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Metallic tin-containing double-decker polyhedral oligomeric silsesquioxane, and preparation method and application thereof

A polysilsesquioxane and polyhedral technology, which is applied in the field of double-tower-type polyhedral oligomeric silsesquioxane, can solve the problems of little and little research on polyhedral oligomeric silsesquioxane.

Active Publication Date: 2018-05-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Due to the unique structure and properties of DDSQ, the research on this kind of special inorganic / organic hybrid materials is becoming more and more extensive, such as designing its structure or studying the properties of its mixture with polymer materials. However, for metal-based There are few researches on the polyhedral oligomeric silsesquioxanes, and most of the existing researches revolve around its use as a curing catalyst. There is little research on oxane

Method used

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  • Metallic tin-containing double-decker polyhedral oligomeric silsesquioxane, and preparation method and application thereof
  • Metallic tin-containing double-decker polyhedral oligomeric silsesquioxane, and preparation method and application thereof
  • Metallic tin-containing double-decker polyhedral oligomeric silsesquioxane, and preparation method and application thereof

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Embodiment approach

[0030] According to a preferred embodiment of the present invention, the alkyl group is selected from C 1 ~C 16 of alkyl.

[0031] In a further preferred embodiment, the alkyl group is selected from C 1 ~C 8 of alkyl.

[0032] In a further preferred embodiment, the alkyl group is selected from methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl, cyclopropyl, cyclobutanyl, One or more of cyclopentyl and cyclohexyl, such as methyl and cyclohexyl.

[0033] According to a preferred embodiment of the present invention, the alkyl-substituted phenyl group is selected from p-tolyl, o-tolyl or m-tolyl.

[0034] According to a preferred embodiment of the present invention, in formula (I), R is selected from phenyl, and its structural formula is shown in formula (II):

[0035]

[0036] In a further preferred embodiment, in formula (II), R' is selected from phenyl or methyl.

[0037] Another aspect of the present invention provides a method for preparing the metal-...

Embodiment 1

[0099] Add 2mmol double-tower type octaphenyltetrasilanol silsesquioxane and 4mmol dimethyl tin dichloride in the reaction flask, then continuously pump the vacuum three times to the reaction flask, so that the whole reaction system is under an argon atmosphere, Then inject 40mL toluene and stir;

[0100] Inject 9mmol triethylamine into the reaction flask, and stir the reaction at 50°C for 6h;

[0101] Finish the reaction, filter the system with suction, then recrystallize in absolute ethanol, and carry out vacuum drying at 30°C to obtain the double-tower polyhedral oligomeric silsesquioxane containing metal tin, with a yield of 90%.

[0102] (1) Carry out infrared test to product, obtain its infrared spectrogram such as figure 1 shown, among them, in figure 1 Among them, DDOH stands for double-towered octaphenyltetrasilanol silsesquioxane (raw material), and DDOSn-Me stands for double-towered polyhedral oligomeric silsesquioxane containing methyl tin (product).

[0103] e...

Embodiment 2

[0113] Add 2mmol of double-tower octaphenyltetrasilanol silsesquioxane and 4.4mmol of diethyltin dichloride to the reaction flask, and then continuously pump the vacuum three times to the reaction flask, so that the entire reaction system is under an argon atmosphere , then inject 50mL of toluene and stir;

[0114] Inject 10mmol of tetramethylethylenediamine into the reaction flask, and stir the reaction at 30°C for 6h;

[0115] Finish the reaction, filter the system with suction, then recrystallize in absolute ethanol, and carry out vacuum drying at 30°C to obtain the double-tower polyhedral oligomeric silsesquioxane containing metal tin, with a yield of 80.43%.

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Abstract

The invention discloses a metallic tin-containing double-decker polyhedral oligomeric silsesquioxane, and a preparation method and an application thereof. The metallic tin-containing double-decker polyhedral oligomeric silsesquioxane contains bimetallic tin, and has a structural formula represented by formula (I). The preparation method is carried out in a protective atmosphere, and comprises thefollowing steps: hydroxyl group-containing double-decker polyhedral oligomeric silsesquioxane and a metallic tin organic compound are dispersed in a solvent, then an additive is added, a reaction is performed, and post-treatment is finally performed to obtain the metallic tin-containing double-decker polyhedral oligomeric silsesquioxane. The metallic tin-containing double-decker polyhedral oligomeric silsesquioxane can be used as a catalyst for coordination ring-opening polymerization, and is especially used as a catalyst for the polymerization of polylactic acid. The metallic tin-containing double-decker polyhedral oligomeric silsesquioxane can obtain a narrow molecular weight distribution polymer when used as a coordination ring-opening polymerization catalyst, and they can be stored fora long time without affecting the catalytic performance.

Description

technical field [0001] The invention relates to the field of polyhedral oligomeric silsesquioxanes, in particular to the field of double-towered oligomeric silsesquioxanes, in particular to a double-towered polyhedral oligomeric silsesquioxane containing metal tin and its preparation and application. Background technique [0002] As an organic / inorganic hybrid nanomaterial, Double-decker Silsesquioxane (DDSQ) has many excellent properties: its polyhedral skeleton makes it low density and good air permeability; The traditional characteristics of high strength and high temperature resistance of inorganic materials and the quantum size effect and small size effect of nanomaterials; it also has the advantages of low density, good solubility, and good thermal stability of organic materials, as well as the designability of organic groups at the end, etc. . [0003] Due to the unique structure and properties of DDSQ, the research on this kind of special inorganic / organic hybrid m...

Claims

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Application Information

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IPC IPC(8): C08G77/398C08G63/08C08G63/85
CPCC08G63/08C08G63/823C08G63/85C08G77/398
Inventor 徐日炜张月明文勇刘蕊余鼎声
Owner BEIJING UNIV OF CHEM TECH
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