A kind of siloxane bridging ladder polysiloxane and its preparation method

A technology of siloxane bridge and polysiloxane, which is applied in the field of siloxane bridge ladder polysiloxane and its preparation, can solve the difficulties in the performance of organic polymers, the reduction of the flexibility of trapezoidal double chains, and the high brittleness of polymers, etc. problems, to achieve the effect of good optical performance, high strength and high flexibility

Active Publication Date: 2016-12-28
ETERNAL CHINA INVESTMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of oxygen atoms as bridging groups, the flexibility of the trapezoidal double chains will be reduced, and the brittleness of the polymer will be high. In particular, the general trapezoidal polysilsesquioxane has poor compatibility with organic polymers and is difficult to dissolve in each other. The performance of macromolecules brings difficulties; while the organic bridging ladder polysiloxane (such as phenylene bridging group or phenylene ether bridging base, etc.) has high flexibility and good compatibility with general-purpose organic polymers, which is helpful for improving The performance of organic polymers is very favorable, but its heat resistance is slightly inferior to that of ladder polysilsesquioxane

Method used

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  • A kind of siloxane bridging ladder polysiloxane and its preparation method
  • A kind of siloxane bridging ladder polysiloxane and its preparation method
  • A kind of siloxane bridging ladder polysiloxane and its preparation method

Examples

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Embodiment 1

[0040] Preparation of siloxane bridging ladder polysiloxane by phenyltrichlorosilane and diphenyldihydroxysilane.

[0041] (1) Under the protection of dry nitrogen, put 50.8 grams (0.24 moles) of phenyltrichlorosilane, 150 grams of toluene, and 150 grams of tetrahydrofuran into a multi-necked flask equipped with a condenser tube and a dropping funnel, and stir evenly; Add 26.0 grams (0.12 moles) of diphenyldihydroxysilane to the multi-neck flask in batches at -10°C, and add 26 grams (0.26 moles) of triethylamine dropwise at the same time; after the addition, gradually raise the temperature to 60 ℃ reaction for 1 hour; after stopping the reaction, filter the solution, collect the clear liquid, and obtain an intermediate solution; concentrate the obtained intermediate solution by distillation to obtain an intermediate solution with a concentration of about 30wt%;

[0042] (2) At a temperature of 0°C, add 2.88 grams (0.16 moles) of water and 40.5 grams (0.4 moles) of triethylamin...

Embodiment 2

[0045] Via phenyltrichlorosilane, vinyltrichlorosilane and HO(MePhSiO) 5 H Preparation of siloxane bridging ladder polysiloxane.

[0046] (1) Under the protection of dry nitrogen, 31.7 grams (0.15 moles) of phenyltrichlorosilane, 24.2 grams (0.15 moles) of vinyltrichlorosilane were placed in a multi-necked flask equipped with a condenser tube and a dropping funnel and 500 grams of toluene, stir evenly; at -10 ° C, 83.9 grams of HO (MePhSiO) 5 H (0.12 mol) was added to the multi-neck flask in batches, and 60.7 g (0.6 mol) of triethylamine was added dropwise at the same time; after the dropwise addition, the temperature was gradually raised to 60°C for 3 hours; after the reaction was stopped, the solution was filtered, Collect the supernatant to obtain an intermediate solution;

[0047] (2) At a temperature of 25°C, add 9 grams (0.5 moles) of water and 60.7 grams (0.6 moles) of triethylamine (molecular weight: 101.19) dropwise to the intermediate solution obtained in step (1)....

Embodiment 3

[0050] Via methyltrichlorosilane, 3-acryloyloxytrichlorosilane and HO(MePhSiO) 3 H Preparation of siloxane bridging ladder polysiloxane.

[0051] (1) Under the protection of dry nitrogen, 17.9 grams (0.06 moles) of methyltrichlorosilane and 29.7 grams (0.18 moles) of 3-acryloyloxy 300 grams of trichlorosilane and cyclohexanone, stirred evenly; 51.2 grams of HO(MePhSiO) 3 H (0.12 mol) was added to the multi-neck flask in batches, and 60.7 g (0.6 mol) of triethylamine was added dropwise; after the dropwise addition, the temperature was gradually raised to 60°C for 5 hours; after the reaction was stopped, the solution was filtered, Collect the clear liquid to obtain an intermediate solution; the obtained intermediate solution is concentrated by distillation and then added toluene to obtain an intermediate solution with a concentration of about 30wt%;

[0052] (2) At a temperature of 25°C, add 21.6 grams (1.2 moles) of water and 0.18 grams (0.002 moles) of triethylamine dropwise...

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Abstract

The invention relates to siloxane bridged ladderlike polysiloxane with siloxane as the bridge base and the main chain and a preparation method thereof. The method includes: subjecting RSiX3, R'SiX3 and alpha, omega-silandiol to first step condensation reaction so as to form an intermediate; and then further subjecting the intermediate to second step condensation reaction, and then carrying out separation and purification to obtain the siloxane bridged ladderlike polysiloxane with the following structure. The siloxane bridged ladderlike polysiloxane gives consideration to the high temperature resistance, high strength and high compatibility of a ladderlike polymer and polysiloxane with general organic macromolecules, and by changing the bridge base, the side group, the terminal group and degree of polymerization, the air tightness, adhesion, refraction and other comprehensive performance of the siloxane bridged ladderlike polysiloxane can be regulated. (formula I).

Description

technical field [0001] The invention relates to a ladder-shaped organosilicon polymer, in particular to a siloxane bridging ladder polysiloxane with siloxane as a bridging group and a main chain of siloxane and a preparation method thereof. Background technique [0002] General industrially practical silicone polymers, such as silicone oil and silicone rubber, are polysiloxane polymers whose main chain is a single chain. Compared with general-purpose organic polymers, their outstanding advantage lies in excellent high temperature resistance (temperature resistance) Grade can reach above 200°C), low temperature resistance (below -100°C), radiation resistance, weather resistance and high air permeability, etc. The "ladder silicone polymer" is a polysiloxane polymer (R-LPS) with a double-chain main chain. Compared with the general single-chain polysiloxane polymer, they have better high temperature resistance (temperature resistance Grade can reach above 300°C), radiation resi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/16C08G77/24C08G77/26C08G77/14
Inventor 曹新宇张榕本谢萍方世壁马永梅
Owner ETERNAL CHINA INVESTMENT
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