A kind of preparation method of single-ended trialkoxysiloxy-terminated polysiloxane fluid
A technology of trialkoxysiloxy sealing and trialkoxychlorosilane, which is applied in the field of preparation of polysiloxane fluids, can solve the problems of unrealized commercialization, and achieve regular structure, low toxicity and high thermal conductivity Effect
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Embodiment 1
[0037] In the 250mL there-necked flask under the protection of dry nitrogen, adding 16mL water content is tetrahydrofuran (THF mole number is 0.197mol) of 400ppm, the there-necked flask is placed in the low temperature tank of-10 ℃ and the stirring is opened, and the 16mL concentration is 2.5mol / L of n-butyllithium hexane solution (n-butyllithium effective content of 0.04mol) was injected into the three-necked flask at a rate of 1mL / min, and maintained at -10°C for 90min after the injection; The tetrahydrofuran solution of trisiloxane (50 g (0.225 mol) of hexamethylcyclotrisiloxane was dissolved in 50 mL of tetrahydrofuran solution with a water content of 400 ppm (the number of moles of tetrahydrofuran was 0.615 mol)) was uniformly added dropwise to the In the three-necked flask of the above reaction mixture, after the dropwise addition was completed, it was maintained at -10°C for 60min; then the temperature of the reaction mass was raised to 25°C, and the reaction was contin...
Embodiment 2
[0040] To the 250mL there-necked flask under the protection of dry nitrogen, add 32mL of tetrahydrofuran with a water content of 50ppm, place the there-necked flask in the low-temperature tank of -20°C and turn on stirring, and 16mL concentration is the n-butyllithium hexane of 2.5mol / L. The solution (n-butyllithium effective content of 0.04mol) was injected into the three-necked flask at a rate of 2mL / min, and maintained at -20°C for 20min after the injection; then the pre-prepared tetrahydrofuran solution of hexamethylcyclotrisiloxane ( 50g (0.225mol) of hexamethylcyclotrisiloxane was dissolved in 100mL of tetrahydrofuran solution with a water content of 50ppm) was uniformly added dropwise to the there-necked flask containing the above-mentioned reaction mixture for 20min, after the dropwise addition, in- Maintained at 20°C for 20min; then the temperature of the reaction material was raised to 30°C, and the reaction was continued at this temperature for 6h; then 38.8mL (0.269...
Embodiment 3
[0043] To the 2000mL there-necked flask under the protection of dry nitrogen, add 120mL of tetrahydrofuran with a water content of 100ppm, place the there-necked flask in the low temperature tank of -30 ℃ and turn on stirring, and 80mL concentration is the n-butyl lithium hexane of 2.5mol / L. The solution (n-butyllithium effective content of 0.2mol) was injected into the three-necked flask at a rate of 5mL / min, and maintained at -30°C for 30min after the injection; then the pre-prepared tetrahydrofuran solution of hexamethylcyclotrisiloxane ( 250g (1.13mol) of hexamethylcyclotrisiloxane was dissolved in 375mL of tetrahydrofuran solution with a water content of 100ppm) uniformly added dropwise to the there-necked flask containing the above-mentioned reaction mixture for 20min, after the dropwise addition, in- Maintained at 30°C for 30min; then the temperature of the reaction mass was raised to 35°C, and the reaction was continued for 8h at this temperature; then 179mL (1.24mol) t...
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