JP5260048B2 - シラン処理されたシリカ - Google Patents
シラン処理されたシリカ Download PDFInfo
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- JP5260048B2 JP5260048B2 JP2007501142A JP2007501142A JP5260048B2 JP 5260048 B2 JP5260048 B2 JP 5260048B2 JP 2007501142 A JP2007501142 A JP 2007501142A JP 2007501142 A JP2007501142 A JP 2007501142A JP 5260048 B2 JP5260048 B2 JP 5260048B2
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- silica
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- structurally modified
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- vinyl
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3081—Treatment with organo-silicon 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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
- Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
- Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
- Y10T428/2995—Silane, siloxane or silicone coating
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Description
BET表面積m2/g:25〜400、
平均一次粒径nm:5〜50、
pH:3〜10、
炭素含量%:0.1〜10、
DBP値%:200未満または測定不可能
を有することを特徴とする、シラン処理され、構造的に変性されたシリカを提供する。
2)DIN ISO 787/XI、JIS K 5101/18(スクリーニングされていない)に関連して
3)DIN ISO 787/11、 ASTM D 280、 JIS K 5101/21に関連して
4)DIN 55921、 ASTM D 1208、 JIS K 5101/23に関連して
5)DIN ISO 787/IX、 ASTM D 1208、 JIS K 5101/24に関連して
6)DIN ISO 787/XVIII、JIS K 5101/20に関連して
7)105℃で2時間乾燥された物質に基づいて
8)1000℃で2時間アニールされた物質に基づいて
9)特殊な湿分排除パッケージング
10)灼熱減量成分中でのHCl成分。
LSR(liquid silicone rubber)の試験は、本発明による実施例1〜3に記載の構造変性された疎水性酸化物が、疎水性出発物質(熱分解法シリカ)と比較して液状シリコーン中で顕著に低い粘度を生じることを示す。
熱分解法シリカをミキサー中に装入し、これにまず水を、次いで表面変性剤または表面変性剤の混合物を噴霧した。次に、この反応混合物を、一段階または多段階の熱処理にさらした。この状態調節された材料を、ボールミルで構造変性し、引続き必要な場合に歯付きディスクミルで後粉砕した。構造変性されたかまたは構造変性されかつ後粉砕された材料を、必要な場合にさらに熱処理にさらした。
A=ビニルトリエトキシシラン、
B=ヘキサメチルジシラザン、
C=1,3−ジビニル−1,1,3,3−テトラメチルジシラザン
D=メチルトリメトキシシラン
1つ以上のSMを使用する場合には、配合物を使用する。
**)Post-grinding=構造変性後に微粉砕
***)Heat treatment=後微粉砕後の熱処理
比較シリカの製造
アエロジル(AEROSIL (R))2kgをミキサー中に装入し、混合しながら、最初に水0.1kgを、次いでヘキサメチルジシラザン0.4kgとビニルトリエトキシシラン0.17kgとの混合物を噴霧した。噴霧を完了した後に、混合をさらに15分間続け、反応混合物を、まず50℃で5時間、次いで140℃で1時間状態調節した。
第2表からの生成物をLSRシリコーン調製物の形で試験した。構造変性のために使用した疎水性出発物質を、比較材料として使用した。
シリカ20%をオルガノポリシロキサン(Silopren U 10 GE Bayer)中に高速遊星ミキサーで低速(50/500rpm 遊星ミキサー/高速ミキサー)で混入した。
前記シリカが完全に湿潤された後に、約200mbarの真空をかけ、この混合物を100rpmの速度(遊星ミキサー)で30分間、および2000rpmの速度(高速ミキサー)で分散させた(水道水で冷却)。冷却後に、この基本混合物は架橋させることができた。
混合物4×50gまたは2×100gが2mmの加硫物を加硫させるために必要であった。次に、シートをプレス機中で100バールの圧力下および120℃の温度で10分間圧縮した。混合物120gは、6mmの加硫物を加硫させるために必要であった。シートをプレス機中で100バールの圧力下および120℃の温度で12分間圧縮した。更に、加硫物を炉内で200℃で4時間、後加硫させた。
Claims (5)
- シラン処理され、構造的に変性されたシリカの製造法において、
a)熱分解法により製造されたシリカを噴霧の形の表面変性剤で処理し、この場合この変性剤は、ビニル基またはビニルシリル基、ならびにトリメチルシリル、ジメチルシリル、モノメチルシリルまたはこれらの混合物から選択された疎水性基をシリカの表面に固着させるのに適しており、
b)表面変性剤で変性されたシリカを熱処理し、
c)熱処理され、表面変性剤で変性されたシリカを機械的作用によって構造的に変性し、低構造化され、表面変性剤で変性された熱分解法シリカを形成させ、
d)構造的に変性されたシリカを後微粉砕および熱処理し、および
e)微粉砕され、熱処理され、シラン処理され、構造的に変性されたシリカを回収し、この場合このシリカは、このシリカの表面に固着された、ビニル基またはビニルシリル基、ならびにトリメチルシリル、ジメチルシリル、モノメチルシリルまたはこれらの混合物から選択された疎水性基を有することを特徴とする、シラン処理され、構造的に変性されたシリカの製造法。 - シリカの処理工程がシリカを最初に水で噴霧し、次に表面変性剤で噴霧することを含む、請求項1記載のシラン処理され、構造的に変性されたシリカの製造法。
- さらに熱処理工程b)の前に、さらに、処理されたシリカ混合物を混合する、請求項2記載のシラン処理され、構造的に変性されたシリカの製造法。
- 請求項1の記載により製造された、シラン処理され、構造的に変性されたシリカにおいて、このシリカの表面がこのシリカの表面に固着された、ビニル基またはビニルシリル基、ならびにトリメチルシリル、ジメチルシリル、モノメチルシリルまたはこれらの混合物から選択された疎水性基を有し、次の物理化学的性質:
