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Method for preparing trapezoidal phenyl polysiloxane

A technology of phenyl polysiloxane and trapezoid is applied in the field of preparation of trapezoidal phenyl polysiloxane, which can solve the problems of high cost and complicated synthesis process, and achieve simple reaction steps, strong operability, and easy industrialization. Effect

Inactive Publication Date: 2010-01-13
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product ladder-shaped phenyl polysiloxane is highly ordered, but the synthesis process is complex and expensive

Method used

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  • Method for preparing trapezoidal phenyl polysiloxane
  • Method for preparing trapezoidal phenyl polysiloxane
  • Method for preparing trapezoidal phenyl polysiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) 10ml (0.054mol) phenyltrimethoxysilane (C 6 h 5 Si(OCH 3 ) 3 ) after being dissolved in 60ml of toluene (the concentration of the monomer in the solvent is 1mol / kg), stirring and adding dropwise 15ml (0.833mol) of water and 0.151ml of a mixed solution of mass concentration of 36.5% hydrochloric acid at a rate of 2 drops / min (PH=3) at the same time (the molar ratio of water and monomer is 15:1), react at 10°C for 24h;

[0034] 2) The reaction solution in step 1) was allowed to stand for stratification, and after removing the lower aqueous phase, the upper toluene phase was washed with ultrapure water until the pH of the washing solution was ≈7;

[0035] 3) Rotate the excess solvent in the toluene phase after washing with water and add 2ml of methanol solution (PH=13) of KOH with a concentration of 1g / ml (the consumption of the basic catalyst is 5wt% of the oil phase system after washing), in Reflux at 80°C for 8h;

[0036] 4) After concentrating the polymer organ...

Embodiment 2

[0038] 1) 10ml (0.054mol) phenyltrimethoxysilane (C 6 h 5 Si(OCH 3 ) 3) was dissolved in 60ml of toluene (the concentration of the monomer in the solvent was 1mol / kg), stirred and added dropwise at a rate of 2 drops / minute a mixture of 9.72ml (0.54mol) water and 0.1ml mass concentration of 36.5% hydrochloric acid Solution (PH=3) at the same time (the molar ratio of water and monomer is 10:1), react at -15°C for 10h;

[0039] 2) with step 2) in embodiment 1;

[0040] 3) Rotate the excess solvent in the toluene phase after washing with water and add 2ml of methanol solution (PH=13) of KOH with a concentration of 1g / ml (the consumption of the basic catalyst is 5wt% of the oil phase system after washing), in Reflux at 25°C for 5h;

[0041] 4) After concentrating the polymer organic solution by rotary evaporation, add 2 times the volume of the concentrated solution to precipitate methanol, and vacuum-dry the precipitate to obtain white trapezoidal phenyl polysiloxane powder. ...

Embodiment 3

[0043] 1) 10ml (0.054mol) phenyltrimethoxysilane (C 6 h 5 Si(OCH 3 ) 3 ) was dissolved in 60ml of toluene (the concentration of the monomer in the solvent was 1mol / kg), stirred and added dropwise at a rate of 2 drops / minute a mixture of 5.832ml (0.324mol) water and 0.06ml mass concentration of 36.5% hydrochloric acid Solution (PH=3) at the same time (the molar ratio of water and monomer is 6:1), react at 0°C for 16h;

[0044] 2) with step 2) in embodiment 1;

[0045] 3) Rotate the excess solvent in the toluene phase after washing with water and add 2ml of methanol solution (PH=13) of KOH with a concentration of 1g / ml (the consumption of the basic catalyst is 5wt% of the oil phase system after washing), in Reflux at 60°C for 3h;

[0046] 4) After concentrating the polymer organic solution by rotary evaporation, add 2 times the volume of the concentrated solution to precipitate methanol, and vacuum-dry the precipitate to obtain white trapezoidal phenyl polysiloxane powder. ...

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Abstract

The invention relates to a method for preparing trapezoidal phenyl polysiloxane, which belongs to the field of preparing polymer materials. The prior trapezoidal phenyl polysiloxane has poor regularity and poor solubility. The method comprises the following steps: dissolving a C6H5-Si-(OR1)(OR2)(OR3) monomer into an organic solvent, and then adding acidic aqueous solution into the mixture to perform hydrolytic condensation so as to obtain a prepolymer, wherein R1, R2 and R3 are selected from hydrogen, methyl or ethyl respectively; standing and demixing the prepolymer solution, then washing an oil phase system into neutral with water, adding a basic catalyst into the mixture, and performing condensation reaction at a temperature of between 25 and 100 DEG C for 3 to 8 hours; and concentrating the reaction solution, and adding methanol into the reaction solution for sedimentation and drying to obtain the trapezoidal phenyl polysiloxane. The method has the advantages of simple reaction steps, strong operability, innocuity and no contamination, easy industrialization, high trapezoidal regularity of products, good solubility and the like.

Description

technical field [0001] The invention belongs to the field of polymer material preparation, and in particular relates to a preparation method of trapezoidal phenylpolysiloxane. Background technique [0002] Ladder polysiloxane polymers containing one phenyl side chain and 1.5 oxygen atoms per silicon atom are referred to as ladder polysiloxanes. The trapezoidal structure endows phenyl polysiloxane with good electrical insulation, optical transparency, water resistance, flame retardancy and heat resistance, weather resistance, water resistance and chemical resistance. [0003] There have been many reports on the synthesis and application of ladder-shaped phenylpolysiloxanes. [0004] The traditional method is to use the hydrolyzate of trichlorosilane-type monomer as raw material, and use the "thermal equilibrium polycondensation method" under alkaline and high temperature conditions to synthesize phenyl polysiloxane with high molecular weight, such as US5081202 and US6008310....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/16
Inventor 武德珍冯玉仲吴战鹏刘婧婧杨小平
Owner BEIJING UNIV OF CHEM TECH
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