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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

Active Publication Date: 2022-07-29
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem that single-ended trialkoxysiloxy-terminated polysiloxane has not yet been commercialized due to the influence of raw material sources and other factors, the present invention proposes a single-ended trialkoxysiloxy-terminated polysiloxane The preparation method of the oxane fluid, the prepared single-ended trialkoxysiloxy-terminated polysiloxane fluid has high purity, regular structure, low viscosity, high filling density of powder filler and easy mixing uniformly, and the preparation method is easy for industrial production

Method used

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  • A kind of preparation method of single-ended trialkoxysiloxy-terminated polysiloxane fluid
  • A kind of preparation method of single-ended trialkoxysiloxy-terminated polysiloxane fluid
  • A kind of preparation method of single-ended trialkoxysiloxy-terminated polysiloxane fluid

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Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to the field of organic synthesis. In order to solve the problem that currently single-ended trialkoxysiloxy-terminated polysiloxane has not been commercialized due to the influence of raw material sources and other factors, the present invention proposes a single-ended trialkoxy The preparation method of siloxy-terminated polysiloxane fluid, the prepared single-end trialkoxysiloxy-terminated polysiloxane fluid has high purity, regular structure, low viscosity, high packing density of powder filler and easy mixing uniform, and the preparation method is easy for industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of a single-ended trialkoxysiloxy-terminated polysiloxane fluid. Background technique [0002] The single-ended trialkoxysiloxy-terminated polysiloxane fluid is also called single-ended trialkoxysiloxy-terminated silicone oil, which means that one end of the polysiloxane molecule is end-capped with an inert organic functional group, and the other end is end-capped with an inert organic functional group. Terminated with trialkoxysiloxy and the polymer repeating unit chain is [R 1 R 2 SiO 2 / 2 ] linear or branched silicone polymers where R 1 and R 2 Representing the same or different saturated alkyl or unsaturated alkenyl, alkynyl functional groups, the structural formula of the single-ended trialkoxysiloxy-terminated polysiloxane fluid is shown in formula (1): [0003] [0004] where R a including methyl or ethyl, R b represents n-butyl group, and n r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/18C08G77/06
CPCC08G77/18C08G77/06
Inventor 瞿志荣薛启浩苏锦华伍川董红肖顺超苏腾刘清月
Owner HANGZHOU NORMAL UNIVERSITY