Heptatridecafluorooctylpropyl polyhedral oligomeric silsesquioxane and functionalized derivates thereof

A technology of heptapolytridecafluorooctylpropyl cage and fluorooctylpropyl cage, which is applied in the field of preparation of T7 configuration tridecafluorooctylpropyl cage silsesquioxane and its functionalized derivatives , can solve the problems of high regularity long-chain functionalized T8 configuration fluorine-containing POSS, etc.

Inactive Publication Date: 2013-07-03
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are still no reports on long-chain functionaliz

Method used

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  • Heptatridecafluorooctylpropyl polyhedral oligomeric silsesquioxane and functionalized derivates thereof
  • Heptatridecafluorooctylpropyl polyhedral oligomeric silsesquioxane and functionalized derivates thereof
  • Heptatridecafluorooctylpropyl polyhedral oligomeric silsesquioxane and functionalized derivates thereof

Examples

Experimental program
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Example Embodiment

[0055] Example 1

[0056] The technical solutions of the present invention will be described in detail below by way of embodiments, but the protection scope of the present invention is not limited to the embodiments.

Example Embodiment

[0057] Example 1 Preparation of seven polytridecafluorooctyl propyl cage silsesquioxane

[0058] Put 52.4g tridecafluorooctylpropyltrimethoxysilane (trade name: Actyflon-G602, molecular formula: CF 3 (CF 2 ) 5 CH 2 CH(CH 3 )CH 2 CH 2 CH 2 Si(OCH 3 ) 3 Add 500 mL of tetrahydrofuran to 0.1 mol, then add 2 g of NaOH and 3 g of deionized water, stir evenly, and heat to 75°C and reflux for 20 hours;

[0059] Rotate the solution to remove the solvent and volatile substances to obtain a large amount of viscous substance, and then wash with methanol (the temperature of methanol is controlled at -10~0℃), spin dry, and dry to obtain heptatrifluorooctyl propyl group Sodium silsesquioxane trisilanol; its molecular formula: (CF 3 (CF 2 ) 5 CH 2 CH(CH 3 )CH 2 CH 2 CH 2 ) 7 Si 7 O 12 Na 3

[0060] Its chemical structural formula is:

[0061]

[0062] R is CH 2 CH 2 CH 2 (CH 3 )CHCH 2 (CF 3 ) 5 CF 3 , Which is a POSS with a missing corner T7 configuration.

[0063] Infrared characterization of the pro...

Example

[0065] Examples 2-6 Preparation of seven polytridecafluorooctyl propyl cage silsesquioxane

[0066] The specific steps are the same as in Example 1. The preparation process parameters, the raw materials used and the specific dosage are Table 1:

[0067] Table 1 Preparation process parameters, raw materials used and specific dosages in Examples 2 to 6

[0068]

[0069] In this step, potassium hydroxide can also be used as the alkali catalyst to replace tetramethylammonium hydroxide, and the alkali-catalyzed incomplete hydrolysis reaction can also be realized.

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Abstract

The invention provides a preparation method for heptatridecafluorooctylpropyl polyhedral oligomeric silsesquioxane and functionalized derivates thereof. The preparation method comprises the steps as follows: adding tridecafluorooctylpropyl trimethoxy silane into an organic solvent, adding de-ionized water and NaOH, heating, stirring, reacting under reflux condition, washing by a washing solvent, and drying to obtain trisilanol sodium salt of heptatridecafluorooctylpropyl polyhedral oligomeric silsesquioxane; and adding trisilanol sodium salt into an organic reagent, dropwise adding hydrochloric acid, triethylamine and a silane coupling agent, stirring a mixture at normal temperature for reaction, removing generated deposit, carrying out rotary evaporation, removing the solvent, obtaining white crystals, dissolving the crystals in methanol, filtering for collecting insoluble parts, and carrying out vacuum drying to obtain a T8-type monofunctional tridecafluorooctylpropyl POSS (polyhedral oligomeric silsesquioxane) monomer. The preparation method can obtain long branch chain type active fluorine-containing POSS, is simple and easy in process, low in cost, high in yield and higher in product purity, and is suitable for large-scale industrial production.

Description

technical field [0001] The present invention relates to a long-chain branched T7 configuration fluorine-containing POSS (heptadecafluorooctylpropyl cage silsesquioxane) and its functionalized derivatives. The present invention also relates to this T7 configuration thirteen The preparation method of fluorooctylpropyl cage silsesquioxane and its functionalized derivatives. Background technique [0002] Sanitation, water conservancy engineering, national defense and aerospace and other fields have very broad application prospects, and are closely related to people's daily life. Super-hydrophobic and super-oleophobic materials have a small surface energy, do not stick to water or oil, and can be made into various self-cleaning intelligent surface coatings, which can be used for surface sealing and waterproof and anti-corrosion of hydraulic / marine structures and components; Reduce surface resistance and increase buoyancy, so that aircraft, ships, submarines and other means of tr...

Claims

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Application Information

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IPC IPC(8): C07F7/21
Inventor 何辉蒋亚清徐晨李坤何功庆相秋迪
Owner HOHAI UNIV
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