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Preparation method of phenolphthalein allyl amine-type benzoxazine/polyurethane blend resin

A technology of phenolphthalein allylamine type and benzoxazine, which is applied in the field of preparation of new modified resins, can solve the problem of low decomposition temperature of mixed resin, insufficient crosslinking density of bisphenol A aniline type benzoxazine resin, bisphenol Problems such as poor thermal stability of type A resin, to achieve the effect of increasing crosslinking density, excellent flame retardancy and mechanical properties, and improving heat resistance

Inactive Publication Date: 2015-01-14
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the insufficient crosslinking density of the bisphenol A aniline benzoxazine resin used, and the poor thermal stability of the structure of the bisphenol A resin, the decomposition temperature of the mixed resin is relatively low, about 200°C

Method used

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  • Preparation method of phenolphthalein allyl amine-type benzoxazine/polyurethane blend resin
  • Preparation method of phenolphthalein allyl amine-type benzoxazine/polyurethane blend resin
  • Preparation method of phenolphthalein allyl amine-type benzoxazine/polyurethane blend resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033]1. Under the condition of ice bath, add 3.00g (0.1mol) paraformaldehyde and 3.75ml (0.05mol) allylamine to a 250mL three-necked flask equipped with a condenser tube and a stirring rod, and add 150ml of absolute ethanol as a solvent. After stirring for 2 hours, 7.96g (0.025mol) of phenolphthalein was added, and the temperature was raised to reflux temperature of 80°C for 8 hours to complete the reaction. The solvent was removed by rotary evaporating the reaction liquid, dried in vacuo for 3 h, the crude product after vacuum drying was dissolved in chloroform, and 2mol·L -1 The above solution is washed with NaOH, and then washed with distilled water, and then the washed solution is rotated to remove the solvent, and finally vacuum-dried to obtain the phenolphthalein allylamine-type benzoxazine.

[0034] 2. To have N 2 Add 20g (0.02mol) PPG-1000 and 50ml of solvent acetone to the protected four-necked flask, then add 8.84g (0.04mol) diisocyanate dropwise to the four-necke...

Embodiment 2

[0038] 1. Under ice bath conditions, add 6.00g (0.1mol) paraformaldehyde and 7.5ml (0.05mol) allylamine to a 250mL three-neck flask equipped with a condenser tube and a stirring rod, and add 150ml of absolute ethanol as a solvent. After stirring for 2 hours, 15.92 g (0.025 mol) of phenolphthalein was added, and the temperature was raised to reflux temperature of 80°C for 8 hours to complete the reaction. The solvent was removed by rotary evaporating the reaction liquid, dried in vacuo for 3 h, the crude product after vacuum drying was dissolved in chloroform, and 2mol·L -1 The above solution is washed with NaOH, and then washed with distilled water, and then the washed solution is rotated to remove the solvent, and finally vacuum-dried to obtain the phenolphthalein allylamine-type benzoxazine.

[0039] 2. Step 2 of this embodiment is the same as that of Embodiment 1, and a polyurethane prepolymer is prepared.

[0040] 3, the 1.8g phenolphthalein allylamine type benzoxazine p...

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Abstract

The invention discloses a preparation method of phenolphthalein allyl amine-type benzoxazine / polyurethane blend resin. The preparation method comprises the following steps of: synthesising phenolphthalein allyl amine-type benzoxazine by virtue of a solvent method at first, and then synthesising the polyurethane prepolymer of phenol-blocked-NCO; dissolving the phenolphthalein allyl amine-type benzoxazine and the polyurethane prepolymer of phenol-blocked-NCO in acetone; adequately stirring to uniformly disperse the phenolphthalein allyl amine-type benzoxazine and the polyurethane prepolymer of phenol-blocked-NCO; performing vacuum drying treatment; and then performing program curing to obtain the blend resin. According to the preparation method, the brittleness of benzoxazine is improved by virtue of the good low temperature flexibility and processability of the polyurethane prepolymer, thus improving the processability of benzoxazine; and moreover, polyurethane can form a cross-linked network shape with benzoxazine during curing, thus increasing the cross-linking degree of benzoxazine, and then improving the thermodynamic property of benzoxazine to a certain extent.

Description

1. Technical field [0001] The invention relates to the preparation of a novel modified resin, in particular to a preparation method of a phenolphthalein allylamine type benzoxazine / polyurethane blended resin. 2. Background technology [0002] Benzoxazine resin is a new type of thermosetting resin, which is generally synthesized from phenol, amine and paraformaldehyde. It is a six-membered heterocyclic ring system composed of oxygen and nitrogen atoms. It was originally developed by Holly and Cope in the study of Mannich reaction. Find. Benzoxazine resin has the following characteristics: (1) The melt viscosity is relatively low, and the molding process is convenient; (2) No small molecules are released during polymerization, and the porosity of the product is low; (3) The shrinkage is small during polymerization, Approximate zero shrinkage, the precision of the product can be guaranteed; (4) No strong acid is needed as a catalyst during curing; (5) The polymer has excellent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08L79/04C08L75/08C08G73/06C08G18/48
Inventor 史铁钧王启东吴竞张方
Owner HEFEI UNIV OF TECH
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