Double-ring cage shape substituted silsesquioxane and its preparation method and uses

A technology of silsesquioxane and ring cage, applied in the field of polymer additives synthesis, can solve the problems of poor impact resistance, crack resistance and humidity and heat resistance, large internal stress and high cross-linking density, and achieve good permeability. effect, the effect of improving weather resistance and abrasion resistance

Inactive Publication Date: 2007-08-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, epoxy resin has high crosslinking density after curing, and has disadvantages such as large internal stress, brittleness, poor impact resistance, crack resistance, and heat and humidity resistance, and the commonly used amines and acid anhydrides are more toxic. It largely limits its application in some high-tech fields

Method used

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  • Double-ring cage shape substituted silsesquioxane and its preparation method and uses
  • Double-ring cage shape substituted silsesquioxane and its preparation method and uses
  • Double-ring cage shape substituted silsesquioxane and its preparation method and uses

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Stir and mix 36.4mL of 25% tetramethylammonium hydroxide aqueous solution with 54.6mL of distilled water, then add 1-oxo-1-phospha-2,6,7-trioxa in 3 times within 1h Bicyclo[2,2,2]octane-4-methylenealkoxy substituted tetracoordinated silicon (0.1mol), vigorously stirred during the feeding process to accelerate dissolution, stirred at 25°C for 20h, then heated to 65°C for 5h, Stop the reaction, remove a small amount of insoluble matter by suction filtration, the filtrate is light yellow, change to a distillation device, evaporate about 30mL of solvent, and place it in a refrigerator at 5°C to cool. After two days, a large amount of crystals are produced, take them out, and place them at room temperature for 1 hour to let them After the ethylene glycol crystals were dissolved, they were suction filtered, and the product was cleaned with 60 mL of acetone, and then dried at 60°C for 48 hours to obtain a white granular substance, which was a bicyclic cage-like substituted sils...

Embodiment 2

[0033] Potassium hydroxide (0.01mol) and methanol aqueous solution (79%wt, 68.8mL) were stirred and mixed evenly, and then 1-oxo-1-phospha-2,6,7-trioxa was added in portions within about 1 h Bicyclo[2,2,2]octane-4-methylenealkoxy was substituted with tetracoordinated silicon (0.1mol). During the process, vigorously stirred to accelerate the dissolution. The reaction was stirred at 30°C for 20h, and the temperature was raised to 60°C for 6h. Filter out a small amount of insoluble matter, the filtrate is light yellow, change to a distillation device, evaporate about 30mL of solvent, and then cool it in the refrigerator. After two days, a large amount of crystals are produced, take them out, and place them at room temperature for 1 hour to dissolve the ethylene glycol crystals. Afterwards, suction filtration, the product was washed with acetone (70 mL) and dried at 60° C. for 48 hours to obtain a white granular substance which was a bicyclic cage-shaped substituted silsesquioxane ...

Embodiment 3

[0036] Concentrated hydrochloric acid (2×10 -3 mol) and ethanol aqueous solution (25.4%wt, 36.2mL) were stirred and mixed evenly, and then 1-oxo-1-phospha-2,6,7-trioxabicyclo[2,2, 2] Octane-4-methylenealkoxy is substituted with tetracoordinated silicon (0.1mol). During the process, stir vigorously to accelerate the dissolution. Stir and react at room temperature (28°C) for 24h, heat up to 70°C for 5h, and remove it by suction filtration A small amount of insoluble matter, the filtrate was light yellow, changed to a distillation device, evaporated about 20mL of solvent, placed it in the refrigerator to cool, two days later a large number of crystals were produced, took it out, and placed it at room temperature for 1 hour to dissolve the ethylene glycol crystals, then pumped After filtering, the product was washed with acetone (80 mL) and dried at 60° C. for 48 hours to obtain a white granular substance which was a bicyclic cage-shaped substituted silsesquioxane according to the...

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Abstract

The invention discloses a bicyclo ring cage substituted sesquialter oxosilane and the method for preparing the same and its application. The compound possesses high sesquialter constructure, the core is cage sesquialter oxosilane, the eight apical angle are 1- oxo- 1- phosphora- 2, 6, 7- trioxa bicyclo [2, 2, 2]- 4- methylene sorbate. The method comprises: dissloving catalyst and solvent, adding bicyclo ring cage coordination silicon, reacting while stirring at room temperature; heating to 60- 70 Deg .C, stopping reaction, sucting, distilling part of solvent from filtering liquid and putting it in fridge for cooling, a large amount of crystal will be generated two days later, putting it at room temperature for 1 hour to make the ethandiol crystal disslove, sucting and drying the crystal at 60 Deg. C. The epoxide resin adjuvant is characterized by ability of increasing toughness, fire-retardancy, heat-proof quality, abradability, weatherability and anti ultraviolet absorption for epoxide resin, and hardening function.

Description

technical field [0001] The invention relates to the technical field of synthesis of polymer additives, in particular to an additive capable of simultaneously curing, flame retardant and toughening epoxy resins and a preparation method thereof. Background technique [0002] Epoxy resin (EP) is a kind of thermosetting resin, which is widely used in casting, packaging, coating, adhesive, composite material matrix and other aspects of electronic materials because of its excellent adhesion, mechanical strength, electrical insulation and other characteristics. However, epoxy resin has high crosslinking density after curing, and has disadvantages such as large internal stress, brittle quality, poor impact resistance, crack resistance, and heat and humidity resistance, and the commonly used amines and acid anhydrides are more toxic. It largely limits its application in some high-tech fields. [0003] A Chinese invention patent with application number CN200510034369.5, a phosphorus-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6596C07F9/6571C08L63/00C08K5/541
Inventor 刘安华张利利袁博曾幸荣
Owner SOUTH CHINA UNIV OF TECH
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