JP2013528154A - シリカゾル材料の製造方法 - Google Patents
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Abstract
Description
(a)酸性水溶液と加水分解性ケイ素化合物との制御された接触、
(b)その後に続くエバポレーションにより、4℃で10s−1のせん断速度において0.5〜30Pa・sの範囲の粘度を有する単相溶液を得ること、および
(c)工程(b)で得られた単相溶液を熟成して、4℃で10s−1のせん断速度において30〜100Pa・sの範囲の粘度および2〜5の損失係数を有するシリカゾル材料を得ること。
SiX4 (I)
〔式中、基Xは、同一であるか、または異なっており、ヒドロキシ、水素、ハロゲン、アミノ、アルコキシ、アシルオキシ、アルキルカルボニルおよび/またはアルコキシカルボニルを表し、1〜20個の炭素原子を有する、好ましくは1〜10個の炭素原子を有する、場合により置換された直鎖、分枝または環状の基であるアルキル基に由来し、酸素もしくはイオウ原子またはアミノ基により中断されていてもよい〕
で示されるケイ素化合物を意味する。本発明の一実施態様において、式(I)のXは、1〜20個の炭素原子を有する、好ましくは1〜10個の炭素原子を有する場合により置換された直鎖、分枝および/または環状のアルコキシ基を表す。特に好ましくは、式(I)におけるXは、場合により置換された直鎖および/または分枝C1〜C5アルコキシ基を表す。置換された、だが好ましくは非置換の直鎖および/または分枝C2〜C3アルコキシ基(例えば、エトキシ、N−プロポキシおよび/またはイソプロポキシなど)がさらに好ましい。本発明によれば、テトラエトキシシラン(TEOS)が、本発明の製造方法におけるケイ素化合物として非常に特に好ましい。
加水分解−縮合の出発材料として、5.4モルTEOS(テトラエトキシシロキサン)/6.8モルエタノールを密閉容器内へ投入した。0.006N HNO3溶液の形態の水(9.6モル)を予め混合した後、制御された方法で、37℃の一定温度(等温線モード)で1時間かけてエタノール/TEOS混合物中に量り入れた。エタノール濃度が約68重量%になるまで、17時間、後撹拌した。その後、4℃で10s−1のせん断速度において1Pa・sの粘度になるまで、引き続き単相溶液を62℃の一定最低温度、500〜120mbarでエバポレートした。シリカゾル材料の熟成は、4℃で10s−1のせん断速度において55Pa・sの粘度および損失係数が3になるまで、28.1℃の温度で撹拌しながら行った。
エタノール(2.6モル;100%)を密閉反応容器へ投入した。残りのエタノール(4.2モル;100%)を、制御された方法で、エタノールとの接触を経た5.4モルのTEOSとともに1時間かけて反応容器内へ量り入れた。同時に、0.006N HNO3溶液の形態の水(9.6モル)を、反応容器への他の投入手段により1時間かけて量り入れた。反応は、反応全体の初めから終わりまで反応容器内の最低温度が37℃(等温線モード)となるようにして行った。熟成温度以外は第1実施例に記載したのと同様にして他の製造工程を行った。熟成温度は4℃であった。
エタノール(6.8モル;100%)を、0.006N HNO3溶液の形態の水(9.6モル)とともに密閉反応容器へ投入した。反応容器に入っている混合物中へ、5.4モルのTEOS(テトラエトキシシロキサン)を制御された方法により1時間かけて量り入れた。反応は、反応全体の初めから終わりまで反応容器内の最低温度が37℃(等温線モード)となるようにして行った。第1実施例に記載したのと同様にして他の製造工程を行った。シリカゾル材料の熟成は、4℃で10s−1のせん断速度において30Pa・sの粘度および損失係数が3.1になるまで、7℃温度で撹拌しながら行った。
Claims (8)
- (a)酸性水溶液と加水分解性ケイ素化合物との制御された接触、
(b)その後に続くエバポレーションにより、4℃で10s−1のせん断速度において0.5〜30Pa・sの範囲の粘度を有する単相溶液を得ること、および
(c)工程(b)で得られた単相溶液を熟成して、4℃で10s−1のせん断速度において30〜100Pa・sの範囲の粘度および2〜5の損失係数を有するシリカゾル材料を得ることによる、
シリカゾル材料の製造方法。 - 工程(a)において、制御された測量添加を少なくとも15分の時間をかけて行うことを特徴とする請求項1に記載の方法。
- 工程(a)を等温状態で行うことを特徴とする、請求項1または2に記載の方法。
- 工程(b)における最低温度を、圧力を調節することにより一定に保つことを特徴とする、請求項1〜3のいずれかに記載の方法。
- 単相溶液を撹拌しながら、工程(c)の熟成を行うことを特徴とする、請求項1〜4のいずれかに記載の方法。
- 1atm標準気圧下−25〜78℃の温度で、または、過圧下78℃より高い温度で、工程(c)の熟成を行うことを特徴とする、請求項1〜5のいずれかに記載の方法。
- 工程(a)〜工程(c)を同一反応容器内で行うことを特徴とする、請求項1〜6のいずれかに記載の方法。
- 溶媒中に存在する酸への加水分解ケイ素化合物の制御された測量添加、その後に続くエバポレーションにより、4℃で10s−1のせん断速度において0.5〜2Pa・sの範囲の粘度を有する単相溶液を得ること、および、該単相溶液を熟成することにより、4℃で10s−1のせん断速度において30Pa・sの粘度および3.1の損失係数を有するシリカゾル材料を得ることにより製造されるシリカゾル材料。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102010023336A DE102010023336A1 (de) | 2010-06-10 | 2010-06-10 | Verfahren zur Herstellung eines Kieselsol-Materials |
DE102010023336.6 | 2010-06-10 | ||
PCT/EP2011/059302 WO2011154361A2 (de) | 2010-06-10 | 2011-06-06 | Verfahren zur herstellung eines kieselsol-materials |
Publications (2)
