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Preparation method for benzoxazine intermediate and synthetic resin of intermediate

A technology of benzoxazine and synthetic resin, which is applied in the field of thermosetting resin and its preparation, can solve the problem of no combination of benzoxazine and raw lacquer, and achieve the elimination of human toxicity, enhanced heat resistance and system stability , High heat resistance effect

Inactive Publication Date: 2012-05-02
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Looking at all the relevant patents and professional literature on benzoxazine and lacquer, no one has combined benzoxazine and lacquer

Method used

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  • Preparation method for benzoxazine intermediate and synthetic resin of intermediate
  • Preparation method for benzoxazine intermediate and synthetic resin of intermediate
  • Preparation method for benzoxazine intermediate and synthetic resin of intermediate

Examples

Experimental program
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Effect test

Embodiment 1

[0067] Add 1.5g paraformaldehyde and 2.3g aniline to 20mL dioxane, control the reaction temperature not to exceed 30°C, and adjust the pH value to 8 with triethylamine to generate N-dimethylol compound and keep the temperature constant for 30min , then add a mixed solution of 9.0g urushiol and 10mL dioxane, heat up to 90°C to reflux, keep the mixed solution reacting at this reflux temperature for 6h, and generate a benzoxazine intermediate solution. After the reaction, the obtained solution was distilled off under reduced pressure to remove dioxane, and 100 mL of dichloromethane was used to dissolve the product, washed 3 times with water, and anhydrous MgSO 4 After drying, dichloromethane was distilled off under reduced pressure, and the red viscous liquid was obtained by vacuum drying, which was a novel benzoxazine intermediate containing urushiol-like structure.

[0068] Pour the above-mentioned benzoxazine intermediate into a mold, and cure in sections in an electric thermo...

Embodiment 2

[0070] Add 3.0 g of paraformaldehyde and 5.0 g of 4,4'-diaminodiphenylmethane into 20 mL of dioxane, control the reaction temperature not to exceed 30 ° C, and adjust the pH value to 8 with triethylamine to generate N-dimethylol compound and keep it for 30min, then add a mixed solution of 17.9g urushiol and 20mL dioxane, heat up to reflux at 90°C, keep the mixed solution reacting at this reflux temperature for 6h, and generate benzoxazine intermediate solution. After the reaction, the obtained solution was distilled under reduced pressure to remove dioxane, and 100 mL of dichloromethane was used to dissolve the product, washed with water for 3 times, and anhydrous MgSO 4 After drying, dichloromethane was distilled off under reduced pressure, and the red viscous liquid was obtained by vacuum drying, which was a novel benzoxazine intermediate containing urushiol-like structure.

[0071] Pour the above-mentioned benzoxazine intermediate into a mold, and cure in sections in an el...

Embodiment 3

[0073] Add 1.5g of paraformaldehyde, 2.3g of aniline, and 9.0g of urushiol into the reaction flask, mix well with mechanical stirring at low temperature (0-10°C), heat to 90°C for 1.5h, and keep stirring vigorously during this period . After the reaction, the volatile small molecules were distilled off under reduced pressure, cooled at room temperature, added a fat-soluble solvent to dissolve the product, filtered and washed 5 times with water, using anhydrous MgSO 4 After drying, the solvent is distilled off under reduced pressure, and vacuum-dried to obtain a novel benzoxazine intermediate containing an urushiol-like structure.

[0074] Pour the above-mentioned benzoxazine intermediate into a mold, and cure in sections in an electric thermostat to obtain a thermosetting benzoxazine resin material containing an urushiol-like structure. The curing temperature rise process is 100°C / 1h, 140°C / 1h, 180°C / 1h, 220°C / 1h.

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Abstract

The invention discloses a preparation method for a benzoxazine intermediate and a synthetic resin of the intermediate. The method comprises the following steps: adding 2 to 2.4 parts by mol of an aldehyde solution with a mass percent of 35 to 40% and 1 part to 1.2 parts by mol of primary amine compounds into 80 to 120 parts by mol of an organic solvent, controlling reaction temperature to be no more than 30 DEG C, adjusting the pH value of an obtained mixture to be 7 to 14, maintaining the mixture at a constant temperature for 30 minutes, adding 1 part by mol of urushiol, heating an obtained mixture to a temperature of 90 DEG C, allowing the mixture to react for 5 to 10 hours, carrying out vacuum distillation on a reaction solution, dissolving a product with a fat-soluble solvent, rinsing the product 3 to 5 times, carrying out drying after removal of the solvents so as to obtain the desired benzoxazine intermediate, and curing the benzoxazine intermediate in an electrothermostat at different stages. According to the invention, the considerable advantages of a simple synthetic method, easily available raw materials, low cost, low viscosity, a liquid state at normal temperature and suitability for industrial production are achieved; polymerized polybenzoxazine has excellent heat resistance and mechanical properties.

Description

technical field [0001] The invention relates to the technical field of thermosetting resin and its preparation, in particular to a preparation method of a benzoxazine intermediate and a synthetic resin thereof. Background technique [0002] Raw lacquer is a milky white milky liquid that flows out from the cut of the phloem of the lacquer tree. It is an important natural polymer material. The use of raw lacquer has a history of more than 7,000 years. The raw lacquer produced in my country has a large output and excellent quality, accounting for more than 85% of the world's total gas production, and is one of the important materials for traditional export. The economic value of raw lacquer is very high. It has the characteristics of corrosion resistance, high hardness, heat resistance, water insulation and high insulation, and high gloss. It is known as the "king of paint". Raw lacquer has many uses in the fields of national defense and military industry, chemical industry, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D265/16C08G73/06
Inventor 张广照徐洪礼
Owner SOUTH CHINA UNIV OF TECH
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