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Synthetic method of diaminophenyl double splint cage silsesquioxane

A technology of silsesquioxane and diaminophenyl, which is applied in the field of synthesis of diaminophenyl double splint cage silsesquioxane to achieve the effects of less by-products, simple synthesis steps and low drying degree

Active Publication Date: 2018-06-29
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the synthesis of aromatic amino-terminated double splint cage silsesquioxanes

Method used

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  • Synthetic method of diaminophenyl double splint cage silsesquioxane
  • Synthetic method of diaminophenyl double splint cage silsesquioxane
  • Synthetic method of diaminophenyl double splint cage silsesquioxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Preparation of tetrasilanol sodium salt

[0042] In a 500mL single-necked flask equipped with a magnet, add 31.7000g of phenyltrimethoxysilane, 160.0000mL of isopropanol, 3.3300g of deionized water and 4.2800g of sodium hydroxide in sequence, react at 85°C for 4 hours, cool Stirring was continued at room temperature for 15 hours to complete the reaction. All solvents were removed by rotary evaporation, and the product was dried in a vacuum oven at 60° C. for 24 hours to obtain 22.7000 g of a white powdery solid product with a yield of 98.1000%.

[0043] (2) Preparation of terminal alkenyl double splint cage silsesquioxane (3,13-divinyl octaphenyl double splint cage silsesquioxane)

[0044]Add 22.4800g of tetrasilanol sodium salt, 200.0000mL of dry tetrahydrofuran and 5.8300mL of triethylamine into a 500mL one-necked flask, and place it in a low-temperature bath to maintain it at -10°C. 6. 7700g of vinylmethyldichlorosilane was added to the reaction flask at one ti...

Embodiment 2

[0053] (1) Preparation of tetrasilanol sodium salt

[0054] In a 500mL single-necked flask equipped with a magnet, add 31.7000g of phenyltrimethoxysilane, 160.0000mL of isopropanol, 3.3300g of deionized water and 4.2800g of sodium hydroxide in sequence, react at 85°C for 4 hours, cool Stirring was continued at room temperature for 15 hours to complete the reaction. All solvents were removed by rotary evaporation, and the product was dried in a vacuum oven at 60° C. for 24 hours to obtain 22.7000 g of a white powdery solid product with a yield of 98.1000%.

[0055] (2) Preparation of terminal alkenyl double splint cage silsesquioxane (3,13-divinyl octaphenyl double splint cage silsesquioxane)

[0056] Add 22.4800g of tetrasilanol sodium salt, 200.0000mL of dry tetrahydrofuran and 5.8300mL of triethylamine into a 500mL one-necked flask, and place it in a low-temperature bath to maintain it at -10°C. 6. 7700g of vinylmethyldichlorosilane was added to the reaction flask at one t...

Embodiment 3

[0062] (1) Preparation of tetrasilanol sodium salt

[0063] In a 500mL single-necked flask equipped with a magnet, add 31.7000g of phenyltrimethoxysilane, 160.0000mL of isopropanol, 3.3300g of deionized water and 4.2800g of sodium hydroxide in sequence, react at 85°C for 4 hours, cool Stirring was continued at room temperature for 15 hours to complete the reaction. All solvents were removed by rotary evaporation, and the product was dried in a vacuum oven at 60° C. for 24 hours to obtain 22.7000 g of a white powdery solid product with a yield of 98.1000%.

[0064] (2) Preparation of terminal alkenyl double splint cage silsesquioxane (3,13-divinyl octaphenyl double splint cage silsesquioxane)

[0065] Add 22.4800g of tetrasilanol sodium salt, 200.0000mL of dry tetrahydrofuran and 5.8300mL of triethylamine into a 500mL one-necked flask, and place it in a low-temperature bath to maintain it at -10°C. 6. 7700g of vinylmethyldichlorosilane was added to the reaction flask at one t...

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Abstract

The invention relates to a synthesis method of diaminophenyl double splint cage-type silsesquioxane. The method uses silane and sodium hydroxide as raw materials to react tetrasilanol sodium salt, and then through tetrasilanol sodium salt and terminal olefin The terminal alkenyl double splint cage silsesquioxane is reacted with the base chlorosilane, and then the terminal alkenyl double splint cage silsesquioxane and the brominated arylamine compound are coupled under the action of a catalyst and a ligand. Linked reaction, promptly make described diaminophenyl double splint cage type silsesquioxane. Compared with the prior art, the present invention has simple synthesis steps, mild conditions, good controllability, short period and high yield, and the prepared diaminophenyl double-splint cage silsesquioxane can be used for thermosetting resin or thermoplastic Modification of resin has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and relates to a synthesis method of silsesquioxane, in particular to a synthesis method of diaminophenyl double splint cage type silsesquioxane. Background technique [0002] In the field of silsesquioxane research, cyclic oligomeric silsesquioxanes are a class of oligomeric silsesquioxanes (MOSS) with a three-dimensional ring structure, and their inorganic properties are similar to those of polyhedral oligomeric silsesquioxanes. (POSS) is similar and has a silsesquioxane skeleton. Compared with the synthesis of POSS, the synthesis of MOSS has the characteristics of simple method, short cycle time and high yield, and requires less dryness of solvent and environment. [0003] Amine compounds are an important class of organic intermediates with a wide range of uses. Silsesquioxane has good thermal stability, mechanical properties, flame retardant properties, dielectric propert...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21C08G73/10C08G69/42C08G59/14
Inventor 郑思珣刘宁
Owner SHANGHAI JIAOTONG UNIV
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