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Preparation method of aromatic ring-containing bridged silsesquioxane monomer

A technology of silsesquioxane and semisiloxane, which is applied in the field of preparation of aromatic ring bridged silsesquioxane monomers, and can solve problems such as difficult separation, difficult synthesis of precursors, and difficult availability of raw materials

Inactive Publication Date: 2013-12-18
HEFEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that the process is simple, but the reaction conditions are harsh, and the reaction system is required to be anhydrous and oxygen-free, and tetraalkoxysilane is used, which makes it difficult to achieve monosubstitution of alkoxy groups, and the product is often a mixture of monosubstitution and double substitution, which is not easy separate
② It is realized by the affinity substitution reaction between a trialkoxychlorosilane with an electrophilic group and an aromatic hydrocarbon with a double nucleophilic end group. This method seems simple and the yield is high, but the raw materials are not easy to obtain. Synthesis of precursors is difficult

Method used

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  • Preparation method of aromatic ring-containing bridged silsesquioxane monomer
  • Preparation method of aromatic ring-containing bridged silsesquioxane monomer
  • Preparation method of aromatic ring-containing bridged silsesquioxane monomer

Examples

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Embodiment 1

[0027] Embodiment 1: Preparation of 1,4-bis(trimethoxysilylethyl)benzene

[0028] In this embodiment, 1,4-bis(trimethoxysilylethyl)benzene was prepared according to the following steps:

[0029] a. Add 15 mg of catalyst Pt (dcp) to the three-necked flask, vacuumize for 15 minutes using the double-pipe system, and fill with nitrogen for 3 minutes. Repeat this three times so that there is no nitrogen atmosphere in the three-necked flask; use a syringe to draw 28 mL of sodium dewatered in advance1,4 - Divinylbenzene and 150 mL of tetrahydrofuran were injected into a sealed three-necked flask.

[0030] b. Add 150 mL of tetrahydrofuran into the three-necked flask that completed step a, and then add 60 mL of trimethoxysilane dropwise while stirring to obtain mixed liquid A.

[0031] c. The mixed liquid A obtained in step b was refluxed for 6 hours under the condition of stirring and heating in an oil bath at 70° C., stopped heating after the reaction was completed, and cooled to ro...

Embodiment 2

[0034] Embodiment 2: Preparation of 1,4-bis(triethoxysilylethyl)benzene

[0035] In this embodiment, 1,4-bis(triethoxysilylethyl)benzene is prepared according to the following steps:

[0036] a. Add 20 mg of catalyst Pt (dcp) to the three-necked flask, vacuumize for 15 minutes using the double-pipe system, and fill with nitrogen for 3 minutes. Repeat this three times, so that there is no nitrogen atmosphere in the three-necked flask; draw 28 mL of pre-dehydrated sodium with a syringe1,4 - Divinylbenzene, injected into a sealed three-necked flask.

[0037] b. Add 300 mL of tetrahydrofuran into the three-necked flask that completed step a, and then add 110 mL of triethoxysilane dropwise while stirring to obtain mixed liquid A.

[0038] c. The mixed liquid A obtained in step b was refluxed for 6 hours under the condition of magnetic stirring and heating in an oil bath at 70° C., stopped heating after the reaction was completed, and cooled to room temperature to obtain mixed liqu...

Embodiment 3

[0041] Example 3: Preparation of 4,4'-bis(trimethoxysilylethyl)biphenyl

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Abstract

The invention discloses a preparation method of an aromatic ring-containing bridged silsesquioxane monomer. The preparation method is characterized in that divinyl aromatic hydrocarbon and trialkoxyl silane are used as raw materials, tetrahydrofuran or diozane is used as a solvent, dicyclopentadiene platinum is used as a catalyst, and C=C double bonds of the divinyl aromatic hydrocarbon and Si-H bond of the trialkoxyl silane are subjected to hydrosilylation to synthesize the aromatic ring-containing bridged silsesquioxane monomer under the water-free and oxygen-free condition. The method has the advantages of simple process flow, high reaction specificity, no byproducts and high product yield.

Description

technical field [0001] The invention relates to a preparation method of a bridged silsesquioxane monomer containing an aromatic ring, and belongs to the technical field of bridged silsesquioxanes. Background technique [0002] In the silsesquioxane family, there is a class with Y 3 Si-X-Si-Y 3 Structured organic-inorganic hybrid molecules, called bridged silsesquioxanes, where Y is a reactive substituent, such as methoxy, ethoxy, etc., and X can be a chemically stable substituent, such as An alkyl group, an aryl group or a combination of the two can also be a reactive group, such as an amino group, an ester group, a carboxyl group, a hydroxyl group, and the like. The bridged polysilsesquioxane monomer is hydrolyzed and polycondensed to obtain bridged polysilsesquioxane, which is a kind of inorganic-organic hybrid material with excellent comprehensive performance. It not only has the advantages of both inorganic and organic substances, but also Due to the wide adjustabilit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 杨本宏王庆杨宪
Owner HEFEI UNIV
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