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Patent 2203726 Summary

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Claims and Abstract availability

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(12) Patent: (11) CA 2203726
(54) English Title: SILANIZED SILICA
(54) French Title: SILICE SILANISEE
Status: Expired
Bibliographic Data
(51) International Patent Classification (IPC):
  • C01B 33/18 (2006.01)
  • C08K 3/36 (2006.01)
  • C08K 9/06 (2006.01)
  • C09C 1/30 (2006.01)
  • C09C 3/12 (2006.01)
  • C09G 1/00 (2006.01)
  • C09K 3/10 (2006.01)
  • C09D 7/00 (2006.01)
(72) Inventors :
  • HARTMANN, WERNER (Germany)
  • MEYER, JURGEN (Germany)
  • JACOBSEN, HAUKE (Germany)
  • HENNIG, THOMAS (Germany)
  • KARBE, HENNING (Germany)
  • SCHACHTELY, UWE (Germany)
(73) Owners :
  • EVONIK DEGUSSA GMBH (Not Available)
(71) Applicants :
  • DEGUSSA AKTIENGESELLSCHAFT (Germany)
(74) Agent: MARKS & CLERK
(74) Associate agent:
(45) Issued: 2001-08-07
(22) Filed Date: 1997-04-25
(41) Open to Public Inspection: 1997-10-26
Examination requested: 1997-10-17
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
196 16 781.7 Germany 1996-04-26

Abstracts

English Abstract

The present invention provides a silanized pyrogenically- produced silica with the following physico-chemical properties: Specific surface area m2/g 80 - 400 Primary particle size nm 7 - 40 Tamped density g/l 50 - 300 pH value 3 - 10 Carbon content % 0.1 - 15 DBP number % < 200. The invention also provides a method of producing the above silanized pyrogenically-produced silica, comprising spraying pyrogenically-produced silica in a mixing container under intensive mixing, first with water or dilute acid and then with hexamethyldisilazane, mixing for 15 to 30 minutes, and tempering at a temperature of 100 to 400°C for a period of 1 to 6 h.


French Abstract

La présente invention fournit une silice produite par pyrogénation silanisée avec les propriétés physico-chimiques suivantes : une surface spécifique de 80 à 400 m/g, des particules primaires d'une taille de 7 à 40 nm, une densité tassée de 50 à 300 g/L, une valeur de pH de 3 à 10, une teneur en carbone de 0,1 à 15 %, un indice DBP d'un pourcentage inférieur à 200. L'invention fournit également une méthode de production de cette silice produite par pyrogénation silanisée, comprenant la pulvérisation de la silice produite par pyrogénation dans un récipient à mélange sous agitation intense, d'abord avec de l'eau ou de l'acide dilué, puis avec de l'hexaméthyldisilazane, en mélangeant pendant 15 à 30 minutes et en mettant à une température de 100 à 400.degrés.C pour une période de 1 à 6 h.

Claims

Note: Claims are shown in the official language in which they were submitted.



The embodiments of the invention in which an exclusive
property or privilege is claimed are defined as follows:
1. Silanized pyrogenically-produced silica with the
following physico-chemical properties:
Specific surface area m2/g 80 - 400
Primary particle size nm 7 - 40
Tamped density g/l 50 - 300
pH value 3 - 10
Carbon content % 0.1 - 15
DBP number % < 200.
2. A method of producing the silanized
pyrogenically-produced silica according to claim 1,
comprising spraying pyrogenically-produced silica in a
mixing container under intensive mixing, first with water
or dilute acid and then with hexamethyldisilazane, mixing
for 15 to 30 minutes, and tempering at a temperature of 100
to 400°C for a period of 1 to 6 h.
3. The method according to claim 2, further
comprising subsequently destructuring or compressing said
silica by mechanical action.
4


4. The method according to claim 2 or 3, further
comprising grinding said silica.
5. A polymer composition comprising a polymer and
the silanized pyrogenically-produced silica according to
claim 1.
6. The polymer composition according to claim 5
which has a low viscosity and low flow point.
7. A method of producing a low-viscosity polymer
system with a low flow point, the method comprising adding
to a polymer composition the silanized pyrogenically-
produced silica of claim 1.
8. A method of modifying the properties of a paint
or a film, the method comprising adding thereto the
silanized pyrogenically-produced silica of claim 1.
9. A coating composition comprising a liquid polymer
system and the silanized pyrogenically-produced silica of
claim 1.