Publication Number | Publication Date |
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JP2013528154A true JP2013528154A (ja) | 2013-07-08 |
JP2013528154A5 JP2013528154A5 (ja) | 2014-06-26 |
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Application Number | Title | Priority Date | Filing Date |
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JP2013513652A Pending JP2013528154A (ja) | 2010-06-10 | 2011-06-06 | シリカゾル材料の製造方法 |
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Country | Link |
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US (1) | US9221690B2 (ja) |
EP (1) | EP2580173A2 (ja) |
JP (1) | JP2013528154A (ja) |
AU (1) | AU2011263823A1 (ja) |
BR (1) | BR112012031454A2 (ja) |
CA (1) | CA2801970C (ja) |
DE (1) | DE102010023336A1 (ja) |
MX (1) | MX2012014213A (ja) |
WO (1) | WO2011154361A2 (ja) |
Families Citing this family (6)
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US9518345B2 (en) | 2011-07-21 | 2016-12-13 | Jiangsu Synecoun Medical Technology Co., Ltd | Method for producing a spinnable silica sol material |
DE102012213843B3 (de) | 2012-08-03 | 2013-09-19 | Automotive Lighting Reutlingen Gmbh | Primäroptikeinheit für ein Lichtmodul |
KR102242683B1 (ko) | 2013-04-17 | 2021-04-23 | 실본드 코포레이션 | 콜로이드 졸 및 그의 제조 방법 |
US10442899B2 (en) | 2014-11-17 | 2019-10-15 | Silbond Corporation | Stable ethylsilicate polymers and method of making the same |
CN105819455B (zh) * | 2016-03-31 | 2017-08-25 | 上海理工大学 | 一种介孔硅胶纳米颗粒的制备方法及其应用 |
DE102017217539B4 (de) * | 2017-10-02 | 2021-04-22 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Biodegradierbare Fasern, Verfahren zu deren Herstellung und deren Verwendung, sowie diese enthaltende Fasergeflechte oder -filter |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA2675181A1 (en) * | 2007-01-15 | 2008-07-24 | Bayer Innovation Gmbh | Silica sol material for producing biologically degradable and/or resorbable silica gel materials, the production and use thereof |
CA2689211A1 (en) * | 2007-06-04 | 2008-12-11 | Axel Thierauf | Nontoxic polyethoxysiloxane material for the production of biologically resorbable and/or bioactive articles containing polyethoxysiloxane material, the production thereof, and the use thereof |
CA2709572A1 (en) * | 2007-12-19 | 2009-06-25 | Bayer Innovation Gmbh | Nontoxic polysiloxane material for producing biologically resorbable and/or bioactive articles containing polysiloxane material, its production and use |
CA2730697A1 (en) * | 2008-07-16 | 2010-01-21 | Bayer Innovation Gmbh | Silica sol material having at least one therapeutically active substance for producing biologically degradable and/or resorbable silica gel materials for human medicine and/or medical technology |
