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

Synthetic method of hexamine phenyl large ring oligomerization silsesquioxane

A technology of polysilsesquioxane and hexaaminephenyl, which is applied in the field of polymer material synthesis to achieve mild reaction conditions, broad application prospects, and extensive functionalization

Active Publication Date: 2016-02-03
SHANGHAI JIAO TONG UNIV
View PDF2 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, currently, there are few literature reports on the synthesis method of aromatic amino-terminated macrocyclic oligomerized silsesquioxanes.

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
  • Synthetic method of hexamine phenyl large ring oligomerization silsesquioxane
  • Synthetic method of hexamine phenyl large ring oligomerization silsesquioxane
  • Synthetic method of hexamine phenyl large ring oligomerization silsesquioxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Preparation of sodium nickel / salt hexasilicate

[0039] 7.7300g of phenyltrimethoxysilane, 1.8000g of NaOH and 0.7000g of H 2 O was added to 130.0000 mL of n-butanol and refluxed for 1.5 hours. After cooling slightly, add 3.0100g hexaamine nickel dichloride at one time, and then reflux for 2 hours. The NaCl salt was filtered off, part of the n-butanol was removed by rotary evaporation, and the orange crystals were precipitated at 0°C overnight. After being obtained by suction filtration, it was vacuum-dried at 80° C. for 1 hour. Weighed 5.4400g, yield 71.8000%.

[0040] (2) Preparation of alkenyl-terminated macrocyclic oligomerized silsesquioxane (hexavinylhexaphenylcyclohexasiloxane)

[0041] 35.0000 mL of dry toluene, 5.5400 mL of dry pyridine and 10.3200 g of vinyl dimethyl chlorosilane were successively added into a 100 mL flask. After 5 minutes, 1.3000 g of sodium / nickel hexaphenylcyclohexasilate was added. After reacting at room temperature for 24 hours,...

Embodiment 2

[0048] (1) Preparation of sodium nickel / salt hexasilicate

[0049] 7.7300g of phenyltrimethoxysilane, 1.8000g of NaOH and 0.7000g of H 2 O was added to 130.0000 mL of n-butanol and refluxed for 1.5 hours. After cooling slightly, add 3.0100g hexaamine nickel dichloride at one time, and then reflux for 2 hours. The NaCl salt was filtered off, part of the n-butanol was removed by rotary evaporation, and the orange crystals were precipitated at 0°C overnight. After being obtained by suction filtration, it was vacuum-dried at 80° C. for 1 hour. Weighed 5.4400g, yield 71.8000%.

[0050] (2) Preparation of alkenyl-terminated macrocyclic oligomerized silsesquioxane (hexavinylhexaphenylcyclohexasiloxane)

[0051] 35.0000 mL of dry toluene, 5.5400 mL of dry pyridine and 10.3200 g of vinyl dimethyl chlorosilane were successively added into a 100 mL flask. After 5 minutes, 1.3000 g of sodium / nickel hexaphenylcyclohexasilate was added. After reacting at room temperature for 24 hours,...

Embodiment 3

[0057] (1) Preparation of sodium nickel / salt hexasilicate

[0058] 7.7300g of phenyltrimethoxysilane, 1.8000g of NaOH and 0.7000g of H 2 O was added to 130.0000 mL of n-butanol and refluxed for 1.5 hours. After cooling slightly, add 3.0100g hexaamine nickel dichloride at one time, and then reflux for 2 hours. The NaCl salt was filtered off, part of the n-butanol was removed by rotary evaporation, and the orange crystals were precipitated at 0°C overnight. After being obtained by suction filtration, it was vacuum-dried at 80° C. for 1 hour. Weighed 5.4400g, yield 71.8000%.

[0059] (2) Preparation of alkenyl-terminated macrocyclic oligomerized silsesquioxane (hexavinylhexaphenylcyclohexasiloxane)

[0060] 35.0000 mL of dry toluene, 5.5400 mL of dry pyridine and 10.3200 g of vinyl dimethyl chlorosilane were successively added into a 100 mL flask. After 5 minutes, 1.3000 g of sodium / nickel hexaphenylcyclohexasilate was added. After reacting at room temperature for 24 hours,...

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

PropertyMeasurementUnit
dielectric lossaaaaaaaaaa
Login to View More

Abstract

The invention relates to a synthetic method of hexamine phenyl large ring oligomerization silsesquioxane. The method comprises the steps that silane, sodium hydroxide and hexamine nickel dichloride serve as raw materials for generating hex-nickel sodium silanolate through a reaction, then alkenyl-terminated large ring oligomerization silsesquioxane is generated through a reaction of hex-nickel sodium silanolate and alkenyl-terminated chlorosilane, then a coupling reaction is conducted through alkenyl-terminated large ring oligomerization silsesquioxane and bromo-arylamine compounds under the action of catalysts and coordination compounds, and the hexamine phenyl large ring oligomerization silsesquioxane is obtained. Compared with the prior art, The synthetic method is simple in synthesis step, mild in condition, good in controllability, short in cycle and high in yield, the obtained hexamine phenyl large ring oligomerization silsesquioxane can be used for modification of thermosetting resin or thermoplastic resin, and good application prospect is achieved.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and relates to a synthesis method of hexaaminephenyl macrocyclic oligomerized silsesquioxane. Background technique [0002] At present, in the field of silsesquioxane research, oligomeric silsesquioxane (POSS) is a three-dimensional spherical inorganic nano-macromolecule with a regular structure composed of eight silicon atoms and 12 oxygen atoms. Its structural formula for [R 8 Si 8 o 12 ], has become a research hotspot in engineering materials, porous materials, low dielectric materials and other fields. Cyclic oligomeric silsesquioxane is a class of oligomeric silsesquioxane (MOSS) with a three-dimensional ring structure, and its inorganic properties are similar to those of polyhedral oligomeric silsesquioxane (POSS). Oxygen skeleton. Compared with the synthesis of POSS, the synthesis of MOSS has the characteristics of simple method, short cycle time and high yield, and...

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): C07F7/10C08G73/10C08G59/50C08G69/28C08K5/544C08J5/18
Inventor 郑思珣刘宁
Owner SHANGHAI JIAO TONG 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