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Liquid cage-shaped silsesquioxane and preparation method thereof

A silsesquioxane and cage technology, applied in the field of liquid cage silsesquioxane and its preparation, can solve the loss performance, poor thermal and mechanical properties of epoxy resin, poor compatibility and dispersibility, etc. problems, to achieve the effect of improving compatibility and dispersion, improving thermal and mechanical properties

Inactive Publication Date: 2017-08-11
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, the problems in the prior art are: the prior art usually loses other properties while improving a certain performance, and the products prepared by the prior art have poor compatibility and dispersibility with epoxy resins, and the environmental Oxygen resin has poor thermal and mechanical properties

Method used

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  • Liquid cage-shaped silsesquioxane and preparation method thereof
  • Liquid cage-shaped silsesquioxane and preparation method thereof
  • Liquid cage-shaped silsesquioxane and preparation method thereof

Examples

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preparation example Construction

[0025] like figure 1 As shown, the preparation method of liquid cage silsesquioxane provided by the embodiments of the present invention specifically includes:

[0026] S101: Add deionized water, tetrabutylammonium hydroxide, and isopropanol into a round-bottomed flask, stir and heat up to 30°C, slowly add aminoethylaminopropyltrimethoxysilane dropwise, stir for 5 hours, then heat up to 78°C, Reaction 19h. The white powder was obtained by filtration, and dried in vacuum for 24 hours to obtain solid aminoethylaminopropyl cage silsesquioxane.

[0027] S102: Add epichlorohydrin and diethylamine to the flask, slowly add deionized water dropwise, react at 29°C for 6h, then cool down to 22°C, dissolve sodium hydroxide in water to make a solution and add it to the reaction flask, Stirring was continued for another 40 min. Separate the organic phase with a separatory funnel, wash with water, extract and dry to obtain N,N-diethylamino-1,2-propylene oxide.

[0028] S103: Take N,N-di...

Embodiment 1

[0034] (1) Add 10g of deionized water, 0.21g of tetrabutylammonium hydroxide, and 31g of isopropanol into a 500ml round bottom flask, stir and heat up to 30°C, slowly add 40.25g of aminoethylaminopropyltrimethoxysilane dropwise, After stirring for 5 hours, the temperature was raised to 78°C, and the reaction was carried out for 19 hours. The white powder was obtained by filtration, and dried in vacuum for 24 hours to obtain solid aminoethylaminopropyl cage silsesquioxane.

[0035] (2) Add 18.5g epichlorohydrin and 14.4 diethylamine into a 250ml round bottom flask, slowly add 6g deionized water dropwise, react at 29°C for 6h, then cool down to 22°C, dissolve 8g sodium hydroxide in 15.2 mL of water was made into a solution and added to the reaction flask, and the stirring was continued for 40 minutes. Separate the organic phase with a separatory funnel, wash with water, extract and dry to obtain N,N-diethylamino-1,2-propylene oxide.

[0036] (3) Take 2.54g of N,N-diethylamino-...

Embodiment 2

[0039] (1) Add 10g of deionized water, 0.21g of tetrabutylammonium hydroxide, and 31g of isopropanol into a 500ml round bottom flask, stir and heat up to 30°C, slowly add 40.25g of aminoethylaminopropyltrimethoxysilane dropwise, After stirring for 5 hours, the temperature was raised to 78°C, and the reaction was carried out for 19 hours. The white powder was obtained by filtration, and dried in vacuum for 24 hours to obtain solid aminoethylaminopropyl cage silsesquioxane.

[0040] (2) Add 18.5g epichlorohydrin and 14.4 diethylamine into a 250ml round bottom flask, slowly add 6g deionized water dropwise, react at 29°C for 6h, then cool down to 22°C, dissolve 8g sodium hydroxide in 15.2 mL of water was made into a solution and added to the reaction flask, and the stirring was continued for 40 minutes. Separate the organic phase with a separatory funnel, wash with water, extract and dry to obtain N,N-diethylamino-1,2-propylene oxide.

[0041] (3) Take 2.54g of N,N-diethylamino-...

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Abstract

The invention belongs to the field of preparation of fine chemical engineering, and discloses liquid cage-shaped silsesquioxane and a preparation method thereof. The preparation method comprises the following step: taking aminoethyl aminopropyl trimethoxy silane as a raw material; synthesizing the aminoethyl aminopropyl trimethoxy silane into solid aminoethyl aminopropyl cage-shaped silsesquioxane through hydrolytic condensation at first; and then reacting the solid aminoethyl aminopropyl cage-shaped silsesquioxane with micromolecular N,N-lignocaine-1,2-epoxypropane to obtain the liquid cage-shaped silsesquioxane. The aminoethyl aminopropyl cage-shaped silsesquioxane is synthesized by the aminoethyl aminopropyl trimethoxy silane, and the liquid cage-shaped silsesquioxane is prepared on the basis of the aminoethyl aminopropyl cage-shaped silsesquioxane. Compatibility and dispersibility of the prepared liquid cage-shaped silsesquioxane and epoxy resin are greatly improved, a construction process is facilitated, the liquid cage-shaped silsesquioxane is used for modification of cured resin of the epoxy resin, and the thermal performance and the mechanical performance of the epoxy resin are improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemical preparation, and in particular relates to a liquid cage-type silsesquioxane and a preparation method thereof. Background technique [0002] Cage silsesquioxane (POSS) is a nano-scale inorganic / organic hybrid material composed of Si and O as an internal cage-type inorganic framework and externally connected with organic groups. Due to the structural characteristics of inorganic / organic hybridization and external functional groups, POSS can be used in conjunction with a variety of thermosetting resins to form inorganic / organic hybrid nano-reinforced polymer materials. [0003] High-performance, high-heat-resistant epoxy resin varieties are mainly those multifunctional epoxy resins with heat-resistant skeletons or that can increase cross-linking density. In addition to the influence of the structure of the epoxy resin itself, the influence of the type of curing agent is another important facto...

Claims

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Application Information

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IPC IPC(8): C08G77/388C08G77/26C08L63/00C08L83/08
CPCC08G77/045C08L63/00C08L2201/08C08L83/08
Inventor 王行柱刘敏渊肖启振闫磊
Owner XIANGTAN UNIV
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