Preparation method of polyhedral oligomeric silsesquioxane hybridized whole and product of polyhedral oligomeric silsesquioxane hybridized whole

A polyhedron and multifold technology, applied in the field of hybrid materials, can solve the problems of initiator residue, cumbersome process, time and manpower consumption, etc., and achieve the effects of property expansion, production efficiency improvement and production cost reduction

Pending Publication Date: 2022-05-20
武汉爱邦高能技术有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, there are certain defects in the method of thermal initiation / photoinitiation of free radical polymerization, such as the residue of the initiator, the process is cumbersome, and more time and manpower are needed.

Method used

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  • Preparation method of polyhedral oligomeric silsesquioxane hybridized whole and product of polyhedral oligomeric silsesquioxane hybridized whole
  • Preparation method of polyhedral oligomeric silsesquioxane hybridized whole and product of polyhedral oligomeric silsesquioxane hybridized whole
  • Preparation method of polyhedral oligomeric silsesquioxane hybridized whole and product of polyhedral oligomeric silsesquioxane hybridized whole

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Embodiment 1

[0024] see figure 1 , In this embodiment, a method for preparing a polyhedral oligomeric silsesquioxane hybrid monolith is provided, and the specific steps are as follows:

[0025] Step 1: Prepare Vinyl-POSS monomer; add the mixture of concentrated hydrochloric acid and deionized water to the acetone solution of vinyltrimethoxysilane, stir and reflux at 40°C for 48h, wash the white powder with ethanol, and dichloromethane Vinyl-POSS monomer can be obtained after recrystallization in a mixed solvent of acetone.

[0026] Step 2: Prepare Vinyl-POSS solution, inject Vinyl-POSS monomer and THF solution into a polyethylene bag and seal it after continuously passing inert gas to remove oxygen. The molar concentration of Vinyl-POSS monomer is 0.01-1.0mol L- 1.

[0027] Step 3: Under room temperature, use an electron accelerator beam device to perform radiation polymerization / crosslinking reaction on the sample obtained in step 2 to obtain a colorless transparent solid. The absorbed ...

Embodiment 2

[0031] In this embodiment, a method for preparing a polyhedral oligomeric silsesquioxane hybrid monolith, the specific steps are as follows:

[0032] Step 1: Dissolve 13.3g of vinyltrimethoxysilane, 90mmol, in 135mL of acetone solvent, drop a mixed solution of 22.5mL of concentrated hydrochloric acid and 25.9mL of deionized water into acetone, stir and reflux at 40°C for 48h;

[0033] When a white solid precipitates on the wall of the flask and the reaction solution turns brown, transfer the solid and the solution in the flask to a beaker, filter with suction, wash the precipitate with ethanol and dry it in vacuum at 60°C for 24 hours to obtain a white powder;

[0034] The crude product was finally recrystallized with a 1:3 mixed solvent of dichloromethane and acetone to obtain 2.37 g of white powder, namely Vinyl-POSS monomer, with a yield of 33.3%.

[0035] Step 2: Add a certain quality of Vinyl-POSS monomer and a certain volume of THF into a polyethylene plastic bag, and se...

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Abstract

The invention discloses a preparation method of a polyhedral oligomeric silsesquioxane hybrid whole and a product thereof, and the preparation method comprises the following steps: synthesizing octahedral vinyl oligomeric silsesquioxane by using vinyl trimethoxy silane as a raw material, dissolving the octahedral vinyl oligomeric silsesquioxane in a tetrahydrofuran solution at room temperature, and reacting at room temperature to obtain the polyhedral oligomeric silsesquioxane hybrid whole. The polyhedral oligomeric silsesquioxane hybrid monolithic material containing the vinyl functional group can be prepared through an ionizing radiation technology. The preparation method disclosed by the invention has the advantages of cleanness, energy conservation, capability of initiating polymerization at normal temperature, no need of a catalyst or an initiator and the like, so that the production efficiency can be improved and the production cost can be reduced; the polymer material contains a certain amount of unreacted vinyl, so that the surface modification of the polymer material can be realized through further functionalization, thereby adjusting the properties of the material and expanding the application range of the material.

Description

technical field [0001] The invention relates to the technical field of hybrid materials, in particular to a method for preparing a polyhedral oligomeric silsesquioxane hybrid monolith and a product thereof. Background technique [0002] Reactive polymers are polymer materials with network structure, reactivity and solvent tolerance, which can play an important role in solid-phase synthesis or separation applications. [0003] Polyhedral oligomeric silsesquioxane (POSS), due to its own unique properties, has a good application prospect as a new type of nanoscale filler in the modification of polymer materials. The typical empirical general formula of POSS molecules is (RSiO 1.5 ) n , where R can be a series of organic groups such as alkyl, alkenyl, amino, hydroxyl, etc. While endowing POSS molecules with reactivity and functionality, these organic groups can also increase the interfacial force and compatibility between them and polymers or monomers, thereby further improvi...

Claims

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Application Information

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IPC IPC(8): C08F130/08C08F2/54
CPCC08F130/08C08F2/54
Inventor 赵龙赵文超齐伟
Owner 武汉爱邦高能技术有限公司
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