Functionalized double tower-type polyhedron oligomeric silsesquioxane and preparation method thereof

A polysilsesquioxane, polyhedron technology, applied in the direction of silicon organic compounds, can solve the problems of low yield and the like, and achieve the effects of high yield, short reaction time and good flame retardant performance

Active Publication Date: 2015-12-30
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Therefore, it is particularly important to carry out functional research on it. The research on DDSQ-containing functionalization mainly includes double-epoxy functionalization (LeiWang, Chongyin Zhang and Sixun Zheng. 2011),叠氮官能化(KunWei,LeiWang,SixunZheng.Organic–InorganicCopolymerswithDouble-DeckerSilsesquioxaneintheMainChainsbyPolymerizationviaClickCh

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  • Functionalized double tower-type polyhedron oligomeric silsesquioxane and preparation method thereof
  • Functionalized double tower-type polyhedron oligomeric silsesquioxane and preparation method thereof
  • Functionalized double tower-type polyhedron oligomeric silsesquioxane and preparation method thereof

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Example Embodiment

[0046] According to another aspect of the present invention, there is provided a method for preparing a bifunctional double-tower polyhedral oligomeric silsesquioxane, which includes the following 4 steps:

[0047] Step 1. Dissolve the double-tower polyhedral oligomeric silsesquioxane containing divinyl groups and the compound containing sulfhydryl groups in an organic solvent, and then add a thermal initiator and stir uniformly.

[0048] In the above preparation method, the divinyl double-tower polyhedral oligomeric silsesquioxane is represented by the following formula II:

[0049]

[0050] Wherein, R can each independently be hydrogen, alkyl, aryl, alicyclic or other organic groups (such as alkylsilyl, nitrile, etc.).

[0051] In a preferred embodiment, R may each independently be hydrogen, isobutyl, cyclohexyl, cyclopentyl or phenyl.

[0052] Furthermore, R is a phenyl group, that is, the double-tower polyhedral oligomeric silsesquioxane containing divinyl groups is more preferably ...

Example Embodiment

[0091] Example 1

[0092] 1) Dissolve 5.8mmol of divinyl double-tower polyhedral oligomeric silsesquioxane and 0.5ml of 2-mercaptoacetic acid, the amount of which is 7.2mmol of 2-mercaptoacetic acid, in 20ml of tetrahydrofuran, then add 0.05 g Thermal initiator AIBN, stir evenly;

[0093] 2) Place the reaction system in a constant temperature oil bath at 80°C and reflux for 5 hours for thermal initiation reaction;

[0094] 3) After the reaction, the reaction solution was added dropwise to 200ml of water for precipitation, and the resulting precipitate was vacuum dried at 40°C to obtain a double-tower polyhedral oligomeric silsesquioxane (diethylcarboxyl DDSQ) with diethyl carboxyl group. The rate is 90%.

[0095] Infrared (IR) and nuclear magnetic tests were carried out on the double-tower polyhedral oligomeric silsesquioxane (double carboxyl DDSQ) obtained above. 1 H-NMR) to characterize the product structure.

[0096] The IR spectrum of the obtained product diethyl carboxyl DDSQ is ...

Example Embodiment

[0097] Example 2

[0098] 1) Dissolve 5.8mmol of divinyl DDSQ and 0.5ml of 2-mercaptoacetic acid, the amount of which is 7.2mmol of 2-mercaptoacetic acid, in 20ml of tetrahydrofuran, then add 0.05g of benzoin methyl ether (DMPA) and stir Evenly

[0099] 2) The photo-initiated reaction is carried out under a 365nm ultraviolet lamp, and the entire reaction system is stirred at room temperature for 12 hours;

[0100] 3) After the reaction, the reaction solution was washed 3 times with 20ml of distilled water, the dichloromethane layer was taken, dried with anhydrous magnesium sulfate overnight, then filtered, and the solvent was removed to obtain the double-tower polyhedral oligomeric silsesquisite of diethyl carboxyl group Oxyane (diethyl carboxyl DDSQ), the yield is 90%.

[0101] The double-tower polyhedral oligomeric silsesquioxane of double ethyl carboxyl (DDSQ) obtained above was subjected to infrared (IR) and nuclear magnetic testing ( 1 H-NMR) to characterize the product structur...

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Abstract

The invention discloses functionalized double tower-type polyhedron oligomeric silsesquioxane. The functionalized double tower-type polyhedron oligomeric silsesquioxane can be widely used in special structure double tower-type polyhedron polysilsesquioxane preparation, polymer modification and polymer synthesis, and can be used in biomedical and photoelectric functional materials. The oligomeric silsesquioxane is obtained by a mercapto-olefin addition reaction of divinyl-containing double tower-type polyhedron oligomeric silsesquioxane, mercapto-terminated carboxylic acid, alcohol and amine. The preparation method has the advantages of control and operation easiness, short reaction time, high yield and purification easiness.

Description

technical field [0001] The invention belongs to the field of organic / inorganic hybrid materials, in particular to functionalized double-tower polyhedral oligomeric silsesquioxane and a preparation method thereof. Background technique [0002] Polyhedral oligomeric silsesquioxane (POSS) has the chemical formula [RSiO 1.5 ] n The general term for substances, where n can be 6, 8, 10, 12, etc. Common silsesquioxane structures include amorphous, ladder, cage and semi-cage. Among them, double-tower polyhedral oligomeric silsesquioxane (DDSQ) is a POSS with a special structure, containing 10 silicon atoms, and has excellent performance itself. [0003] As an organic / inorganic hybrid nanomaterial, double-tower polyhedral oligomeric silsesquioxane has many excellent properties. It not only has the advantages of low density, good solubility, and good thermal stability of organic materials, but also has flexible functions. It also has the traditional characteristics of high strengt...

Claims

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Application Information

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IPC IPC(8): C07F7/21C08K5/549
Inventor 徐日炜李滔代培谷晓昱余鼎声吴一弦
Owner BEIJING UNIV OF CHEM TECH
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