Silanized silicas
Abstract
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Term
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Expired 10 April 2017, 9.5 years ago.
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3 claims: 1 independent, 2 dependent
- 1Silanisierte pyrogen auf dem Wege der Flammenhydrolyse von SiCl 4 hergestellte Kieselsäure mit folgenden physikalisch-chemischen Eigenschaften:Spezifische Oberfläche m 2 /g 80 - 400 Primärteilchengröße nm 7 - 40 Stampfdichte g/l 50 - 300 pH 3 - 10 Kohlenstoffgehalt % 0,1 - 15 DBP-Zahl % < 200
- 2Verfahren zur Herstellung der silanisierten pyrogen auf dem Wege der Flammenhydrolyse von SiCl 4 hergestellte Kieselsäure nach Anspruch 1, dadurch gekennzeichnet, daß man eine Kieselsäure in einem geeigneten Mischgefäß unter intensivem Mischen, gegebenenfalls zunächst mit Wasser oder verdünnter Säure und anschließend mit einem Oberflächenmodifizierungsreagens oder einem Gemisch aus mehreren Oberflächenmodifizierungsreagentien besprüht, 15 bis 30 Minuten nachmischt, bei einer Temperatur von 100 bis 400 °C über einen Zeitraum von 1 bis 6 h tempert, anschließend die hydrophobe silanisierte Kieselsäure durch mechanische Einwirkung destrukturiert/verdichtet und in einer Mühle nachvermahlt.
- 3Verwendung der silanisierten pyrogen auf dem Wege der Flammenhydrolyse von SiCl 4 hergestellte Kieselsäure gemäß Anspruch 1 zur Herstellung von niedrigviskosen Polymersystemen mit niedriger Fließgrenze als Mattierungsmittel (zum Beispiel in Lacken, Folien), Freeflow-Mittel (zum Beispiel SAP, Feuerlöschpulver), Kabelgele, Antisedimentationsmittel in flüssigen Kunststoffsystemen und Reaktionsharzen, Poliermittel und Putzkörper.
Independent claims3
14 paragraphs, as filed
0001The invention relates to a low-thickening, silanized pyrogenic by way of flame hydrolysis of SiCl<sub>4</sub> silica, a process for their Preparation and their use.
0002The invention is a silanized pyrogenically by way of flame hydrolysis of SiCl<sub>4</sub> produced silica with the following physico-chemical properties:<tables><table><tgroup cols="3"><tbody><row><entry align="left">specific surface</entry><entry align="left">m<sup>2</sup>/G</entry><entry align="center">80-400</entry></row><row><entry align="left">primary</entry><entry align="left">nm</entry><entry align="center">7-40</entry></row><row><entry align="left">tamped density</entry><entry align="left">g / l</entry><entry align="center">50-300</entry></row><row><entry align="left">pH</entry><entry align="right" /><entry align="center">3-10</entry></row><row><entry align="left">Carbon content</entry><entry align="left">%</entry><entry align="center">0.1 to 15</entry></row><row><entry align="left">DBP number</entry><entry align="left">%</entry><entry align="center"><200</entry></row></tbody></tgroup></table></tables>
0003Another object of the invention is a method for Preparation of the silanised, pyrogenic low thickened by way of flame hydrolysis of SiCl<sub>4</sub> produced Silica, which is characterized in that a silicic acid in a suitable mixing vessel under intensive mixing optionally first with water or dilute acid and subsequently with a Surface modification or a mixture of several surface sprayed 15 to 30 minutes nachmischt, at a temperature of 100 to 400 ° C tempered over a period of 1 to 6 hours, and then the hydrophobic silanised silica by mechanical action (for example in a ball mill) destructured / compacted and in a mill (for example, Air jet mill, pin mill) nachvermahlt.
0004As the surface, for example, Hexamethyldisilazane are used.
0005Another object of the invention is the use the inventive low thickening, silanized fumed in the way of flame hydrolysis of SiCl<sub>4</sub> produced Silica for producing low viscosity Polymer systems having a low yield point, such as 1- and 2-component and peroxidkondensations- crosslinking silicone rubber compounds, adhesives, Impression materials, sealants, etc., their use as a matting agent, for example, in paints, films, as FreeFlow means (for example, SAP, fire extinguishing powder) for the preparation of Kabelgelen, as anti-sedimentation in liquid Plastic systems and reactive resins (synth, for example. Marble, polymer concrete, dentures) as polishing agents and / or abrasives.
0006The inventive low-thickening, silanized fumed in the way of flame hydrolysis of SiCl<sub>4</sub> produced Silica has the following advantages:
0007In polymer systems with synthetic silicas are amplified, are at very high filler achieved good mechanical strength. This is successful with known silicas only by an in-situ Repellency of the amplifier when silica Manufacture / compounding of appropriate sealing, Abformund Dupliermassen etc. This procedure is very time- and energy-consuming.
0008The silica of the invention made possible by their low thickening action and low flow limit For example, high filler levels and thus good mechanical Strengths. The above complicated compounding process can largely disappeared.
