Siloxane bridged silane terminated siloxane bridged ladder like polysiloxane and preparation method thereof

A technology of siloxane bridge and polysiloxane is applied in the field of siloxane bridge ladder polysiloxane, which can solve the problems of high price, difficult to complete end capping, difficult practical application and the like.

Active Publication Date: 2018-04-06
ETERNAL CHINA INVESTMENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are the following problems at present, including: generally used end-capping agents are monofunctional silanes (such as trimethylsiloxy, etc.), which limit their heat resistance; end-cappi

Method used

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  • Siloxane bridged silane terminated siloxane bridged ladder like polysiloxane and preparation method thereof
  • Siloxane bridged silane terminated siloxane bridged ladder like polysiloxane and preparation method thereof
  • Siloxane bridged silane terminated siloxane bridged ladder like polysiloxane and preparation method thereof

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preparation example Construction

[0113]Preferably, the preparation method of the siloxane bridging silane-terminated siloxane bridging ladder polysiloxane of the present embodiment comprises the following steps: combining structural formulas (2), (3) and (4) silanes (that is, four Functional I-shaped siloxane bridging siloxane monomer and bifunctional I-shaped siloxane bridging silane capping agent) are co-hydrolyzed in the presence of solvents, catalysts, and water, relying on supramolecular weak bond interactions (including π-π superposition, electron donor and acceptor, electrostatic, hydrophilic and hydrophobic, and hydrogen bond interactions) form a trapezoidal superstructure to regulate the polymerization and capping reaction of hydrolyzate to obtain siloxane bridging silane-capped siloxane Alkyl Bridged Ladder Polysiloxane. The preparation method comprises the following steps:

[0114] Add structural formula (2) (3) and (4) silane, solvent, water and catalyst to the reactor in a dropwise or "one-pot c...

Embodiment 1

[0155] Example 1: Ph 2 -I-Ph-SLPS synthesis

[0156] A siloxane bridging silane terminated siloxane bridging ladder polysiloxane was prepared from phenyltrimethoxysilane, diphenyldimethoxysilane and diphenylsilanediol.

[0157] Under the protection of dry nitrogen, 39.6 grams of phenyltrimethoxysilane (0.20mol), 21.6 grams of diphenylsilanediol (0.01mol) and 15 grams of ethyl acetate were placed in a constant pressure dropping funnel equipped with mechanical stirring and a three-necked flask with a reflux condenser, stirred evenly at room temperature, added 0.02 g of triethanolamine at 0°C, and reacted for 8 hours to obtain intermediate 1; at the same time, in another protected by dry nitrogen, equipped with mechanical stirring, constant pressure drop Add 41.9 grams of diphenyldimethoxysilane (0.17mol), 10 grams of ethyl acetate, and 18.6 grams of diphenylsilanediol (0.09mol) into the three-necked flask of the funnel and the reflux condenser, and stir evenly. Add 0.04 g of t...

Embodiment 2

[0159] Embodiment 2: Synthesis of PhMe-I-Ph-SLPS

[0160] A siloxane bridging silane terminated siloxane bridging ladder polysiloxane was prepared from phenyltrimethoxysilane, methylphenyldimethoxysilane and diphenylsilanediol.

[0161] Under the protection of dry nitrogen, 39.6 grams of phenyltrimethoxysilane (0.20mol), 21.6 grams of diphenylsilanediol (0.10mol) and 10 grams of N,N-dimethylacetamide were placed in a mechanically stirred , a constant pressure dropping funnel and a three-necked flask with a reflux condenser, stir evenly at room temperature, add 0.10 g of liquid ammonia at -5°C, and react for 12 hours to obtain Intermediate 1; Add 3.65 grams of methylphenyldimethoxysilane (0.02mol), 10 grams of N,N-dimethylacetamide, 2.16 grams of diphenylsilane into the three-necked flask with stirring, constant pressure dropping funnel and reflux condenser Diol (0.01mol) was stirred evenly, and 0.02 gram of liquid ammonia was added at 0° C., and reacted for 18 hours to obtain...

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Abstract

The invention relates to siloxane bridged silane terminated siloxane bridged ladder-like polysiloxane and a preparation method thereof. The invention provides siloxane bridged silane (namely bifunctional I-shaped silane) terminated siloxane bridged ladder-like polysiloxane and a preparation method thereof. Tetra-functional I-shaped siloxane bridged siloxane monomers and a bifunctional I-shaped siloxane bridged silane end-capping reagent are co-hydrolyzed, and a ladder like super-structure formed by the supermolecule weak bond synergistic effect is used to modulate the polymerization and end capping reactions of hydrolysis products so as to obtain the siloxane bridged silane terminated siloxane bridged ladder like polysiloxane represented by the formula. Compared with common mono-functionalsiloxane bridged silane terminated siloxane bridged ladder like polysiloxane, the polymerization degree and end-capping degree of the bifunctional I-shaped siloxane bridged silane terminated siloxanebridged ladder-like polysiloxane can be effectively controlled. The polymer has the advantages of excellent heatproof property, good mechanical properties, and good compatibility with organic polymer. The end-capping mode has the advantages of simple and easily-available raw materials, low cost, and suitability for industrialization.

Description

technical field [0001] The invention relates to a siloxane bridging ladder polysiloxane, in particular to a siloxane bridging silane-terminated siloxane bridging ladder polysiloxane and a preparation method thereof. Background technique [0002] Generally, the ladder silicone polymer has a double-chain ladder structure. Although the main chain of the ladder will break due to external influence, statistically speaking, the possibility of simultaneous breakage of the upper and lower single chains of the same ladder is very small. Therefore, compared with general single-chain silicone polymers, it shows more excellent properties in terms of heat resistance, radiation resistance, chemical resistance, mechanical and biological effects. [0003] The development of trapezoidal organopolysiloxane is divided into three stages according to the different bridging structures: the first generation is the oxygen bridging ladder ladder polysiloxane (that is, trapezoidal polysilsesquioxane...

Claims

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Application Information

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IPC IPC(8): C08G77/04C08G77/14C08G77/20C08G77/06
CPCC08G77/04C08G77/06C08G77/14C08G77/20
Inventor 潘赏曹菁张榕本方世壁
Owner ETERNAL CHINA INVESTMENT
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