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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
  • Application Information

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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-DeckerSilsesquioxaneintheMainChainsbyPolymerizationviaClickChemistry.Journalofpolymerscience,PartA:Polymerchemistry,2013,51,4221),双羟基官能化(KunWei,LeiWangandSixunZheng.Organic–inorganicpolyurethaneswith3,13-dihydroxypro- pyloctaphenyldouble-deckersilsesquioxanechainextender.Polym.Chem., 2013,4,1491), and the above-mentioned method is mainly obtained through multi-step functionalization conversion, and the yield is low

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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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preparation example Construction

[0046] According to another aspect of the present invention, a kind of preparation method of bifunctional polyhedron polyhedral oligosilsesquioxane is provided, and this method comprises following 4 steps:

[0047] Step 1. Dissolving the double-tower polyhedral oligomeric silsesquioxane containing divinyl groups and the compound containing terminal mercapto groups in an organic solvent, then adding a thermal initiator and stirring evenly.

[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 bi-towered polyhedral oligomeric silsesquioxane containing a divinyl gro...

Embodiment 1

[0092] 1) Dissolve 5.8mmol of divinyl double-tower polyhedral oligomeric silsesquioxane and 0.5ml of 2-mercaptoacetic acid in 20ml of tetrahydrofuran, and 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 to reflux for 5 hours to carry out 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 diethylcarboxylated double-tower polyhedral oligomeric silsesquioxane (diethylcarboxy DDSQ), producing The rate is 90%.

[0095] Carry out infrared (IR), NMR test ( 1 H-NMR) to characterize the product structure.

[0096] The IR spectrogram of gained product diethyl carboxyl DDSQ sees figure 1 ,That 1 H-NMR spectrum see figure 2 . figure 1 1709cm in -1 The C=O stretching vibration peak of the carboxyl group appears, figure 2 6.0ppm of -CH=CH 2...

Embodiment 2

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

[0099] 2) The photoinitiated reaction was carried out under a 365nm ultraviolet lamp, and the entire reaction system was stirred at a constant speed at room temperature for 12 hours;

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

[0101] Carry out infrared (IR), NMR test ( 1 H-NMR) to characterize the product structure.

[0102] The IR spectrogram of gained product diethyl carboxyl DDSQ sees figure 1 ,That 1 H-NMR...

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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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