Dyhydroxyl cage-type silsesquioxane monomer and preparation method thereof

A technology of silsesquioxane and polysilsesquioxane, applied in the direction of silicon organic compounds, etc., can solve the problems of complex process, gap between mechanical properties and thermal properties, complicated operation, etc., and achieve the effect of simple process

Inactive Publication Date: 2013-07-17
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the gap between semi-closed cage silsesquioxane in mechanical properties and thermal properties compared with fully closed cage silsesquioxane, the improvement of thermal properties of the synthesized composite material is limited, and this method needs to make the cage The reason for structural cracking makes the process complex, the operation is cumbersome, and the processed products are easy to pollute the environment
[0006] American International Polymer (Polymer International, 2005, 54 (1): 47-53) reported the formation of semi-closed heptacyclopentyl cage silsesquioxane and polyethylene terephthalate containing three epoxy groups. The hybrid material, through melt in situ polymerization, the epoxy group of the cage silsesquioxane reacts with the terminal hydroxyl group of polyethylene terephthalate to introduce the cage silsesquioxane into the polymer main body chain and make the polymer form a network structure, but the mechanical and thermal properties of the semi-closed cage silsesquioxane are different from those of the fully closed cage silsesquioxane, which limits the cage silsesquioxane / The embodiment of the excellent performance of the polymer hybrid material, and this method is complex in process and low in safety due to the formation of hybrid material between cage silsesquioxane and polyethylene terephthalate

Method used

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  • Dyhydroxyl cage-type silsesquioxane monomer and preparation method thereof
  • Dyhydroxyl cage-type silsesquioxane monomer and preparation method thereof
  • Dyhydroxyl cage-type silsesquioxane monomer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Add DDSQ (5.0g, 0.004mol) and eugenol (1.31g, 0.008mol) into a nitrogen-protected container, add toluene (20mL) as a solvent in the system, raise the temperature to 65°C, and dropwise add Pt with a mass fraction of 0.3 0.2ml of Castel’s Reagent, react at 65°C for 6 hours, then cool down to room temperature, add the reaction mixture to a vacuum distillation device, and distill under reduced pressure at 80°C to remove unreacted eugenol and solvent toluene, then drop to After reaching room temperature, 3.1 g of light yellow solid 2Si-OH was obtained with a yield of 48.2%.

[0017] Use NicoletImpact410 Fourier transform infrared spectrometer to measure the infrared spectrum of 2Si-OH and eugenol, the scanning range is 4000~400cm -1 , resolution 4cm -1 , KBr tablet, see the results figure 1 . Depend on figure 1 It can be seen that the 1639cm in eugenol -1 The C=C bond absorption peak and the 2161cm in DDSQ -1 The Si-H bond absorption peak has disappeared in 2Si-OH, and...

Embodiment 2

[0021] Add DDSQ (5.0g, 0.004mol) and eugenol (1.48g, 0.009mol) into a nitrogen-protected container, add toluene (20mL) as a solvent in the system, raise the temperature to 65°C, and dropwise add Pt with a mass fraction of 0.3 0.2ml of Castel’s reagent, react at constant temperature for 12h and then cool down to room temperature, add the reaction mixture into a vacuum distillation device, and distill under reduced pressure at 90°C to remove unreacted eugenol and solvent toluene, and obtain 3.3g Pale yellow solid 2Si-OH, yield 51.3%.

Embodiment 3

[0023] Add DDSQ (5.0g, 0.004mol) and eugenol (1.64g, 0.01mol) into a nitrogen-protected container, add toluene (20mL) as a solvent in the system, raise the temperature to 70°C, and dropwise add Pt with a mass fraction of 0.3 0.2ml of Castel’s Reagent, react at constant temperature for 12h and cool down to room temperature, add the reaction mixture into a vacuum distillation device, and distill under reduced pressure at 90°C to remove unreacted eugenol and solvent toluene, and obtain 3.4g Pale yellow solid 2Si-OH, yield 53.1%.

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Abstract

The invention discloses a dyhydroxyl cage-type silsesquioxane monomer and a preparation method thereof and belongs to the technical field of preparation of silsesquioxane. The preparation method of the dyhydroxyl cage-type silsesquioxane monomer comprises the following steps of: adding dyhydroxyl cage-type silsesquioxane monomer and eugenol monomer in a nitrogen-gas protected container, wherein the feeding molar ratio of the two monomers is 1:(2-16); adding toluene as a solvent, dropwise adding Pt with mass percentage of 0.3% and Custer reagent which is 0.1% (volume percentage) of solvent as a catalyst; heating up to 65-110 DEG C for reacting for 6-36 hours at a constant temperature; cooling the reaction system to the room temperature and distilling the reaction mixed liquor at 80-110 DEG C under reduced pressure to remove un-reacted eugenol; and cooling the room temperature to obtain light yellow solid, namely the dyhydroxyl cage-type silsesquioxane monomer. By overcoming the defects that the prior art is complex in operations and low in safe, the preparation method is simple in process and pollution-free to the environment. Besides, the preparation method has an important meaning in synthesizing dyhydroxyl POSS (Polyhedral Oligomeric Silsesquioxane); and the POSS can be directly introduced to a linear chain of the polymer.

Description

technical field [0001] The invention belongs to the technical field of preparation of silsesquioxane, and in particular relates to a silsesquioxane monomer with a dihydroxyl cage structure and a preparation method thereof. Background technique [0002] Polyhedral oligomeric silsesquioxane (POSS) is a kind of cage molecule with a nanometer size (0.5-3nm) and a clear structure. It has an inorganic silicon-oxygen core surrounded by 8 organic groups. The molecular formula can be Expressed as (RSiO1.5)8. Because POSS can effectively combine organic and inorganic components through chemical bonds at the molecular level to form a molecular hybrid composite material, it often endows the material with excellent properties, such as high thermal stability, good dissolution Sex and film-forming properties, as well as novel functionality, etc. [0003] Most of the current research focuses on POSS with octafunctional and monofunctional groups, which are mainly used for hyperbranching or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 牟建新张卫海许玖多王岩姜振华
Owner JILIN UNIV
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