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Trapezoidal organic poly sesquisiloxane and preparation method

A silsesquioxane and organic technology, applied in the field of preparation of the above-mentioned ladder polyorganosilsesquioxane, can solve the problems of preparation, lack of verification, lack of mature methods and the like

Inactive Publication Date: 2006-07-05
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is not suitable for the preparation of polymers
In 2004, Yamamoto, S. et al. (Macromolecules, 2004, 37, 2775) reported that phenyl trichlorosilane was hydrolyzed and polyphenylsilsesquioxane oligomers (molecular weight 1400, polymerization degree n≈6), speculated to have a trapezoidal structure, but not confirmed
It can be seen that so far soluble, high molecular weight (Mw=10 3 ~10 6 ), highly regular trapezoidal polysilsesquioxane (Δ 1 / 2 <1ppm, means branching can be neglected) There is no mature method to prepare

Method used

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  • Trapezoidal organic poly sesquisiloxane and preparation method
  • Trapezoidal organic poly sesquisiloxane and preparation method
  • Trapezoidal organic poly sesquisiloxane and preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0096] With stirring, a 50ml dioxane solution containing 1.08g (10mmol) PDA was added dropwise to a solution containing 4.3g (20mmol) phenyltrichlorosilane (PhSiCl 3 ) and 6.1g (60mmol) of triethylamine (TEA) in 50ml of chlorobenzene solution, the temperature was maintained at 0°C, after stirring for half an hour, 10ml of dioxane solution containing 0.36ml (20mmol) of water was added dropwise, and stirred at room temperature for 3 Filter after 1 hour, its filtrate removes most of the solvent with a rotary evaporator, adds anhydrous sodium sulfate to dry, takes out the upper layer drying solution, adds a capping agent trimethylchlorosilane 10.8mg (0.10mmol) to end capping, then adds 0.13g of water and and Stir 1-5 drops of concentrated sulfuric acid at 40 degrees for 24 hours, then wash with saturated aqueous sodium chloride until neutral, and dry with anhydrous sodium sulfate to obtain a colorless and transparent toluene solution of trapezoidal polyphenylsilsesquioxane. 15mg / m...

Embodiment 2

[0098] With stirring, a solution of 25ml of dioxane containing 1.08g (10mmol) of PDA was added dropwise to a solution containing 3.0g (20mmol) of methyltrichlorosilane (MeSiCl 3 ) and 6.1g (60mmol) triethylamine (TEA) in 40ml of toluene solution, the temperature is controlled at about -15°C, stirred for half an hour, and then 20ml dioxane solution containing 0.36ml (20mmol) water is added dropwise to the reaction bottle, stirred at room temperature for 4 hours and filtered, and the filtrate was removed with a rotary evaporator to remove most of the solvent, dried with anhydrous sodium sulfate, filtered to obtain the filtrate and added 10.8 mg (0.10 mmol) of capping agent trimethylchlorosilane under stirring. Then add 0.23g of water and 1-5 drops of concentrated sulfuric acid, stir at room temperature for three hours, raise the temperature to 80-90°C and stir for 5 hours, then wash with saturated aqueous sodium chloride until neutral, and dry with anhydrous sodium sulfate to obt...

Embodiment 3

[0100] Under stirring, 50ml of dioxane solution containing 2.16g (20mmol) pre-aminolysis agent PDA was added dropwise to 6.5g (40mmol) vinyl trichlorosilane (CH 2 =CHSiCl 3 ) and 12.2g (120mmol) of triethylamine (TEA) in 80ml of chlorobenzene solution, the temperature was maintained at about -20°C, after the dropwise addition was completed, the stirring was continued for half an hour, and then the 10ml of tetrahydrofuran solution containing 0.72g (40mmol) of water was slowly Add it dropwise into the reaction flask, stir for 4 hours, filter, remove 1 / 2 of the solvent with a rotary evaporator for the filtrate, and wash the remaining chlorobenzene solution with anhydrous Na 2 SO 4 Dry, take the supernatant liquid with 21.8mg (0.20mmol) trimethylsilyl chloride (Me 3 SiCl) head, add 0.6g of water and 1-5 drops of concentrated sulfuric acid for dehydration condensation, stir at room temperature for 24 hours, wash with saturated aqueous sodium chloride solution until neutral, and t...

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Abstract

A preparation method for highly tactic ladder-like polysilsequioxane with solubility, high molecular weight and different organic side groups is introduced in this invention. Trichlorosilicane with different substituents reacts with template-1, 4-dianiline or its derivatives with ladder-brace template method to produce conjugate precursor containing four silicon-chlorine bonds, which self-assembles into ladder polymers by hydrogen bond template function of p-dianiline and transforms into silanol end-capping organic bridging siloxane polymers after hemihydration-hydrolysis-condensation. Such a compound is then end-capped with trimethylsiloxyl and hydrolyzed to remove p-dianiline, and ladder-like polysilsequioxane can be obtained after further condensation. Or tetrafunctional disiloxane monomers with template-function side groups self-assemble into ladder-like polymers, which are then condensation-polymerized and end-capped with trimethylsiloxyl to obtain ladder-like polysilsequioxane.

Description

technical field [0001] The present invention relates to a ladder polyorganosilsesquioxane. [0002] The present invention also relates to a method for preparing the above-mentioned ladder polyorganosilsesquioxane. Background technique [0003] In 1960, Brown, J.F. et al. (J.Amer.Chem.Soc., 1960, 82, 6194) reported for the first time that phenyltriethoxysilane (PhSi(OEt) 3 ) hydrolyzate using potassium hydroxide as a catalyst to prepare trapezoidal polyphenylsilsesquioxane (LPPS) through "equilibrium thermal polycondensation" at 250°C. In 1970, Frye, C.L. (J.Amer.Chem.Soc., 1971, 93, 4599) pointed out that the LPPS obtained by this method is not a real trapezoidal polymer, but "short-range order, long-range disorder, containing partially open Polycyclic cages", that is, depending on the synthesis conditions, there are different degrees of branching. In 2002, Matsumoto, H. et al. (J.Amer.Chem.Soc., 1971, 93, 4599) reported that the polysilsesquioxane hexamer whose side grou...

Claims

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Application Information

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IPC IPC(8): C08G77/04C08G77/06
Inventor 张韬毅邓奎林张晓静杜晨光张爱芹谢萍张榕本
Owner INST OF CHEM CHINESE ACAD OF SCI
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