Production method for diamin type high fire-retardancy benzoxazine resin containing phosphor

A benzoxazine and diamine-based technology, applied in the field of thermosetting resin preparation, to achieve good flame retardancy, good thermal performance, and high heat resistance

Inactive Publication Date: 2008-07-16
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, no benzoxazine resin containing phosphorus itself without modification has been reported so far. We designed a benzoxazine intermediate with high phosphorus content by using phosphorus-containing diamine, monohydric phenol and formaldehyde as reaction raw materials. Body and high flame retardant benzoxazine resin

Method used

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  • Production method for diamin type high fire-retardancy benzoxazine resin containing phosphor
  • Production method for diamin type high fire-retardancy benzoxazine resin containing phosphor
  • Production method for diamin type high fire-retardancy benzoxazine resin containing phosphor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Synthesis of 3,3'-phosphophenyl-6-methyl-3,4-dihydro-2H-1,3-benzoxazine resin.

[0035] The preparation process of synthesizing benzoxazine resin with phosphorus-containing diamine: 2 (4-aminophenyl) phenyl phosphate, monohydric phenol: p-cresol and formaldehyde as raw materials:

[0036] Add 75ml of chloroform, 0.7g of triethylamine and 24ml of 35% formaldehyde solution in sequence into a 250ml three-neck flask equipped with a stirrer and a condenser, and stir to mix. Slowly add 25.6g of 2(4-aminophenyl)phenyl phosphate, control the reaction temperature not to exceed 30°C, and adjust the pH value to 7 with triethylamine to generate N-dimethylol compound and keep it stable in the solution ;

[0037] Add 15.5g p-cresol after reacting for 15min, heat up to reflux, stop the reaction after the mixed solution reacts at reflux temperature for 5h, and make N-dimethylol compound and phenolic hydroxyl group and the ortho-position on benzene ring produce condensation reaction, ...

Embodiment 2

[0042] Synthesis of 3,3'-phosphophenyl-5-methyl-3,4-dihydro-2H-1,3-benzoxazine resin.

[0043] The preparation process of synthesizing benzoxazine resin with phosphorus-containing diamine: 2 (4-aminophenyl) phenyl phosphate, monohydric phenol: m-cresol and formaldehyde as raw materials:

[0044] Add 90ml of chloroform, 0.84g of triethylamine and 28.8ml of 36% formaldehyde solution in sequence into a 250ml three-neck flask equipped with a stirrer and a condenser, and stir to mix. Slowly add 30.7g of 2(4-aminophenyl)phenyl phosphate, control the reaction temperature not to exceed 30°C, and adjust the pH value to 7 with triethylamine to generate N-dimethylol compound and keep it stable in the solution ;

[0045] After reacting for 15 minutes, add 18.6 g of m-cresol, raise the temperature to reflux, and stop the reaction after the mixed solution reacts at the reflux temperature for 5 hours, so that the N-dimethylol compound, the phenolic hydroxyl group and the ortho position on t...

Embodiment 3

[0050] Synthesis of 3,3'-Phenyl Phosphate-3,4-Dihydro-2H-1,3-Benzoxazine Resin

[0051] The preparation process of synthesizing benzoxazine resin with phosphorus-containing diamine: 2 (4-aminophenyl) phenyl phosphate, monohydric phenol: phenol and formaldehyde as raw materials:

[0052] Add 75ml of chloroform, 0.7g of triethylamine and 24ml of 37% formaldehyde solution in sequence to a 250ml three-necked flask equipped with a stirrer and a condenser, and stir to mix. Slowly add 25.6g of 2(4-aminophenyl)phenyl phosphate, control the reaction temperature not to exceed 30°C, and adjust the pH value to 7 with triethylamine to generate N-dimethylol compound and keep it stable in the solution ;

[0053] After reacting for 15 minutes, add 13.5g phenol, raise the temperature to reflux, and stop the reaction after reacting the mixed solution at the reflux temperature for 5 hours, so that the N-dimethylol compound and the phenolic hydroxyl group and its ortho position on the benzene ri...

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Abstract

The invention discloses a method for preparing diamine type phosphor-containing high flameproofing benzene-oxaxine resin, which uses phosphor-containing diamine, monohydric phenol and formaldehyde as raw reaction materials. A benzene-oxaxine midbody is introduced with a compound containing phosphor to synthesize a phosphor-containing flameproofing benzene-oxaxine midbody which is solidified and crosslinked to obtain thermosetting phosphor-containing high flameproofing benzene-oxaxine resin. Other fire retardants are not required to be added into the flameproofing materials which adopt the phosphor-containing flameproofing benzene-oxaxine resin of the invention as the basic flameproofing material; the flameproofing material using the resin has excellent flameproofing capacity, the flameproofing level can reach V-0, thermal capacity is rather good and the vitrification transforming temperature can reach 229 DEG C. The phosphor-containing flameproofing benzene-oxaxine midbody which is prepared by the method of the invention can be individually used or used by being mixed with other type benzene-oxaxine midbody or phenolic resin or epoxy resin; an obtained solidified product has higher thermal resistance, and the phosphor-containing flameproofing benzene-oxaxine midbody is applicable to the production of structural material, flameproofing material, electric insulation material, electronic encapsulation material, ablation resistance material or braking material with high capacities which are used at the temperature higher than 180 DEG C.

Description

technical field [0001] The invention belongs to the technical field of thermosetting resin preparation, and relates to a preparation method of a diamine-type phosphorus-containing highly flame-retardant benzoxazine resin. Background technique [0002] Benzoxazines are a class of six-membered heterocyclic compounds synthesized by polycondensation reactions of phenolic compounds, amine compounds and formaldehyde. They were initially discovered in the Mannich reaction, and undergo ring-opening polymerization under the action of heating or catalysts to form nitrogen-containing and similar Network structure of phenolic resin. As a new type of phenolic resin, benzoxazine resin not only has the thermal properties, mechanical properties, and electrical properties of traditional phenolic resins, but also has excellent processing properties: no small molecules are released during the forming and curing process, and the volume is close to zero shrinkage , which has aroused extensive r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C08L79/04C08K5/521
Inventor 鲁在君门薇薇张洪春王赐明孟凡君
Owner SHANDONG UNIV
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