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Preparation method of bisphenol A benzoxazine resin with high stability

A benzoxazine, stability technology, applied in the field of preparation of bisphenol A benzoxazine, can solve the problem of easy precipitation of benzoxazine solids, etc.

Active Publication Date: 2011-09-21
HAISO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention provides a highly stable bisphenol A benzoxazine to solve the problem of easy precipitation of benzoxazine solids and chemical storage stability in the existing bisphenol A benzoxazine resin solution during transportation and storage preparation method

Method used

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  • Preparation method of bisphenol A benzoxazine resin with high stability
  • Preparation method of bisphenol A benzoxazine resin with high stability

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] At room temperature, add 93 grams (1mol) of aniline and 60 grams (2mol) of paraformaldehyde into a 1000ml four-necked reaction flask equipped with a reflux and water removal device, stir for 0.5 hours, then gradually raise the temperature to 50-80°C and react for 5 hours. Then add 114 grams (0.5mol) of bisphenol A, and add Pd(OAc) in 3 times on average 2 2H 2 O 1 g, heat up to 90-105 °C for 8 hours and remove water, then gradually heat up to 100-120 °C and keep reacting for 1.5 hours, add 100 g of butanone, cool the product to obtain bisphenol A benzoxazine resin solution.

Embodiment 2

[0023] At room temperature, add 59 grams (1mol) of propylamine and 216 grams (2mol) of benzaldehyde into a 1000ml four-necked reaction flask equipped with a reflux and water removal device, stir for 1 hour, then gradually raise the temperature to 55-80°C and react for 5 hours. Then add 114 grams (0.5mol) of bisphenol A, and add Mg(OAc) in 3 times on average 2 4H 2 O 1.5g, heat up to 90-105°C to react for 8.5 hours and remove water, then gradually raise the temperature to 100-120°C and keep the reaction for 1-2 hours, then add 80g of methyl ethyl ketone, cool the product to obtain bisphenol A benzox oxazine resin solution.

Embodiment 3

[0025] At room temperature, add 97 grams (1mol) of furfurylamine and 64 grams (2.1mol) of paraformaldehyde into a 1000ml four-necked reaction bottle equipped with a reflux and water removal device, stir for 1 hour, then gradually raise the temperature to 50-90°C and react for 4 Hour. Then add 114 grams (0.5mol) of bisphenol A, and add Co(OAc) in 3 times on average 2 4H 2 O 3 grams, heat up to 90-110 ° C for 8.5 hours and remove water, then gradually heat up to 100-120 ° C and keep the reaction for 1-2 hours, add 100 grams of ethylene glycol methyl ether, and cool the product to obtain bisphenol A benzene Oxazine resin solution.

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Abstract

A preparation method of bisphenol A benzoxazine resin with high stability is characterized in that bisphenol A, arabino compounds and primary amine react to synthesize the benzoxazine resin by taking a transition metal complex as a catalyst in the presence of organic solvents or inorganic solvents. The ring-forming rate, the pre-polymerizing rate and the molecular weight distribution of the benzoxazine resin can be stably controlled. The benzoxazine resin has stable physical and chemical storage stability and less possibility of separating out; and a condensate of the benzoxazine resin has excellent high-temperature resistant performance, mechanical property and flame-retardant performance.

Description

technical field [0001] The invention relates to a preparation method of bisphenol A benzoxazine with high stability. Background technique [0002] Bisphenol A benzoxazine is a heat-resistant thermosetting resin produced by bisphenol A, amine, and aldehyde under the action of heat or a catalyst. It has easy-to-obtain raw materials, simple synthesis process, low cost and color after curing. The advantage of being shallower, but due to the different process conditions in the preparation process of bisphenol A benzoxazine, the ring formation rate and prepolymerization rate of benzoxazine are not the same, resulting in a significant difference in the storage stability of benzoxazine big difference. This instability is mainly manifested in the fact that the benzoxazine resin solution is easy to precipitate benzoxazine solids during transportation and storage and has poor chemical stability. The instability of the gel time under the action of heat is manifested in the continuous ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06
Inventor 徐庆玉李翔王洛礼张荔英龚敏
Owner HAISO TECH
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