BET表面積m2/g:25〜400、
平均一次粒径nm:5〜50、
pH:3〜10、
炭素含量%:0.1〜10、
DBP値%:200未満または測定不可能
を有することを特徴とする、請求項1の記載により製造された、シラン処理され、構造的に変性されたシリカ。 - 請求項4記載のシラン処理され、構造的に変性されたシリカを充填剤として含有するシリコーンゴム。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102004010756A DE102004010756A1 (de) | 2004-03-05 | 2004-03-05 | Silanisierte Kieselsäuren |
DE102004010756.4 | 2004-03-25 | ||
PCT/EP2005/001229 WO2005095525A1 (en) | 2004-03-05 | 2005-02-08 | Silanised silicas |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2007526374A JP2007526374A (ja) | 2007-09-13 |
JP5260048B2 true JP5260048B2 (ja) | 2013-08-14 |
Family
ID=34877407
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2007501142A Expired - Fee Related JP5260048B2 (ja) | 2004-03-05 | 2005-02-08 | シラン処理されたシリカ |
Country Status (9)
Country | Link |
---|---|
US (1) | US7713626B2 (ja) |
EP (1) | EP1730240B1 (ja) |
JP (1) | JP5260048B2 (ja) |
KR (1) | KR20060127172A (ja) |
CN (2) | CN103819942B (ja) |
DE (1) | DE102004010756A1 (ja) |
ES (1) | ES2649263T3 (ja) |
TW (1) | TWI304068B (ja) |
WO (1) | WO2005095525A1 (ja) |
Families Citing this family (37)
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DE102004010755A1 (de) * | 2004-03-05 | 2005-09-22 | Degussa Ag | Silikonkautschuk |
DE602005009343D1 (de) | 2005-06-25 | 2008-10-09 | Evonik Degussa Gmbh | Thermoplastische Matrix enthaltend silanisierte pyrogene Kieselsäure |
US8480889B2 (en) | 2006-04-27 | 2013-07-09 | Agilent Technologies, Inc. | Chromatographic stationary phase |
US8455165B2 (en) | 2006-09-15 | 2013-06-04 | Cabot Corporation | Cyclic-treated metal oxide |
US8435474B2 (en) * | 2006-09-15 | 2013-05-07 | Cabot Corporation | Surface-treated metal oxide particles |
US20080070146A1 (en) * | 2006-09-15 | 2008-03-20 | Cabot Corporation | Hydrophobic-treated metal oxide |
US8202502B2 (en) | 2006-09-15 | 2012-06-19 | Cabot Corporation | Method of preparing hydrophobic silica |
US7534352B2 (en) | 2007-05-01 | 2009-05-19 | Agilent Technologies, Inc. | Reversed endcapping and bonding of chromatographic stationary phases using hydrosilanes |
DE102007024099A1 (de) * | 2007-05-22 | 2008-11-27 | Evonik Degussa Gmbh | Klebstoffe |
DE102007024365A1 (de) * | 2007-05-22 | 2008-11-27 | Evonik Degussa Gmbh | Pyrogen hergestellte silanisierte und vermahlene Kieselsäure |
DE102007024100A1 (de) * | 2007-05-22 | 2008-11-27 | Evonik Degussa Gmbh | Pyrogen hergestellte silanisierte und vermahlene Kieselsäure |
DE102007024095A1 (de) * | 2007-05-22 | 2008-11-27 | Evonik Degussa Gmbh | Hydrophobe pyrogen hergestellte Kieselsäure und Silikonkautschukmassen, enthaltend die pyrogene Kieselsäure |
DE102007024097A1 (de) * | 2007-05-22 | 2008-11-27 | Evonik Degussa Gmbh | Kieselsäuren |
DE102007024094A1 (de) | 2007-05-22 | 2008-11-27 | Evonik Degussa Gmbh | Hydrophobe pyrogen hergestellte Kieselsäure und Silikonkautschukmassen, enthaltend die pyrogene Kieselsäure |
DE102007025685A1 (de) * | 2007-06-01 | 2008-12-04 | Evonik Degussa Gmbh | RTV-Zweikomponenten-Silikonkautschuk |
DE102007035952A1 (de) * | 2007-07-30 | 2009-04-09 | Evonik Degussa Gmbh | Oberflächenmodifizierte, pyrogen hergestellte Kieselsäuren |
