A kind of synthetic method of methylphenyl silicone oil
A technology of methyl phenyl silicone oil and synthesis method, which is applied in the field of synthesis of methyl phenyl silicone oil to achieve the effects of narrow molecular weight distribution, moderate viscosity and good stability
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[0024] A synthetic method of methyl phenyl silicone oil, comprising the following steps:
[0025] 1) Mix methylphenyldimethoxysilane and tetramethyldivinyldisiloxane, heat up to 60°C-80°C and stir to react, then add alkali solution, reflux reaction, then heat up to 100°C-105 ℃ decompression reaction, and then heated to 108 ℃ ~ 112 ℃ reaction, drying;
[0026] 2) Filter the silicone oil product obtained in step 1), add lower alcohol to wash, remove the alcohol layer after layering, distill the silicone oil layer under reduced pressure to remove the solvent lower alcohol, and obtain methylphenyl silicone oil.
[0027] Preferably, in step 1), the molar ratio of methylphenyldimethoxysilane to tetramethyldivinyldisiloxane is (10-30):1.
[0028] Preferably, in step 1), the time for heating up to 60°C-80°C for stirring and reacting is 8min-15min; the time for reflux reaction is 1.8-2.5h; 4.5h; the time to heat up to 108°C-112°C is 0.8-1.5h; more preferably, in step 1), specifically...
Embodiment 1
[0039] Add 182g of methylphenyldimethoxysilane and 6.84g of tetramethyldivinyldisiloxane into the reaction flask, raise the temperature to 70°C, mix and stir for 10min, then add 40g of 1.5% KOH aqueous solution dropwise, Reflux for 2 hours, then raise the temperature to 100°C, react under reduced pressure for 4 hours, then raise to 110°C, react for 1 hour, and end the reaction. Add anhydrous MgSO 4 dry. After the above silicone oil product was filtered under reduced pressure, 80 mL of absolute ethanol was added to wash it once, the ethanol layer was removed by layering, and the low boilers were removed from the silicone oil layer under reduced pressure to obtain a colorless and transparent high-refraction methylphenyl silicone oil product. The ratio is 1.55 and the viscosity is 1500cP. attached figure 1 It is the nuclear magnetic spectrum of the methylphenyl silicone oil product that embodiment 1 obtains.
Embodiment 2
[0041] Add 182g of methylphenyldimethoxysilane and 5.7g of tetramethyldivinyldisiloxane into the reaction flask, raise the temperature to 70°C, mix and stir for 10min, then add 30g of 1.5% KOH aqueous solution dropwise, Reflux for 2 hours, then raise the temperature to 100°C, react under reduced pressure for 4 hours, then raise to 110°C, react for 1 hour, and end the reaction. Add anhydrous MgSO 4 dry. After the above silicone oil product was filtered under reduced pressure, 80 mL of absolute ethanol was added to wash it once, the ethanol layer was removed by layering, and the low boilers were removed from the silicone oil layer under reduced pressure to obtain a colorless and transparent high-refraction methylphenyl silicone oil product. The ratio is 1.56 and the viscosity is 1550cP.
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