Preparation method of terminal alkoxy polysiloxane
A technology of alkoxy polysiloxane and polysiloxane, applied in the field of preparation of terminal alkoxy polysiloxane, which can solve the problems of difficult formation of terminal alkoxy polysiloxane and low hydrolysis activity , to achieve the effects of easy control of reaction conditions, reduction of operation steps, and low energy consumption
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Embodiment 1
[0051] In a high-speed disperser, add 100 parts by mass of α,ω-dihydroxy polydimethylsiloxane with a viscosity (25°C) of 650 mPa·s that was cooled to room temperature by dehydration under reduced pressure at 100°C for 3h. 1 H NMR) see attached figure 1 . 4 parts by mass of methyltrimethoxysilane and 2 parts by mass of vinyltrimethoxysilane were added, and after mixing uniformly, the measured viscosity was 473 mPa·s; 1 part by mass of γ-aminopropyltrimethoxysilane, 2 parts by mass of N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane was stirred at a high speed of 2000r / min for 2min under the protection of inert gas. Under the protection of inert gas, it was placed at 50 °C for 2 hours, and the end-capping condition was checked by the rapid titanium reagent chemical method, and there was no viscosity peak phenomenon. The obtained terminal alkoxypolysiloxane had a viscosity of 478 mPa·s, which 1 H NMR see attached figure 2 . Continue to stand for 30 days under the protection o...
Embodiment 2
[0053] In a high-speed disperser, add 600 parts by mass of α,ω-dihydroxy polydimethylsiloxane with a viscosity (25°C) of 17700 mPa·s and 60 parts by mass of α,ω-dihydroxy polydimethylsiloxane and 60 parts by mass of a viscosity (25 ℃) α,ω-dihydroxy polydimethylsiloxane of 150000mPa·s, after uniform dispersion, add 24 parts by mass of tetraethoxysilane and 6 parts by mass of phenyltrimethoxysilane, and after mixing uniformly, the measured viscosity is 18600 mPa·s; 4 parts by mass of N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane and 5 parts by mass of imidazolylpropyltriethoxysilane are added, and the vacuum degree is kept at 0.08~ Under the condition of 0.099MPa, stir at a high speed of 1500r / min for 5min. Keep the vacuum degree at 0.08~0.099MPa, put it at 30°C for 4h, use the rapid titanium reagent chemical method to check the end capping, and there is no viscosity peak phenomenon. The viscosity of the obtained terminal alkoxypolysiloxane was 19400 mPa·s. Continue to s...
Embodiment 3
[0055] In a high-speed disperser, add 1,000 parts by mass of α,ω-dihydroxypolydimethylsiloxane with a viscosity (25°C) of 49,500 mPa·s, 10 parts by mass of vinyltrimethoxysilane, and 30 parts by mass of methyltriethyl Oxysilane, after mixing evenly, the measured viscosity is 42800mPa·s; add 1 part by mass of N-cyclohexyl-γ-aminopropyltrimethoxysilane, 2 parts by mass of piperidinylpropyltriethoxysilane, 2 parts by mass of parts by mass of piperazinylpropyltriethoxysilane, under the protection of inert gas, stirred at a high speed of 800r / min for 15min. Under the protection of inert gas, it was placed at 25 °C for 6 hours, and the end-capping condition was checked by the rapid titanium reagent chemical method, and there was no viscosity peak phenomenon. The viscosity of the obtained terminal alkoxypolysiloxane was 47700 mPa·s. Continue to stand for 30 days under the protection of inert gas, and the measured viscosity is 47900mPa·s. through 1 H NMR analysis, no silanol groups...
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