Compositions of resin-linear organosiloxane block copolymers
A technology of organosiloxane and block copolymers, which is applied in coatings, circuits, electrical solid devices, etc., and can solve the problems of lack of toughness, non-durability, and non-durability of coatings
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[0197] Containing for example at least 80 mol% [R 2 SiO 3 / 2 ] Organosiloxane resins of siloxy units and their preparation methods are known in the art. They are prepared in some embodiments by hydrolyzing organosilanes with three hydrolyzable groups (such as halogen or alkoxy) on the silicon atom in an organic solvent. Representative examples for preparing silsesquioxane resins can be found in U.S. Patent No. 5,075,103. In addition, many organosiloxane resins are commercially available and sold as solids (flakes or powders) or dissolved in organic solvents. Suitable non-limiting commercially available organosiloxane resins that can be used as component b) include: Dow 217 Flake Resin, 233Flake, 220Flake, 249Flake, 255Flake, Z-6018Flake (Dow Corning, Midland, Michigan).
[0198] Those skilled in the art realize that containing such a high amount of [R 2 SiO 3 / 2 ] The organosiloxane resin with siloxy units can have a certain concentration of Si-OZ, where Z can be hydrogen (ie sil...
example
[0221] The following examples are included to illustrate specific embodiments of the present invention. However, according to the present disclosure, those skilled in the art should understand that many changes can be made in the disclosed specific embodiments and still obtain similar or identical results without departing from the spirit and scope of the present invention. All percentages are in weight %. Unless otherwise specified, all measurements are performed at 23°C.
[0222] Characterization technique
[0223] 29 Si and 13 C NMR spectrum
[0224] By combining about 3 grams of solvent-free resin-linear copolymer (prepared by drying the sample overnight at room temperature), 1 gram of CDCl 3 And 4 grams of 0.04M Cr(acac) 3 CDCl 3 The solution was weighed into a vial and mixed thoroughly to prepare an NMR sample of the resin linear product. The sample was then transferred into a silicon-free NMR tube. The spectrum was acquired by Varian Mercury 400MHz NMR. By diluti...
example 1
[0235] Example 1: Preparation of 60 wt% Ph-T–230dp PhMe
[0236] Example 1
[0237] A 500 mL 4-neck round bottom flask was filled with toluene (60.00 g) and 217 flake resin (60.0 g, 0.439 mol Si). The flask was equipped with a thermometer, a Teflon stirring blade, and a Dean Stark device attached to a water-cooled condenser. Apply a nitrogen blanket. The Dean Stark device was precharged with toluene. Use an oil bath for heating.
[0238] The reaction mixture was heated under reflux for 30 minutes, during which time 0.30 mL of water was removed. The reaction mixture was cooled to 108°C (pot temperature).
[0239] A toluene (18.46g) solution of silanol-terminated PhMe siloxane (61.54g solution=40.0g siloxane, 0.293 mole Si) was used 50 / 50 methyltriacetoxysilane / ethyltriacetoxysilane (MTA / ETA) (0.60 g, 0.00260 mol Si) capped. The blocked PhMe siloxane was prepared in a glove box under nitrogen (on the day) by adding 50 / 50 MTA / ETA to the siloxane and mixing for 1 hour at room temp...
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