Compositions of resin-linear organosiloxane block copolymers
An organosiloxane, block copolymer technology, used in semiconductor/solid-state device parts, coatings, semiconductor devices, etc., can solve problems such as being not durable, difficult to apply, and unable to cure quickly enough
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example 1
[0345] Example 1: Representative Preparation of Resin-Linear (RL) Block Copolymers
[0346] A 12 L three neck round bottom flask was charged with phenyl-T resin (1800 g, 13.18 mol Si, Dow Corning 217 flakes) and toluene (1482 g) under nitrogen. The flask was equipped with a thermometer, a Teflon stirring impeller, and a Dean-Stark apparatus (the Dean-Stark apparatus was preloaded with toluene) attached to a water-cooled condenser. The reaction mixture was heated at reflux for 30 minutes and 8.18 g of water were removed. The reaction solution was cooled to 108°C, and MTA / ETA (methyltriacetoxysilane / ethyltriacetoxysilane)-terminated silanol-terminated PhMe siloxane (synthesized by adding 50 / 50% by weight of MTA / ETA (methyltriacetoxysilane / ethyltriacetoxysilane) (46.96g, 0.207mol Si) was added to siloxane (2200g, 16.13mol Si, DP=127; where "DP " represents the degree of polymerization as determined by NMR) and they were stirred in a glove box at room temperature for 1 hour)....
example 2
[0347] Example 2: M with 3.5 mol% Vi Vi Preparation of Resin-Linear Block Copolymer
[0348] A 1 L dry three-neck round bottom flask was charged with the resin-linear block copolymer (100 g, 0.77 mol Si, 0.138 mol silanol) prepared according to Example 1 in toluene (150 g) and triethylamine (TEA, 5.76 mol) under nitrogen. mL, 0.0414mol) in solution, then stirred for 10 minutes. Vinyldimethylsilyl chloride (5.7 mL, 0.0414 mol) was slowly added to the flask via syringe over 10 minutes. A white salt precipitate formed within 1 minute after the addition of the chlorosilane. The reaction mixture was stirred under nitrogen at room temperature for 3 h, then 1 mL of deionized water was added to quench unreacted chlorosilane. Finally, 5 g of anhydrous Na 2 SO 4 Add to the flask, then stir overnight under air to dry the solution completely. The next day, the reaction solution was filtered with 1.2 μm filter paper at 20 psi to remove white salt precipitates. The solvent was comp...
example 3
[0349] Example 3: M with 2 mol% Vi Vi Preparation of Modified Resin-Linear Block Polymer
[0350] (i) M Vi 0.045 T Ph 0.955 Preparation of the resin: deionized water (1011.9 g) was charged into a 3L three-neck round bottom flask, and then cooled to 4° C. with an ice-water bath. The flask was equipped with a thermometer, a Teflon stirring impeller and a water-cooled condenser. A premixed solution of phenyltrichlorosilane (500.5 g, 2.366 mol), vinyldimethylchlorosilane (15.03 g, 0.125 mol) and toluene (494.4 g) was added to cold water over 2 minutes, followed by removal of the ice Stir for 5 minutes in a water bath (the maximum temperature of the solution during the reaction is at most 74° C.). The reaction mixture was transferred to a 2L round bottom flask fitted with a bottom drain valve, and the aqueous layer was removed. Deionized water (82.4 g) was added to the remaining material, which was then heated at 80° C. for 10 minutes, followed by cooling and removal of th...
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