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Preparation method for phenolic benzoxazine resin

A technology of benzoxazine and phenolic resin, which is applied in the field of preparation of phenolic benzoxazine, can solve the effects of benzoxazine resin storage stability, cured product heat resistance and flame retardancy, oxazine ring Issues such as low proportion

Active Publication Date: 2013-08-28
HAISO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the small number of moles of aldehydes and amines relative to -OH, some -OH in the thermoplastic phenolic resin (Novolak phenolic resin) failed to participate in the reaction and were exposed, resulting in the presence of active reactive functional groups -OH in the product benzoxazine resin , so that the storage stability of the product benzoxazine resin is greatly affected, and because the proportion of oxazine rings in the benzoxazine resin is relatively small, the heat resistance and flame retardancy of the cured product are also greatly affected influences

Method used

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  • Preparation method for phenolic benzoxazine resin
  • Preparation method for phenolic benzoxazine resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] At room temperature, add 121 grams of aniline and 75 grams of paraformaldehyde into a reaction flask containing a water removal device, stir for 2 hours, then gradually raise the temperature to 60-90° C. and react for 5 hours. Then add 104 grams of thermoplastic phenolic resin (Novolak phenolic resin), and 2.4 grams of Zn (OAc) 2 2H 2 Add O in 3 times on average, raise the temperature to 80-100°C for 7 hours and remove water, then gradually raise the temperature to 100-130°C and keep the reaction for 2 hours to obtain benzoxazine resin, wash the benzoxazine resin with methanol and after drying, dissolve the benzoxazine resin with methyl ethyl ketone to obtain a novolak type benzoxazine resin solution. The resin cyclization rate is shown in Table 1, and the storage stability of the resin is shown in Table 2.

Embodiment 2

[0019] At room temperature, add 62 grams of allylamine and 226 grams of benzaldehyde into a reaction flask containing a water removal device, stir for 3.5 hours, then gradually raise the temperature to 60-90° C. and react for 3.5 hours. Then add 104 grams of thermoplastic phenolic resin (Novolak phenolic resin), and 2.8 grams of Mn(OAc) 2 4H 2 Add O in 3 times on average, raise the temperature to 80-100°C for 5.5 hours and remove water, then gradually raise the temperature to 100-130°C and keep the reaction for 3 hours to obtain benzoxazine resin, wash the benzoxazine resin with ethanol After drying, the benzoxazine resin is dissolved with 2-butanone to obtain a phenolic benzoxazine resin solution. The resin cyclization rate is shown in Table 1, and the storage stability of the resin is shown in Table 2.

Embodiment 3

[0021] At room temperature, add 118 grams of furfurylamine and 64 grams of paraformaldehyde into a reaction flask containing a water removal device, stir for 2.5 hours, then gradually raise the temperature to 60-90°C and react for 4 hours. Then add 104 grams of thermoplastic phenolic resin (Novolak phenolic resin), and 2.8 grams of Co(OAc) 2 4H 2 O and 1.1 g Ni(OAc) 2 2H 2 The mixture of O was added in 3 times on average, the temperature was raised to 80-100°C for 7 hours and the water was removed, and then the temperature was gradually raised to 100-130°C and kept for 2.5 hours to obtain benzoxazine resin. Wash the benzoxazine with n-propanol After the oxazine resin is dried, the benzoxazine resin is dissolved with toluene to obtain a phenolic benzoxazine resin solution.

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Abstract

The invention discloses a preparation method for a phenolic benzoxazine resin. The resin has a high oxazine ring formation rate and high storage stability. The preparation method comprises the following step of: reacting a Novolak resin with an aldehyde compound and primary amine under the condition of organic solvent or no solvent by taking a metallic compound as a catalyst to synthesize the benzoxazine resin. In the preparation process of the benzoxazine resin, the metallic compound is used as the catalyst, and the mole ratio of the primary amine to phenolic hydroxy is more than 1, namely excessive primary amine and excessive aldehyde compound are used, so that the oxazine ring formation rate of the phenolic hydroxyl is greatly increased, and the storage stability of the benzoxazine resin is also greatly improved.

Description

technical field [0001] The invention relates to a preparation method of phenolic benzoxazine. Background technique [0002] Thermoplastic phenolic resins (Novolak phenolic resins, novolac resins) are easy to synthesize, in large quantities, and relatively low in cost. The benzoxazine resin prepared by it has the characteristics of low cost and high-quality production technology, and is suitable as a bulk product. In the thermoplastic phenolic resin synthesis process, the 2, 4, and 6 positions of phenol all have strong reactivity, which may make the prepared thermoplastic phenolic resin have no active hydrogen on the ortho-position of the hydroxyl group, containing this structure The phenolic hydroxyl group of the unit cannot form an oxazine ring structure with primary amines and aldehyde compounds. Although we can synthesize high ortho-position thermoplastic phenolic resins (Novolak phenolic resins) through reasonable processes and catalysts, there is at least one active h...

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
Owner HAISO TECH
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