Curable and cured silicone rubber compositions and methods therefor
View Patent ↗A method for producing a functionalized silica, compositions and methods for forming curable silicone rubber compositions by using the functionalized silica are also disclosed. Compositions and methods for forming cured silicone resin compositions and products having high transparency, high tensile strength, desirable percent elongation, or a combination of the foregoing properties are also disclosed.
1. A method for preparing a functionalized silica, comprising:
mixing an aqueous alcoholic solution and a catalyst with a first portion of a first organosilicon functionalizing agent to form a first reaction mixture;
reacting said first reaction mixture with a tetraalkoxysilane at a controlled rate to form a second reaction mixture comprising a sol gel silica; and
further reacting said second reaction mixture with a mixture of a second portion of said first organosilicon functionalizing agent and a second organosilicon functionalizing agent to functionalize the sol gel silica to form said functionalized silica.
2. The method of claim 1 further comprising adding at least one additional solvent wherein a suspension is formed comprising said functionalized silica.
3. The method of claim 2 wherein the solvent is selected from the group consisting of hydrocarbons, silicone based monomers, liquid carbon dioxide, ionic liquids and mixtures thereof.
4. The method of claim 3 wherein said hydrocarbon solvent is selected from the group consisting of xylene, toluene, cyclohexane, heptane, octane, iso-octane, isododecanol and mixtures thereof.
5. The method of claim 3 wherein the silicone based monomer solvent is selected from the group consisting of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane and mixtures thereof.
6. The method of claim 1 wherein the first organosilicon functionalizing agent comprises a organosilazane, and the catalyst comprises a base catalyst or a neutral catalyst.
7. The method of claim 6 wherein the organosilazane comprises a hexaalkyldisilazane.
8. The method of claim 7 wherein said catalyst comprises a base catalyst.
9. The method of claim 7 wherein said hexaalkyldisilazane comprises hexamethyldisilazane.
10. The method of claim 1 , wherein said first organosilicon functionalizing agent comprises a halosilane, and said catalyst is an acid catalyst or a neutral catalyst.
11. The method of claim 10 , wherein said dialkenyl(tetraalkyl)disilazane comprises divinyl(tetramethyl)disilazane.
12. The method of claim 1 , wherein said second organosilicon functionalizing agent comprises at least one alkenyl group.
13. The method of claim 12 , wherein said second organosilicon functionalizing agent comprises a (dialkenyl)disilazane.
14. The method of claim 13 , wherein said (dialkenyl)silazane comprises a dialkenyl(tetraalkyl)disilazane.
15. The method of claim 1 , wherein said second organosilicon functionalizing agent comprises a (alkenyl)halosilane, and said catalyst is an acid catalyst or a neutral catalyst.
16. The method of claim 1 , wherein said second portion and said first portion of said first organosilicon functionalizing agent are employed in a relative mole ratio of from about 1:0.5 to about 1:1.
17. The method of claim 1 , wherein said tetraalkoxysilane and said first portion of said first organosilicon functionalizing agent are in a relative mole ratio of from 1:0.2 to about 1:0.6.
18. A method for forming a curable silicone rubber composition, comprising:
a) forming a functionalized silica by a method comprising:
mixing an aqueous basic alcoholic solution with a first organosilicon functionalizing agent to form a first reaction mixture;
reacting said first reaction mixture with a tetraalkoxysilane at a controlled rate to form a second reaction mixture comprising a sol gel silica;
further reacting said second reaction mixture with a mixture of a second portion of said first organosilicon functionalizing agent and a second organosilicon functionalizing agent to form the functionalized silica;
b) adding a solvent to the mixture of (a) wherein a suspension is formed comprising the functionalized silica; and
c) compounding and devolatilizing said suspension of (b) with a silicone polymer to form said curable silicone rubber composition.
19. The method of claim 18 , wherein said curable silicone rubber composition is a curable liquid silicone rubber composition.
20. The method of claim 18 , further comprising treating said curable silicone rubber composition with a further portion of said first organosilicon functionalizing agent.
21. The method of claim 20 , further comprising heating to a temperature from greater than 100° C. to about 150° C. under vacuum.
22. A curable silicone rubber composition prepared in accordance with the method of claim 18 .
23. The curable silicone rubber composition of claim 22 , having a shear viscosity from about 200 pascal-second to about 1500 pascal-second, when measured at 10 radians per second in accordance with ASTM D440 test method.
24. The curable silicone rubber composition of claim 22 , having a shear viscosity from about 500 pascal-second to about 1000 pascal-second, when measured at 10 radians per second in accordance with ASTM D440 test method.
25. The curable silicone rubber composition of claim 18 , further comprising a fumed silica.
26. A method for forming a cured silicone rubber composition, comprising:
forming a functionalized silica by a method comprising:
mixing an aqueous basic alcoholic solution with a first organosilicon functionalizing agent to form a first reaction mixture;
reacting said first reaction mixture with a tetraalkoxysilane at a controlled rate to form a second reaction mixture comprising a sol gel silica;
further reacting said second reaction mixture with a mixture of a second portion of said first organosilicon functionalizing agent and a second organosilicon functionalizing agent to form the functionalized silica;
adding a solvent wherein a suspension is formed comprising the functionalized silica;
compounding and devolatilizing said suspension with a liquid silicone polymer to form a curable silicone rubber composition; and
further compounding and devolatilizing said curable silicone rubber composition to form said cured silicone rubber composition.
27. The method of claim 26 , further comprising dividing said curable silicone rubber composition into a first stream and a second stream.
28. The process of claim 27 , wherein a platinum catalyst is added to said first stream to produce a component mixture A and a cross-linker is added to said second stream to produce a component mixture B.
29. The process of claim 28 , comprising injecting and curing said component mixture A and said component mixture B into a mold to produce a cured silicone rubber part.
30. The method of claim 26 , wherein compounding and devolatilizing said curable silicone rubber composition is implemented in a co-rotating, intermeshing double screw extruder.
31. A cured silicone rubber composition prepared in accordance with the method of claim 26 .
32. The cured silicone rubber composition of claim 31 , having a percent light transmission of greater than 90 percent as measured on a 2.3 millimeters thick plaque using ASTM D1003 test method; a tensile strength of greater than 4.5 megapascals as measured using ASTM D612 test method; and an elongation of at least 200 percent as measured using ASTM D612 test method.
33. An article manufactured using the cured silicone rubber composition of claim 32 .
34. The article of claim 33 , comprising a compression molded sheet, an diving mask, infant nipple, a face mask, a surgical tubing, a pacifier, a light emitting diode, or a disposable ocular lens.