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Synthesizing and curing method of carborane epoxy resin

A technology of epoxy resin and carborane, applied in epoxy resin glue, adhesive type, adhesive and other directions, can solve the problem that the addition reaction cannot be carried out

Inactive Publication Date: 2014-08-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is suitable for the addition reaction of substituted acetylene without amino, hydroxyl and epoxy groups, etc. This is because decaborane will disintegrate itself in compounds containing such polar groups, resulting in the addition reaction being unable to proceed

Method used

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  • Synthesizing and curing method of carborane epoxy resin
  • Synthesizing and curing method of carborane epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1,7-carborane diphenol (0.5996 g), tetramethylammonium bromide (0.0169 g) and epichlorohydrin (1.6891 g) were added to a 100 mL two-necked flask. Install a condensing reflux system, evacuate nitrogen, and shake the flask during the heating process to completely dissolve 1,7-carborane diphenol and tetramethylammonium bromide in epichlorohydrin. Under the protection of nitrogen, the temperature was raised to 100 °C for 2 hours, and a light yellow solid appeared at the bottom of the flask; after the temperature was lowered to 85 °C, 48 wt% NaOH aqueous solution (0.15 g NaOH) was added dropwise with a needle tube within 1 hour, during which time azeotropic desorption under normal pressure Remove water, and then keep the temperature and heat for 1 hour to obtain a light yellow viscous liquid, and there is a light yellow solid insoluble matter at the bottom of the flask; remove the viscous liquid, remove epichlorohydrin by rotary evaporation, and add to the crude product Tolu...

Embodiment 2

[0031] 1,7-Carborane diphenol (0.6004 g), tetramethylammonium bromide (0.0170 g) and epichlorohydrin (1.2580 g) were added to a 100 mL two-necked flask. Install a condensing reflux system, evacuate nitrogen, and shake the flask during the heating process to completely dissolve 1,7-carborane diphenol and tetramethylammonium bromide in epichlorohydrin. Under the protection of nitrogen, the temperature was raised to 50°C for 6 hours, and a light yellow solid appeared at the bottom of the flask; after the temperature was lowered to 70°C, a 48wt% NaOH aqueous solution (0.15gNaOH) was added dropwise with a needle within 1 hour, during which the azeotropic removal of water, and then keep the temperature and heat for 1h to obtain a light yellow viscous liquid, and there is a light yellow solid insoluble matter at the bottom of the flask; remove the viscous liquid, remove epichlorohydrin by rotary evaporation, and add toluene to the crude product React with 5wt% NaOH aqueous solution a...

Embodiment 3

[0033] 1,2-Carborane diphenol (1.00 g), tetramethylammonium bromide (0.028 g) and epichlorohydrin (2.82 g) were added to a 100 mL two-necked flask. Install a condensing reflux system, evacuate nitrogen, and shake the flask during the heating process to completely dissolve 1,2-carborane diphenol and tetramethylammonium bromide in epichlorohydrin. Under the protection of nitrogen, the temperature was raised to 100 ° C for 2 hours, and a light yellow solid appeared at the bottom of the flask; after the temperature was lowered to 85 ° C, 48 wt% NaOH aqueous solution (0.26 g NaOH) was added dropwise with a needle tube within 1 hour, during which time azeotropic desorption under normal pressure Remove water, and then keep the temperature and heat for 1 hour to obtain a light yellow viscous liquid, and there is a light yellow solid insoluble matter at the bottom of the flask; remove the viscous liquid, remove epichlorohydrin by rotary evaporation, and add to the crude product Toluene...

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Abstract

The invention provides a synthesizing and curing method of carborane epoxy resin. The method is used for preparing carborane epoxy resin from raw materials, namely, diphenyl carborane and epoxy chloropropane through two-step condensation polymerization. The synthesizing and curing method has the advantages of short reaction time, stability in operation, small temperature fluctuation, easiness for control, short alkaline adding time, capability of preventing a great deal of epoxy chloropropane from hydrolyzing, good and stable product quality and high yield. The obtained resin is simple and feasible in curing process, no harsh pollution control measures are needed, a cured product has excellent high-temperature carbon yield and high-temperature adhesive property, and the carborane epoxy resin can be used as a high-temperature-resistant adhesive.

Description

technical field [0001] The invention relates to a preparation and curing method of carborane epoxy resin. The method uses carborane diphenol and epichlorohydrin as raw materials to obtain the target product through two-step condensation polymerization, and the mixture of carborane epoxy resin, curing agent and solvent is cured under different temperature and time conditions. , to test its curing properties, mechanical properties and bonding properties used as an adhesive. Background technique [0002] Epoxy resin generally refers to a polymer prepolymer containing 2 or more epoxy groups, and is an important thermosetting resin. The cured epoxy resin is a kind of polymer synthetic material with high mechanical strength, good electrical insulation, high bonding strength, wide bonding surface, low shrinkage, good stability, and good processing performance. [0003] Carborane is a polyhedral compound composed of carbon, boron, and hydrogen. It is generally divided into open ty...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06C08G59/50C08G59/44C08G59/30C09J163/00
Inventor 张孝阿汪尧双刘杨齐士成齐僖李久龙
Owner BEIJING UNIV OF CHEM TECH
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