Description

Note: Descriptions are shown in the official language in which they were submitted.



CA 02203726 2000-10-26
..
SILANIZED SILICA
Introduction
The present invention relates to a low-thickening,
silanized silica, a method of its production and its use.
Summary of the Invention
The present invention provides a silanized
pyrogenically-produced silica with the following physico-
chemical properties:
Specific surface area m2/g 80 400
-


Primary particle size nm 7 - 40


Tamped density g/1 50 300
-


pH value 3 - 10


Carbon content ~ 0.1 -
15


DBP number ~ < 200.



The invention also provides a method of producing the
above silanized pyrogenically-produced silica, comprising
spraying pyrogenically-produced silica in a.mixing
container under intensive mixing, first with water or
dilute acid and then with hexamethyldisilazane, mixing for
15 to 30 minutes, and tempering at a temperature of 100 to
400°C for a period of 1 to 6 h.
Preferably, the hydrophobic, silanized silica obtained
thereby is subsequently destructured/compressed by
mechanical action (e.g. in a ball mill) and then ground in
a mill (e. g. an air-jet mill or pinned disk mill).
1


CA 02203726 2000-10-26
Detailed Description of Invention
In carrying out the present invention, a silica
pyrogenically produced by the flame hydrolysis of SiCl4 can
be preferably used as the starting material silica.
Hexamethyldisilazane is preferably used as the
surface-modifying reagent.
In a further aspect of the present invention, the low-
thickening, silanized silica produced in accordance with
the method disclosed herein is used for producing low-
viscosity polymer systems with a low flow point such as
e.g. 1- and 2-component peroxide condensation- and
addition-cross-linking silicon rubber systems, adhesives,
molding compounds, jointing compounds, etc. In addition,
the silica of the invention can be used as a flatting
agent, e.g. in paints, foils, as free-flow agent (e. g.
S.A.P., fire-extinguishing powder), for the production of
cable gels, as an anti-sedimentation agent in liquid
plastic systems and reaction resins (e. g. synthetic marble,
polymer concrete, dentures), and as a polishing agent
and/or scouring bodies.
Good mechanical strength is obtained in a polymer
system reinforced with synthetic silicas only with a very
high degree of filling. Good mechanical strength can be
provided in known silicas only by an in-situ hydrophobing
of the reinforcing silica during the production/compounding
of corresponding jointing compounds, molding compounds and
doubling compounds, etc. This method consumes a
significant amount of time and energy.
The silica in accordance with the invention makes
possible a high degree of filling, and therewith good
2


CA 02203726 2000-10-26
' mechanical strength, by means of its low thickening action
and low flow point. Hence, the above-mentioned, expensive
compounding process using known silicas can be eliminated.
The method in accordance with the invention has the
advantage that, as a result of the continuous nature of the
method, reduced variations occur in the~quality of the
product.
EXAMPLE
Aerosil'?' 200, a pyrogenically-produced silica by
Degussa AG, is mixed with 4.3 parts water and 18.5 parts
HMDS (hexamethyldisilazane) and tempered at 140°C. The
hydrophobic, silanized silica is then compressed on a
continuously operating vertical ball mill to approximately
250 g/1. The silica is then ground by an air-jet mill.
The silica obtained has the following properties:
ExampleBET Tamped pH C-contentDrying AnnealingDBP


m2/g density loss loss number



VT 145 188 7.3 2.7 2.4 0.3 90


1128/I


Application technology test
2K-RTV silicone rubber (degree of filling 20~)
Rheology: Flow point 1.9 Pa
Viscosity 30.9 s-1
Mechanical properties: Tensile strength 1.7 N/mm2
Breaking elongation 230
Tear strength 14.0 N/mm
Shore A hardness 34
3

Representative Drawing

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Administrative Status

For a clearer understanding of the status of the application/patent presented on this page, the site Disclaimer , as well as the definitions for Patent , Administrative Status , Maintenance Fee  and Payment History  should be consulted.