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Publication number | Priority date | Publication date | Assignee | Title |
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DE19609551C1 (de) | 1996-03-12 | 1997-07-17 | Fraunhofer Ges Forschung | Biologisch degradierbare und/oder biologisch resorbierbare (Endlos)Fasern, Verfahren zu deren Herstellung und deren Verwendung als Verstärkungsfasern |
DE102004063599B4 (de) * | 2004-12-30 | 2007-07-12 | Bayer Innovation Gmbh | Verkürzte Wundheilungsprozesse mittels neuartiger Faservliese |
-
2010
- 2010-06-10 DE DE102010023336A patent/DE102010023336A1/de active Pending
-
2011
- 2011-06-06 US US13/702,676 patent/US9221690B2/en active Active
- 2011-06-06 EP EP11725672.7A patent/EP2580173A2/de not_active Withdrawn
- 2011-06-06 BR BR112012031454A patent/BR112012031454A2/pt not_active IP Right Cessation
- 2011-06-06 JP JP2013513652A patent/JP2013528154A/ja active Pending
- 2011-06-06 WO PCT/EP2011/059302 patent/WO2011154361A2/de active Application Filing
- 2011-06-06 AU AU2011263823A patent/AU2011263823A1/en not_active Abandoned
- 2011-06-06 MX MX2012014213A patent/MX2012014213A/es not_active Application Discontinuation
- 2011-06-06 CA CA2801970A patent/CA2801970C/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA2675181A1 (en) * | 2007-01-15 | 2008-07-24 | Bayer Innovation Gmbh | Silica sol material for producing biologically degradable and/or resorbable silica gel materials, the production and use thereof |
CA2689211A1 (en) * | 2007-06-04 | 2008-12-11 | Axel Thierauf | Nontoxic polyethoxysiloxane material for the production of biologically resorbable and/or bioactive articles containing polyethoxysiloxane material, the production thereof, and the use thereof |
CA2709572A1 (en) * | 2007-12-19 | 2009-06-25 | Bayer Innovation Gmbh | Nontoxic polysiloxane material for producing biologically resorbable and/or bioactive articles containing polysiloxane material, its production and use |
CA2730697A1 (en) * | 2008-07-16 | 2010-01-21 | Bayer Innovation Gmbh | Silica sol material having at least one therapeutically active substance for producing biologically degradable and/or resorbable silica gel materials for human medicine and/or medical technology |
Also Published As
Publication number | Publication date |
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DE102010023336A1 (de) | 2011-12-15 |
EP2580173A2 (de) | 2013-04-17 |
CA2801970A1 (en) | 2011-12-15 |
WO2011154361A2 (de) | 2011-12-15 |
US20130145964A1 (en) | 2013-06-13 |
AU2011263823A1 (en) | 2013-01-24 |
BR112012031454A2 (pt) | 2016-11-08 |
WO2011154361A3 (de) | 2012-04-12 |
MX2012014213A (es) | 2013-02-07 |
RU2012157528A (ru) | 2014-07-20 |
CA2801970C (en) | 2017-10-24 |
US9221690B2 (en) | 2015-12-29 |
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