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Dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane and preparation method thereof

A technology of dodecafluoroheptyl propyl cage and fluoroheptyl propyl cage is applied in the field of preparation of dodecafluoroheptyl propyl cage type silsesquioxane, and achieves the reduction of synthesis cost, high yield, and high technology. Simple and easy effects

Inactive Publication Date: 2012-09-05
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If it is prepared as the corresponding cage-type silsesquioxane, it will endow it with better hydrophobic and oleophobic interfacial properties because of the special three-dimensional nanostructure of POSS, while there is no dodecafluoroheptylpropyl cage-type silsesquioxane at home and abroad Related reports on the synthesis and preparation of oxane

Method used

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  • Dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane and preparation method thereof
  • Dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane and preparation method thereof
  • Dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0031] At room temperature, 0.1 mol of 47.8g dodecafluoroheptylpropyltrimethoxysilane (trade name: Actyflon-G502, molecular formula: (CF3)2CFCFHCF(CF3)CH2CH2CH2CH2Si(OCH3)3) was added dropwise to 1000ml of methanol, and the catalyst concentrated Hydrochloric acid 100ml (concentration 37.5%), water 10ml, after the dropwise addition, stir at room temperature for 1 day, then let stand for 30 days, a large amount of white crystal-like precipitates are generated in the solution.

[0032] 2) The reaction mixture was filtered to obtain white crystals, washed with methanol, and dried to obtain some products. Concentrate the filtrate, filter, wash and dry to obtain the remaining part of the product. A total of 11.6 g of the product was obtained by combining the two, with a yield of about 28%.

[0033] Product dodecafluoroheptyl propyl cage type silsesquioxane of the present invention (dodecafluoroheptyl propyl POSS), its chemical molecular formula is: ((CF 3 ) 2 CFCFHCF(CF 3 )CH 2...

Embodiment 2～6

[0038] The preparation method of dodecafluoroheptylpropyl cage silsesquioxane, its specific steps are the same as in Example 1, the preparation process parameters, raw materials used and specific consumption Table 1:

[0039] Preparation process parameters, raw materials used and specific consumption in table 1 embodiment 2~6

[0040]

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Abstract

The invention provides a preparation method of dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane, which comprises the following steps: dripping each 1mol of dodecafluoroheptyl-propyl-trimethoxylsilane into 250-10000ml of organic solvent under the condition of 0-40 DEG C, carrying out hydrolysis condensation reaction under the action of acid catalysis, carrying out the reaction for a certain period of time, and carrying out concentration, filtration, drying and other steps for preparing dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane (dodecafluoroheptyl-propyl POSS)crystals. The invention further provides the dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane. The method has simple and easy process, low cost, high yield and high product purity, and the prepared dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane product has excellent hydro-oleophobic performances, heat resistance, flame retardance and low dielectric constant performance, and can be widely applied in the fields of polymer modification, hydro-oleophobic interface materials, flame retardants, low dielectric constant materials, building coatings, space materials, medical materials, light-emitting materials, liquid crystal materials and the like.

Description

technical field [0001] The present invention relates to a dodecafluoroheptylpropyl cage silsesquioxane (dodecafluoroheptylpropyl POSS), and the present invention also relates to this dodecafluoroheptylpropyl cage silsesquioxane method of preparation. Background technique [0002] The molecular formula of Polydehral Oligomer Silsesquioxane (POSS) is (RSiO 1.5 ) 8 , the cage-shaped skeleton is composed of SiO bonds, with a size of about 1.5nm. POSS molecules are highly consistent on the nanometer scale and can be uniformly dispersed in the matrix at the molecular level, which can further optimize the interaction between material components and effectively knead and polymerize. With the advantages of good processing technology, low cost, high strength and stable performance of inorganic materials, it endows materials with better performance and solves the problems that traditional inorganic nanoparticle modified polymers cannot solve. The POSS cage skeleton composed of silic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21
Inventor 何辉蒋亚清张继尹史燕南陆佳路维
Owner HOHAI UNIV
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