Preparation method of sulfate brace type benzoxazine resin

A technology of benzoxazine and sulfuric acid ester, which is applied in the field of preparation of benzoxazine resin, can solve the problems of low impact resistance, high brittleness, poor workmanship, etc., achieve good heat resistance and modulus, and the preparation method is simple , highly operable effect

Inactive Publication Date: 2015-07-01
JIANGXI SUNWAY CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Phenolic resin is the earliest thermosetting resin that was artificially synthesized and successfully industrialized. For a long time, phenolic resin has been widely used in various fields, such as construction, paint, automobile, electronics and other industries. Its main advantages include good heat resistance , good acid resistance, fast curing speed and excellent flame retardancy and electrical properties. At the same time, low-cost raw materials and manufacturing processes are also the main reasons for occupying a large market share. However, traditional phenolic resins also have some inevitable Disadvantages: curing requires strong acid as a catalyst, volatiles are produced during curing, the volume of the product shrinks more seriously, the storage period of the prepolymer is shorter, and the manufacturability is poor, etc.
Ordinary benzoxazine resins without toughening treatment generally have high brittleness (low impact resistance), which cannot meet the needs of practical applications. Therefore, it is very important to improve the toughness of the resin. However, how to maintain the toughness of the resin itself while improving the toughness Glass transition temperature and modulus, this is a very challenging problem, although the current traditional thermosetting resin toughening agent can toughen benzoxazine resin, but the test results show that in most cases , these conventional toughening agents will significantly reduce the glass transition temperature and modulus of the final benzoxazine resin product, in order to fundamentally solve these problems, it is necessary to develop a new benzoxazine monomer, from the structure and Finding solutions on functional groups

Method used

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  • Preparation method of sulfate brace type benzoxazine resin
  • Preparation method of sulfate brace type benzoxazine resin
  • Preparation method of sulfate brace type benzoxazine resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] [Example 1] The structural formula of the benzoxazine resin and the phenolic compound used is as follows by solution method:

[0035]

[0036] At room temperature, add aniline (1mol), paraformaldehyde (2mol) and toluene (240mL) into a 1L three-neck round bottom flask equipped with a reflux condenser and a thermometer, gradually raise the temperature to 40°C and react for 15 minutes. Then add phenolic compound (0.5mol) and Na2CO3 (0.4 wt%) and stir evenly, then raise the temperature to 60-80°C and react for 4 hours. The reactant was washed three times with water, and the solvent was distilled off under reduced pressure to obtain benzoxazine resin with a yield of 81.4%.

Embodiment 2

[0037] [Example 2] The structural formula of the benzoxazine resin and the phenolic compound used is as follows:

[0038]

[0039] At room temperature, add aniline (1mol), paraformaldehyde (1.9mol) and chloroform (200mL) into a 1L three-neck round bottom flask equipped with a reflux condenser and a thermometer, gradually raise the temperature to 50oC and react for 30 minutes. Then add phenolic compound (0.5mol) and NaOH (0.2 wt%) and stir evenly, then raise the temperature to 70-90°C and react for 6 hours. The reactant was washed three times with water, and the solvent was distilled off under reduced pressure to obtain the residual moisture to obtain a benzoxazine resin with a yield of 82.3%.

Embodiment 3

[0040] [Example 3] The structural formula of the benzoxazine resin and the phenolic compound used is as follows:

[0041]

[0042] At room temperature, add methylamine (1.2mol), formaldehyde aqueous solution (2mol) and dioxane (300mL) into a 1L three-neck round bottom flask equipped with a reflux condenser and a thermometer, gradually raise the temperature to 45oC and react for 40 minutes. Then add phenolic compound (0.5mol) and triethylamine (3 wt%) and stir evenly, then raise the temperature to 80-100°C and react for 3.5 hours. The reactant was washed three times with water, and the solvent was distilled off under reduced pressure to obtain benzoxazine resin with a yield of 83.6%.

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Abstract

The invention relates to a preparation method of sulfate brace type benzoxazine resin. The preparation method comprises the following steps: synthesizing sulfate brace type benzoxazine resin by taking phenol compounds, aldehyde and amine as reactants by adopting a solution method or a melting method under the action of a catalyst, uniformly mixing primary amine and aldehyde in an organic solvent, reacting for 10-60 minutes at 40-60 DEG C, then adding the phenol compounds and the catalyst into a mixture, heating to 60-120 DEG C, reacting for 1-8 hours, washing by water after reaction, and removing the solvent and residual water in a system to obtain a product. The sulfate brace type benzoxazine resin disclosed by the invention has relatively more aromatic rings in a molecular structure, and is high in sulfate group stability to ensure that the resin can obtain relatively good heat resistance and modulus after being cured; in cured molecules, the distance between molecular chains is relatively large, and thus the crosslinking degree of cured products can be relatively reduced; meanwhile, a sulfate group has relatively good flexibility, and thus sulfate brace type benzoxazine resin molecules have relatively good toughness compared with general benzoxazine resin; and the preparation method disclosed by the invention is simple and is worthy of being popularized.

Description

technical field [0001] The invention relates to a preparation method of a benzoxazine resin, in particular to a preparation method of a sulfate propylene type benzoxazine resin. Background technique [0002] Phenolic resin is the earliest thermosetting resin that was artificially synthesized and successfully industrialized. For a long time, phenolic resin has been widely used in various fields, such as construction, paint, automobile, electronics and other industries. Its main advantages include good heat resistance , good acid resistance, fast curing speed and excellent flame retardancy and electrical properties. At the same time, low-cost raw materials and manufacturing processes are also the main reasons for occupying a large market share. However, traditional phenolic resins also have some inevitable Disadvantages: curing requires strong acid as a catalyst, volatiles are produced during curing, the volume of the product shrinks more seriously, the storage period of the p...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C08G73/06
Inventor余小康朱兆江朱刚
OwnerJIANGXI SUNWAY CHEM CO LTD