Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of cage poly (phenylsilsequioxane)

A technology of polysilsesquioxane and phenyltrialkoxysilane, which is applied in the field of organic-inorganic hybrid materials, can solve the problems of complex structure of raw material monomers and low product yield, and achieve industrial scale production, The effect of high reuse rate and short reaction cycle

Active Publication Date: 2012-08-22
SHANDONG UNIV
View PDF4 Cites 17 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the shortcomings of the prior art, such as low product yield and complex structure of raw material monomers, the present invention provides a cage with easy-to-obtain raw materials, mild reaction conditions, simple operation, short reaction cycle, high yield, low cost and environmentally friendly process. Type octaphenyl polysilsesquioxane preparation method

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of cage poly (phenylsilsequioxane)
  • Preparation method of cage poly (phenylsilsequioxane)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 200.0mL ethanol and 20.0mL phenyltriethoxysilane monomer into a 500.0mL three-necked round-bottom flask, stir and mix evenly, add 15.0mL hydrochloric acid (36.0wt%) dropwise to the above mixed solution within 40min, and keep stirring Speed, control the reaction temperature at 55 ° C, hydrolysis polycondensation 72h. After the reaction was completed, it was lowered to room temperature, and the reaction mother liquor was removed by filtration to obtain a white powdery solid. The obtained solid was washed with methanol, recrystallized from dichloromethane, and vacuum-dried to obtain 6.88 g of a solid product with a yield of 64.3%.

[0031] Structural characterization data: FTIR, 1110cm -1 (νSi-O-Si), 1135cm -1 (νSi-C), 3094cm -1 , 3073cm -1 and2924cm -1 (νC-H), 1595cm -1 and 1491cm -1 (νC=C); 1 H-NMR, δ=7.802-7.399, (CDCl 3 ); 13 C-NMR, 135.89ppm, 130.14ppm and 128.53ppm (CDCl 3 ); 29 Si-NMR, -78.47ppm (CDCl 3 ).

Embodiment 2

[0033] Add 240.0 mL of methanol and 9.0 mL of concentrated hydrochloric acid (28.0 wt %) into a 500.0 mL three-necked round-bottom flask, and stir to mix evenly. Under mechanical stirring, 25.0 mL of phenyltrimethoxysilane monomer was added dropwise into the mixed solution within 30 minutes, the reaction temperature was controlled at 35° C., and hydrolysis and polycondensation were allowed to stand for 76 hours. After the reaction was completed, it was lowered to room temperature, and the reaction mother liquor was removed by filtration to obtain a white powdery solid. The obtained solid was washed with methanol, recrystallized with dichloromethane, and vacuum-dried to obtain 9.42 g of a solid product with a yield of 70.4%.

Embodiment 3

[0035] Add 280.0 mL of isopropanol and 20.0 mL of concentrated hydrochloric acid (30.0 wt %) into a 500.0 mL three-neck round bottom flask, and stir to mix evenly. Under mechanical stirring, 30.0 mL of phenyltriethoxysilane monomer was added dropwise into the mixed solution within 35 minutes, the reaction temperature was controlled at 50° C., the stirring speed was constant, and hydrolysis and polycondensation were carried out for 82 hours. After the reaction was completed, it was lowered to room temperature, and the reaction mother liquor was removed by filtration to obtain a white powdery solid. The solid obtained by washing with ethanol was recrystallized with a mixed solvent of dichloromethane and acetone (3:1 volume ratio), and vacuum-dried to 15.09 g solid product, yield 72.7%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a preparation method of cage poly (octaphenylsilsequioxane). The method is characterized in that phenyltriethoxysilane or phenyltrimethoxysilane is used as a monomer raw material, organic alcohol is used as solvent and the cage poly (phenylsilsequioxane) is prepared through one-step hydrolytic polycondensation under the catalytic effect of hydrochloric acid. The method provided by the invention has the advantages that the raw material is easy to obtain, the reaction conditions are moderate, the operation is simple and convenient to conduct, the reaction period is short, the yield is high, the cost is low, the method is an environmental-friendly poly (octaphenylsilsequioxane) synthesis method and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a synthesis method of cage-type polysilsesquioxane, in particular to a preparation method of cage-type octaphenyl oligomeric silsesquioxane, which belongs to the field of organic-inorganic hybrid materials. Background technique [0002] The chemical formula of cage octaphenyl polysilsesquioxane is [C 6 h 5 SiO 3 / 2 ] 8 , structure such as formula I. , [0003] [0004] The Si atoms on the eight corners of the cage octaphenyl polysilsesquioxane hexahedral structure are respectively connected with phenyl groups, which has excellent thermal stability. Compared with commonly used fillers, the phenyl groups connected to the outside of the cage-type octaphenylpolysilsesquioxane skeleton improve the compatibility with organic polymers, and the dispersion is better. Therefore, the cage octaphenyl polysilsesquioxane can be introduced into other materials to improve or enhance the performance of the materials. When introduced in...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 朱庆增李正强刘慧
Owner SHANDONG UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com