0009The inventive method has the advantage that reduced due to the continuous process control Fluctuations in product quality occur.
example
0010Aerosil 200 is with 4.3 parts water and 18.5 parts of HMDS (Hexamethyldisilazane) were mixed and heated to 140 ° C. The hydrophobic silanized silica is then a continuously operating vertical ball mill to approximately 250 g / l compacted. Thereafter, the silica is by an air jet mill re-ground.
0011The Kieseläsure obtained has the following characteristics:<tables><table><tgroup cols="8"><tbody><row><entry align="center"><b>example</b></entry><entry align="center"><b>BET</b><b>m<sup>2</sup>/G</b></entry><entry align="center"><b>tamped density</b><b>g / l</b></entry><entry align="center"><b>pH</b></entry><entry align="center"><b>C-Gehatt</b></entry><entry align="center"><b>loss on drying%</b></entry><entry align="center"><b>loss on ignition%</b></entry><entry align="center"><b>DBP number</b><b>%</b></entry></row><row><entry align="center">VT 1128/1</entry><entry align="center">145</entry><entry align="center">188</entry><entry align="center">7.3</entry><entry align="center">2.7</entry><entry align="center">2.4</entry><entry align="center">0.3</entry><entry align="center">90</entry></row></tbody></tgroup></table></tables>
Performance Testing
0012<tables><table><tgroup cols="3"><tbody><row><entry namest="1" nameend="3">2K RTV Silicone Rubber (degree of filling 20%)</entry></row><row><entry align="left">rheology</entry><entry align="left">flow limit</entry><entry align="left">1.9 Pa</entry></row><row><entry align="left" /><entry align="left">viscosity</entry><entry align="left">30,9 s<sup>-1</sup></entry></row><row><entry align="left">Mechanical properties</entry><entry align="left">tensile strenght</entry><entry align="left">1.7 N / mm<sup>2</sup></entry></row><row><entry align="left" /><entry align="left">elongation</entry><entry align="left">230%</entry></row><row><entry align="left" /><entry align="left">Tear resistance</entry><entry align="left">14.0 N / mm</entry></row><row><entry align="left" /><entry align="left">Shore A hardness</entry><entry align="left">34</entry></row></tbody></tgroup></table></tables>
Every citation, both ways
| Document | Relation | Office | Cited during |
|---|---|---|---|
| US7402293B2 | Cited by | United States of America | Applicant |
| KR100899294B1 | Cited by | Republic of Korea | Examiner |
| KR100899294B1 | Cited by | Republic of Korea | Search report |
| DE2403783A | Cites | Germany | – |
| US4208316A | Cites | United States of America | – |
14 members in 7 offices
Priority claims4
| Document | Office | Kind | Date |
|---|---|---|---|
| 19616781 | Germany | – | |
| 19616781 | Germany | A | |
| DE1996116781 | – | – | – |
| 19616781 | – | – | – |
Members14
| Document | Office | Kind | |
|---|---|---|---|
| CA2203726A1 | Canada | A1 | |
| DE19616781A1 | Germany | A1 | |
| KR970069878A | Republic of Korea | A | |
| EP0808880A2 | European Patent Office (EPO) | A2 | |
| CN1167729A | China | A | |
| JPH1087317A | Japan | A | |
| US5959005A | United States of America | A | |
| EP0808880A3 | European Patent Office (EPO) | A3 | |
| KR100260325B1 | Republic of Korea | B1 | |
| CA2203726C | Canada | C | |
| CN1083397C | China | C | |
| EP0808880B1This record | European Patent Office (EPO) | B1 | |
| DE59709069D1 | Germany | D1 | |
| JP3553315B2 | Japan | B2 |
35 legal events, as 5 offices reported them to INPADOC
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Numbers
- Publication
- 0808880
- Publication, DOCDB
- 0808880
- Publication, EPODOC
- EP0808880
- Application
- 971059092
- Application, DOCDB
- 97105909
- Application, EPODOC
- EP19970105909
Titles3
- German
- Silanisierte Kieselsäure
- English
- Silanized silicas
- French
- Silices silanisées
Classification
- CPC, 17
- B82Y30/00
- C01B33/18
- C01P2004/64
- C01P2006/10
- C01P2006/11
- C01P2006/12
- C01P2006/19
- C01P2006/22
- C01P2006/80
- C01P2006/82
- C01P2006/90
- C08K3/36
- C09C1/3081
- C09D7/42
- C09G1/00
- C09K3/10
- C09K2200/0247
- IPC, 14
- B01J2 30
- C01B33 18
- C08K3 36
- C08K9 06
- C09C1 30
- C09C1 68
- C09C3 12
- C09D7 00
- C09D7 12
- C09D7 45
- C09G1 00
- C09K3 00
- C09K3 10
- C09K3 14
Designated states4
- Contracting states, 4
- Germany
- France
- United Kingdom
- Netherlands (Kingdom of the)