Administrative Status

Title Date
Forecasted Issue Date 2001-08-07
(22) Filed 1997-04-25
Examination Requested 1997-10-17
(41) Open to Public Inspection 1997-10-26
(45) Issued 2001-08-07
Expired 2017-04-25

Abandonment History

There is no abandonment history.

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $300.00 1997-04-25
Request for Examination $400.00 1997-10-17
Maintenance Fee - Application - New Act 2 1999-04-26 $100.00 1999-04-08
Registration of a document - section 124 $50.00 1999-04-30
Maintenance Fee - Application - New Act 3 2000-04-25 $100.00 2000-03-27
Maintenance Fee - Application - New Act 4 2001-04-25 $100.00 2001-03-21
Final Fee $300.00 2001-05-01
Registration of a document - section 124 $50.00 2001-11-26
Maintenance Fee - Patent - New Act 5 2002-04-25 $150.00 2002-03-20
Maintenance Fee - Patent - New Act 6 2003-04-25 $150.00 2003-03-18
Maintenance Fee - Patent - New Act 7 2004-04-26 $200.00 2004-03-19
Maintenance Fee - Patent - New Act 8 2005-04-25 $200.00 2005-03-24
Maintenance Fee - Patent - New Act 9 2006-04-25 $200.00 2006-03-24
Maintenance Fee - Patent - New Act 10 2007-04-25 $250.00 2007-03-26
Maintenance Fee - Patent - New Act 11 2008-04-25 $250.00 2008-03-25
Registration of a document - section 124 $100.00 2009-03-31
Maintenance Fee - Patent - New Act 12 2009-04-27 $250.00 2009-04-09
Maintenance Fee - Patent - New Act 13 2010-04-26 $250.00 2010-04-09
Maintenance Fee - Patent - New Act 14 2011-04-25 $250.00 2011-04-15
Maintenance Fee - Patent - New Act 15 2012-04-25 $450.00 2012-04-12
Maintenance Fee - Patent - New Act 16 2013-04-25 $450.00 2013-04-15
Maintenance Fee - Patent - New Act 17 2014-04-25 $450.00 2014-04-14
Maintenance Fee - Patent - New Act 18 2015-04-27 $450.00 2015-04-13
Maintenance Fee - Patent - New Act 19 2016-04-25 $450.00 2016-04-12
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
EVONIK DEGUSSA GMBH
Past Owners on Record
DEGUSSA AG
DEGUSSA AKTIENGESELLSCHAFT
DEGUSSA-HULS AKTIENGESELLSCHAFT
HARTMANN, WERNER
HENNIG, THOMAS
JACOBSEN, HAUKE
KARBE, HENNING
MEYER, JURGEN
SCHACHTELY, UWE
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Cover Page 1997-12-05 1 34
Abstract 1997-04-25 1 14
Description 1997-04-25 3 111
Claims 1997-04-25 2 42
Cover Page 2001-07-26 1 30
Abstract 2000-10-26 1 19
Description 2000-10-26 3 107
Claims 2000-10-26 2 46
Prosecution-Amendment 1999-12-20 4 107
Assignment 2001-11-26 5 204
Correspondence 2001-05-01 1 30
Assignment 1997-10-02 2 69
Prosecution-Amendment 1997-10-17 1 29
Prosecution-Amendment 2000-10-26 13 385
Prosecution-Amendment 2000-10-26 10 320
Assignment 1997-04-25 3 74
Correspondence 1997-05-20 1 36
Prosecution-Amendment 2000-04-27 2 77
Assignment 1999-04-30 3 84
Assignment 2009-03-31 5 244