Synthetic method of hexaaminephenyl macrocyclic oligomerized silsesquioxane

A technology of polysilsesquioxane and hexaaminephenyl, which is applied in the direction of silicon organic compounds, etc., to achieve the effect of less by-products, simple synthesis steps and high yield

Active Publication Date: 2018-09-11
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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

Method used

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  • Synthetic method of hexaaminephenyl macrocyclic oligomerized silsesquioxane
  • Synthetic method of hexaaminephenyl macrocyclic oligomerized silsesquioxane
  • Synthetic method of hexaaminephenyl macrocyclic oligomerized silsesquioxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0039] 7.7300g phenyltrimethoxysilane, 1.8000g NaOH and 0.7000g 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, the whit...

Embodiment 2

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

[0049] 7.7300g phenyltrimethoxysilane, 1.8000g NaOH and 0.7000g 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, the whit...

Embodiment 3

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

[0058] 7.7300g phenyltrimethoxysilane, 1.8000g NaOH and 0.7000g 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 whit...

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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

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21C08G73/10C08G59/50C08G69/28C08K5/544C08J5/18
Inventor 郑思珣刘宁
Owner SHANGHAI JIAOTONG UNIV
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