Synthesis method of crude phenol-based benzoxazines resin prepolymers

The technology of a crude phenolic benzene and a synthesis method is applied in the synthesis field of resin prepolymer, can solve the problems of environmental pollution, high process cost and the like, and achieves the effects of simple and easy-to-obtain raw materials, low cost, and improved utilization of added value.

Inactive Publication Date: 2016-08-24
SOUTHWEST PETROLEUM UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high cost of purification and separation process, crude phenol is usually burned as coking waste, which has great pollution to the environment

Method used

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  • Synthesis method of crude phenol-based benzoxazines resin prepolymers
  • Synthesis method of crude phenol-based benzoxazines resin prepolymers
  • Synthesis method of crude phenol-based benzoxazines resin prepolymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0023] Example 2: A synthetic method of a crude phenolic benzoxazine resin prepolymer, which uses crude phenols, formaldehydes and primary amines as raw materials, adding a reaction solvent and reacting at 90°C for 7 hours, and the reaction is complete Finally, the organic phase was washed with deionized water and then separated, added anhydrous magnesium sulfate to dry for 3 hours and filtered, and the filtrate was vacuum-dried at 50°C for 6 hours to obtain a crude phenolic benzoxazine resin prepolymer, wherein , the molar mass ratio of the crude phenols, formaldehydes and primary amine compounds is 3:2:3; the crude phenols are industrial crude phenols and phenolic compounds The blended phenols, wherein, the mass percentage of crude phenols in the blended phenols is ≥50%; R 1 is one or more H; the primary amine compound is R 2 NH 2 , R 2 for C 2 -C 20 Halogenated alkyl; Described formaldehyde is paraformaldehyde; Described reaction solvent is chloroform; The H NMR spect...

Embodiment 3

[0024] Embodiment 3: a kind of synthetic method of crude phenolic benzoxazine resin prepolymer, it is to be raw material with crude phenols, formaldehydes and primary amine compounds, add reaction solvent and react at 72 ℃ for 5.5h, react After completion, wash the organic phase with deionized water and separate the organic phase, add anhydrous magnesium sulfate to dry for 2.5 hours and then filter, and the filtrate is vacuum-dried at 40°C for 4.5 hours to obtain the crude phenolic benzoxazine resin prepolymerized body, wherein the molar mass ratio of the crude phenols, formaldehydes and primary amine compounds is 1.5:2:0.8; the crude phenols are industrial crude phenols and phenolic compounds The blended phenols, wherein, the mass percentage of crude phenols in the blended phenols is ≥50%; R 1 is a halogen atom; the primary amine compound is R 2 NH 2 , R 2 for C 2 -C 20 Aminoalkyl; the formaldehydes are the mixture of aqueous formaldehyde and paraformaldehyde; the react...

Embodiment 4

[0025]Example 4: A synthetic method of a crude phenolic benzoxazine resin prepolymer, which uses crude phenols, formaldehydes and primary amines as raw materials, adding a reaction solvent and reacting at 75°C for 6 hours, and the reaction is complete Finally, the organic phase was washed with deionized water, and the organic phase was separated, dried by adding anhydrous magnesium sulfate for 2.8 hours, and then filtered. The filtrate was vacuum-dried at 42°C for 5 hours to obtain a crude phenolic benzoxazine resin prepolymer. Wherein, the molar mass ratio of the crude phenols, formaldehydes and primary amine compounds is 1.8:2:1; the crude phenols are industrial crude phenols and phenolic compounds The blended phenols, wherein, the mass percentage of crude phenols in the blended phenols is ≥50%; R 1 for C 1 -C 20 The alkyl or alkoxy group; the primary amine compound is R 2 NH 2 , R 2 The formaldehyde is an amino group; the formaldehyde is an aqueous formaldehyde soluti...

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Abstract

The invention discloses a synthesis method of crude phenol-based benzoxazines resin prepolymers. The method takes crude phenols, formaldehydes and primary amines compounds as raw materials, and comprises the steps of carrying out a reaction for 5-7 hours at the temperature of 70-90 DEG C, and then carrying out aftertreatment to obtain the crude phenol-based benzoxazines resin prepolymers. The synthesis method is easy in obtaining of raw materials, low in cost and suitable for large-scale industrial production; the synthesis method is simple in reaction technology, does not need any catalyst, does not need inert gas for protection, and is higher in yield and good in repeatability. The novel crude phenol-based benzoxazine resin prepared by the invention is the same as other benzoxazine resins, and can be cross-linked and solidified under the condition of heating or adding a catalyst so as to obtain corresponding thermosetting resin.

Description

technical field [0001] The invention relates to a method for synthesizing a resin prepolymer, in particular to a method for synthesizing a crude phenolic benzoxazine resin prepolymer. Background technique [0002] Crude phenol is obtained by processing the phenol-containing fraction obtained from the distillation of coal tar, and can be used to produce synthetic fibers, pesticides, engineering plastics and dye intermediates. It is mainly used to extract phenol, o-cresol, m-p-cresol, xylenol, 3,5-xylenol, etc. It is a solvent for high-grade insulating paint and an important raw material for plastics, medicine, and antifungal agents. [0003] Due to the complex composition of crude phenol, the boiling points of the components are very close, and the processing and separation process is cumbersome. At present, the processing volume of crude phenol in my country is still relatively low, mainly to separate single components such as phenol, m-cresol, ortho-cresol, and mixed creso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06
CPCC08G73/06
Inventor 石伟解正峰吴新祥王晓刚陈科罗修文于文涛张艺鹏
Owner SOUTHWEST PETROLEUM UNIV
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