontinuation
- 2009-05-27 RU RU2010152678/05A patent/RU2502554C2/ru not_active IP Right Cessation
- 2009-05-27 CN CN200980119335.2A patent/CN102099104B/zh not_active Expired - Fee Related
- 2009-05-27 EP EP09753540.5A patent/EP2296804B1/de not_active Revoked
- 2009-05-27 JP JP2011510824A patent/JP5639047B2/ja not_active Expired - Fee Related
- 2009-05-27 WO PCT/DE2009/000727 patent/WO2009143824A1/de active Application Filing
- 2009-05-27 BR BRPI0912045-9A patent/BRPI0912045B1/pt not_active IP Right Cessation
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Also Published As
Publication number | Publication date |
---|---|
EP2296804B1 (de) | 2014-03-12 |
CA2725366A1 (en) | 2009-12-03 |
CN102099104A (zh) | 2011-06-15 |
KR20110040784A (ko) | 2011-04-20 |
CA2725366C (en) | 2017-07-18 |
US9617391B2 (en) | 2017-04-11 |
JP2011523926A (ja) | 2011-08-25 |
BRPI0912045A2 (pt) | 2016-01-05 |
CN102099104B (zh) | 2014-08-27 |
RU2010152678A (ru) | 2012-07-10 |
EP2296804A1 (de) | 2011-03-23 |
MX2010012992A (es) | 2011-05-30 |
AU2009253523A1 (en) | 2009-12-03 |
UA102545C2 (ru) | 2013-07-25 |
DE102008025260B4 (de) | 2010-03-18 |
IL209578A0 (en) | 2011-01-31 |
AU2009253523B2 (en) | 2015-09-03 |
RU2502554C2 (ru) | 2013-12-27 |
US20110284796A1 (en) | 2011-11-24 |
BRPI0912045B1 (pt) | 2017-10-17 |
WO2009143824A1 (de) | 2009-12-03 |
DE102008025260A1 (de) | 2009-12-17 |
KR101659098B1 (ko) | 2016-09-22 |
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