Bridged polysilsesquioxane, monomer thereof and preparation method for two

A technology of polysilsesquioxane and silane monomers is applied in the field of bridged polysilsesquioxane and its monomers and their preparation. High yield, simple synthesis method, mild process effect

Active Publication Date: 2010-06-23
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Method 1 needs to use Grignard reagent, organolithium or metal hydride to treat trialkoxysilane, which makes the synthesis process complicated and the reaction conditions are harsh; method 2 usually uses noble metal catalysts, such as chloroplatinic acid, Karsted catalyst, etc. to catalyze Addition reactions of Si-H groups of trichlorosilane or trialkoxysilane on the carbon-carbon double bond

Method used

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  • Bridged polysilsesquioxane, monomer thereof and preparation method for two
  • Bridged polysilsesquioxane, monomer thereof and preparation method for two
  • Bridged polysilsesquioxane, monomer thereof and preparation method for two

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Under nitrogen protection, 45ml of 3-(2,3-epoxypropoxy)propyltrimethoxysilane was added to a three-necked flask equipped with a condenser, a thermometer and a dropping funnel, and then 18ml of 3-aminopropyl Trimethoxysilane, heated to 70°C, reacted for 48 hours to obtain a light yellow bridging monomer.

[0030] There are 9 trialkoxy groups in the bridging monomer obtained, take 5ml of the bridging monomer and dissolve it in 10ml of tetrahydrofuran, add 1ml of formic acid aqueous solution with a mass percentage concentration of 88%, and leave it open at 50°C for 24 hours. A bridged polysilsesquioxane is obtained.

[0031] The infrared and nuclear magnetic resonance spectra of the compound are as follows figure 1 with figure 2 shown. It can be seen from the figure that the structure of the compound is correct.

Embodiment 2

[0033] Under nitrogen protection, 23ml of 3-(2,3-epoxypropoxy)propyltrimethoxysilane was added to a three-necked flask equipped with a condenser, a thermometer and a dropping funnel, and then 12ml of 3-aminopropyl Triethoxysilane, heated up to 70°C, reacted for 48 hours to obtain a light yellow bridging monomer.

[0034] There are 9 trialkoxyl groups in the bridging monomer obtained. Dissolve 5ml of the bridging monomer in 10ml of methanol, add 1ml of formic acid aqueous solution with a mass percentage concentration of 88%, and leave it open at 50°C for 24 hours. A bridged polysilsesquioxane is obtained.

Embodiment 3

[0036] Under nitrogen protection, 43ml of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane was added to a three-necked flask equipped with a condenser, a thermometer and a dropping funnel, and then 16ml of 3- Aminopropylmethyldimethoxysilane, heated to 70°C, reacted for 48 hours to obtain a light yellow bridging monomer.

[0037] There are 6 trialkoxyl groups in the bridging monomer obtained. Dissolve 5ml of the bridging monomer in 10ml of tetrahydrofuran, add 1ml of formic acid aqueous solution with a concentration of 88% by mass, and leave it open at 50°C for 36 hours. A bridged polysilsesquioxane is obtained.

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Abstract

The invention discloses a bridged polysilsesquioxane, a monomer thereof and a preparation method for the two. The structural general formula of the monomer is as shown in Formula I, wherein in the structural general formula of the Formula I, R is a structure of Formula II or Formula III, and R1, R2 and R3 are selected from the following groups of methoxyl, ethoxy, methyl and phenyl; R' is C1-C10 aliphatic hydrocarbon, C4-C12 alicyclic hydrocarbon or C4-C12 aromatic hydrocarbon; and n is an integral number ranging from 0 to 10. The preparation method comprises the following step: in the inert atmosphere, making the silane monomer containing an epoxy group shown in the structural general formula of Formula IV react with the silane monomer containing amino shown in the structural general formula of Formula V or diamine shown in the structural general formula of Formula VI. The preparation method has the advantages of easy procuration of raw materials, simple synthetic method and moderate process and can prepare the bridged monomer with 6-12 alkoxy groups, the number of the alkoxy groups can be controlled by the selection of initial raw materials, and high product yield can be realized. H2N-R'-NH2 (Formula VI).

Description

technical field [0001] The invention relates to the field of bridged polysilsesquioxane, in particular to a bridged polysilsesquioxane, its monomers and their preparation method. Background technique [0002] Bridged polysilsesquioxane is an organic-inorganic hybrid material prepared by a sol-gel process from a monomer composed of variable organic bridging groups and two or more trialkoxysilane groups. Such an arrangement offers special opportunities to combine several important properties from the organic and inorganic fields and to create entirely new compounds with unique properties. The molecular diversity, coupled with mild sol-gel conditions and processability to make sheets, films, fibers, etc., make this class of chemically and thermally stable materials a key class in advanced materials science and technology Material. [0003] The diversity and many unique properties of this class of materials originate from the bridging organic groups covalently bonded to the tr...

Claims

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Application Information

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IPC IPC(8): C07F7/18C08G77/14
Inventor 戴珍张小莉徐坚
Owner INST OF CHEM CHINESE ACAD OF SCI
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