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EP2070992A1 (de) * | 2007-12-11 | 2009-06-17 | Evonik Degussa GmbH | Lacksysteme |
DE102007059860A1 (de) * | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Schülpen aus pyrogen hergestelltem Siliziumdioxid |
DE102007059862A1 (de) * | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Durch-und-durch hydrophobe Schülpen aus pyrogen hergestelltem Siliziumdioxid |
DE102007055879A1 (de) | 2007-12-19 | 2009-06-25 | Wacker Chemie Ag | Hydrophobierung von Kieselsäuren und oxidierenden Bedingungen |
WO2010059710A1 (en) * | 2008-11-19 | 2010-05-27 | Dow Corning Corporation | A silicone composition and a method for preparing the same |
DE102009000614A1 (de) | 2009-02-04 | 2010-08-05 | Evonik Degussa Gmbh | Fluorfreie Zusammensetzung zur wasserabweisenden Beschichtung von Oberflächen mit verbesserten Abperleigenschaften |
WO2011150004A2 (en) | 2010-05-25 | 2011-12-01 | The Procter & Gamble Company | Oral care compositions and methods of making oral care compositions comprising silica from plant materials |
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FR2979107A1 (fr) * | 2011-08-16 | 2013-02-22 | Bluestar Silicones France | Procede de preparation d'une silice greffee par un compose organosilicie |
JP6122251B2 (ja) * | 2012-04-12 | 2017-04-26 | 石原産業株式会社 | 有機化合物被覆粉体の製造方法 |
DE102012211121A1 (de) | 2012-06-28 | 2014-01-02 | Evonik Industries Ag | Granuläre, funktionalisierte Kieselsäure, Verfahren zu deren Herstellung und deren Verwendung |
WO2017130890A1 (ja) * | 2016-01-28 | 2017-08-03 | 富士フイルム株式会社 | 音響波プローブ用組成物、これを用いた音響波プローブ用シリコーン樹脂、音響波プローブおよび超音波プローブ、ならびに、音響波測定装置、超音波診断装置、光音響波測定装置および超音波内視鏡 |
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2004
- 2004-03-05 DE DE102004010756A patent/DE102004010756A1/de not_active Withdrawn
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- 2005-02-08 KR KR1020067017929A patent/KR20060127172A/ko not_active Application Discontinuation
- 2005-02-08 JP JP2007501142A patent/JP5260048B2/ja not_active Expired - Fee Related
- 2005-02-08 US US10/591,609 patent/US7713626B2/en not_active Expired - Fee Related
- 2005-02-08 EP EP05707248.0A patent/EP1730240B1/en active Active
- 2005-02-08 WO PCT/EP2005/001229 patent/WO2005095525A1/en not_active Application Discontinuation
- 2005-02-08 ES ES05707248.0T patent/ES2649263T3/es active Active
- 2005-02-08 CN CN201410040325.2A patent/CN103819942B/zh not_active Expired - Fee Related
- 2005-02-08 CN CNA2005800070906A patent/CN1930249A/zh active Pending
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Also Published As
Publication number | Publication date |
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TW200538458A (en) | 2005-12-01 |
ES2649263T3 (es) | 2018-01-11 |
CN103819942A (zh) | 2014-05-28 |
DE102004010756A1 (de) | 2005-09-22 |
CN1930249A (zh) | 2007-03-14 |
JP2007526374A (ja) | 2007-09-13 |
US7713626B2 (en) | 2010-05-11 |
WO2005095525A1 (en) | 2005-10-13 |
EP1730240B1 (en) | 2017-10-11 |
CN103819942B (zh) | 2016-07-06 |
KR20060127172A (ko) | 2006-12-11 |
EP1730240A1 (en) | 2006-12-13 |
TWI304068B (en) | 2008-12-11 |
US20070191537A1 (en) | 2007-08-16 |
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