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Tridecafluorooctyl propyl cage-shaped silsesquioxane and preparation method thereof

A technology of fluorooctylpropyl cage and fluorooctylpropyltrimethoxysilane is applied in the field of preparation of tridecafluorooctylpropyl cage-type silsesquioxane, and can solve the problem that fluorine-containing POSS structure compounds are difficult to synthesize and other problems, to achieve the effect of good separation effect, simple and easy process, and high yield

Inactive Publication Date: 2012-07-04
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] In order to solve the problem that fluorine-containing POSS structure compounds with long carbon chain structure and many fluorine atoms are difficult to synthesize in the prior art, the invention provides a tridecafluorooctylpropyl cage-type silsesquioxane and its preparation The method has the advantages of simple and convenient preparation process, cheap and easy-to-obtain raw materials, long carbon chain structure and large number of fluorine atoms

Method used

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  • Tridecafluorooctyl propyl cage-shaped silsesquioxane and preparation method thereof
  • Tridecafluorooctyl propyl cage-shaped silsesquioxane and preparation method thereof
  • Tridecafluorooctyl propyl cage-shaped silsesquioxane and preparation method thereof

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preparation example Construction

[0037] The preparation method of tridecafluorooctylpropyl cage-type silsesquioxane provided by the invention, the specific steps are:

[0038] Step 1. Add 1mol of tridecafluorooctylpropyltrimethoxysilane dropwise into 250-10000ml of organic solvent, then add dropwise 0.5-1.5mol of acid catalyst, 0-250ml of deionized water, and then stir evenly after the dropwise addition , heated to the reflux temperature of the organic solvent, reacted under reflux conditions for 12 to 24 hours, and then stood at room temperature for 7 to 30 days, until a large amount of white crystal precipitates were formed in the solution; in order to obtain a better reaction effect, you can add some deionized water.

[0039] Described organic solvent selects any one or the mixture of several in ethanol, methyl alcohol, acetone, THF, propanol or Virahol usually, is preferably methyl alcohol or ethanol; Described acid catalyst is hydrochloric acid, nitric acid, sulfuric acid, formic acid or Any one or a mi...

Embodiment 1

[0050] 52.4g of tridecafluorooctylpropyltrimethoxysilane (trade name: Actyflon-G602, molecular formula: C 6 f 13 CH 2 CH(CH 3 )C 3 h 6 Si(OCH 3 ) 3 ) 0.1mol dropwise added 8000ml ethanol, then added catalyst concentrated hydrochloric acid 100ml (concentration 37.5%), water 10ml. White crystalline precipitate.

[0051] 2) The reaction mixture was filtered to obtain white crystals, washed with methanol, and dried to obtain some products. The filtrate was heated and concentrated to 2000ml, the organic solvent was recovered, and 14000ml of water was added under agitation (after concentration, the volume ratio of the filtrate to water was 1:7), filtered, washed, and vacuum-dried. A total of 21.4 g of the product was obtained by combining the two, with a yield of about 47%.

[0052] Product tridecafluorooctylpropyl cage type silsesquioxane of the present invention (tridecafluorooctylpropyl POSS), its chemical molecular formula is: (CF 3 (CF 2 ) 5 CH 2 CH(CH 3 )CH 2 CH...

Embodiment 2～6

[0058] The preparation method of tridecafluorooctylpropyl cage silsesquioxane, its specific steps are the same as in Example 1, the preparation process parameters, raw materials used and specific consumption Table 1:

[0059] Preparation process parameters, raw materials used and specific consumption in table 1 embodiment 2~6

[0060]

[0061]

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Abstract

The invention provides a tridecafluorooctyl propyl cage-shaped silsesquioxane and a preparation method thereof. The preparation method comprises the following steps: tridecafluorooctyl propyl polyhedral oligomeric silsesquioxane is dripped into an organic solvent; the tridecafluorooctyl propyl cage-shaped silsesquioxane and the organic solvent are evenly mixed in the presence of an acid catalyst;the mixture is heated to an organic solvent backflow temperature for reaction, and a standing reaction is carried out at room temperature; after a great quantity of white crystalline precipitates is produced in the solution, the mixture is pumped and filtered to obtain the white crystalline precipitates; then the obtained white crystalline precipitates are washed and dried in vacuum to obtain white tridecafluorooctyl propyl cage-shaped silsesquioxane. Filtrate obtained by pumping and filtering is heated and concentrated to 1 / 4 volume of the original filtrate volume; the organic solvent is recovered; then, the concentrated filtrate is added into water while stirred; then the obtained product is filtered, washed and dried in vacuum to obtain the white tridecafluorooctyl propyl cage-shaped silsesquioxane. The total recovery is 37-50%. The invention has simple and easy technology, low cost, high yield and high purity of product, the product has excellent hydrophobicity and oleophobic property and has excellent thermal stability and flame retardance and low dielectric constant.

Description

technical field [0001] The present invention relates to a tridecafluorooctylpropyl cage silsesquioxane (tridecafluorooctylpropyl POSS), and the present invention also relates to this tridecafluorooctylpropyl 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, and the molecules are highly consistent on the nanoscale, and can be uniformly dispersed in the matrix at the molecular level, which can further optimize the interaction between material components and effectively knead polymer materials. The advantages of low cost, high strength and stable performance of inorganic materials endow the material with better performance, which solves the problems that traditional inorganic nanoparticle modified polymers cannot solve. The POSS cage skeleton composed of silicon and oxygen elements has good heat resistance and flame r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21
Inventor 何辉蒋亚清史燕南谢岩陶涛
Owner HOHAI UNIV
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