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Synthesis and curing method of carborane benzo oxazine resin

A technology of benzoxazine and carborane, which is applied in the field of benzoxazine prepolymers containing carborane, can solve the problems that the addition reaction cannot be carried out, achieve strong thermal stability and thermal oxygen stability, and Handling of simple, short reaction time effects

Active Publication Date: 2015-02-04
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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  • Synthesis and curing method of carborane benzo oxazine resin
  • Synthesis and curing method of carborane benzo oxazine resin
  • Synthesis and curing method of carborane benzo oxazine resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] First, a 100mL three-neck flask equipped with a magnetic stirrer, a thermometer and a reflux condenser was placed in an ice bath, and then a mixed solution of formalin (37%) (0.3294g) and 8mL of dioxane was added to keep the temperature at 10°C Next, a mixed solution of aniline (0.1867 g) and 2 mL of dioxane was subsequently added, and stirred for 30 min. Dissolve 1,7-carborane bisphenol (0.3268g) in 10mL of dioxane, slowly add it dropwise to the above solution, raise the temperature to 94°C, and react for 8h. After the reaction, remove the solvent by rotary evaporation, dissolve the obtained viscous liquid in 80 mL of chloroform, wash with 200 mL of 1.5 mol / L NaOH solution for several times, and finally wash with deionized water until neutral, remove the chloroform by rotary evaporation, and dry in vacuum at 70 °C. Dry for 5h to obtain the product. FTIR,ν(cm -1 , KBr tablet): 939.42 (characteristic peak of oxazine ring), 1498.02 and 1599.45 (skeleton vibration of ben...

Embodiment 2

[0038] First, a 100mL three-neck flask equipped with a magnetic stirrer, a thermometer and a reflux condenser was placed in an ice bath, and then a mixed solution of formalin (37%) (0.3278g) and 8mL of dioxane was added to keep the temperature at 10°C. Next, a mixed solution of methylamine (0.0622 g) and 2 mL of dioxane was subsequently added, and stirred for 30 min. Dissolve 1,2-carborane bisphenol (0.3264g) in 10mL of dioxane, slowly add it dropwise to the above solution, raise the temperature to 100°C, and react for 8h. After the reaction, remove the solvent by rotary evaporation, dissolve the obtained viscous liquid in 80 mL of chloroform, wash with 200 mL of 1.5 mol / L NaOH solution for several times, and finally wash with deionized water until neutral, remove the chloroform by rotary evaporation, and dry in vacuum at 70 ° C. Dry for 5h to obtain the product. FTIR,ν(cm -1 , KBr tablet): 934.20 (characteristic peak of oxazine ring), 751.53 and 837.97 (C-H bending vibratio...

Embodiment 3

[0040] First, a 100mL three-necked flask equipped with a magnetic stirrer, a thermometer and a reflux condenser was placed in an ice bath, then a mixed solution of formalin (37%) (0.3275g) and 8mL of dioxane was added to keep the temperature at 10°C Thereafter, a mixed solution of allylamine (0.1143 g) and 2 mL of dioxane was subsequently added, and stirred for 30 min. Dissolve 1,7-carborane bisphenol (0.3277g) in 10mL of dioxane, slowly add it dropwise to the above solution, raise the temperature to 94°C, and react for 6h. After the reaction, remove the solvent by rotary evaporation, dissolve the obtained viscous liquid in 80 mL of chloroform, wash with 200 mL of 1.5 mol / L NaOH solution for several times, and finally wash with deionized water until neutral, remove the chloroform by rotary evaporation, and dry in vacuum at 70 °C. Dry for 5h to obtain the product. FTIR,ν(cm -1 , KBr tablet): 939.42 (characteristic peak of oxazine ring), 750.34 and 828.05 (C-H bending vibratio...

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Abstract

The present invention designs a synthesis and curing method of carborane benzo oxazine resin, and a carborane-containing benzo oxazine prepolymer has the structural formula as shown in the specification, wherein Cb is o-carborane, m-carborane or p-carborane; R is alkyl, aryl and alkylaryl. The resin is prepared by using carborane bisphenol, formaldehyde and amine as raw materials and 1, 4-dioxane as a solvent. The prepolymer can be cured by simple heating in air atmosphere. The curing process is very simple and does not require strict pollution control measures. A curing product has good thermal stability and high temperature carbon residue rate, and can be used for the study of high temperature resistant materials.

Description

technical field [0001] The present invention relates to a process for preparing curable carborane-containing benzoxazine prepolymers and obtaining curable properties of the resulting product. Background technique [0002] Carborane is a polyhedral compound composed of three elements: carbon, boron and hydrogen. It is generally divided into open type and closed type. Among them, the open type has nest shape and network shape, while the closed type generally refers to the cage type. The formula structure is an icosahedron composed of two carbon atoms, ten boron atoms, and twelve hydrogen atoms. This cage-like carborane has the largest number and is the most stable, and it is one of the most important raw materials for the synthesis of heat-resistant polymer materials. Formula - dodecaborane (C 2 B 10 h 12 ). Carborane has three isomers, namely 1,2-carborane, 1,7-carborane and 1,12-carborane, and the corresponding positions are ortho, meta and para-carbon respectively bor...

Claims

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Application Information

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IPC IPC(8): C07F5/02C08G73/06C09J179/04
CPCC07F5/05C08G73/0688C09J179/04
Inventor 张孝阿王红睿韩果齐士成
Owner BEIJING UNIV OF CHEM TECH
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