Dyhydroxyl cage-type silsesquioxane monomer and preparation method thereof

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...

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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

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