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Phthalonitrile, benzoxazine and tetraaminophthalocyanine lead-based anti-radiation composite material and preparation method

A technology of phthalonitrile and base phthalonitrile is applied in the field of phthalonitrile/benzoxazine/tetraaminophthalocyanine lead-based anti-radiation composite material and preparation thereof, and can solve the problem of low thermal performance. , High curing temperature of benzoxazine resin, low crosslinking density of cured products, etc., to achieve the effect of reducing curing temperature, improving processability, excellent heat resistance and radiation resistance

Active Publication Date: 2020-06-16
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the curing temperature of the benzoxazine resin itself is also high, and the crosslinking density of the cured product is low, and its thermal performance is far lower than that of the phthalonitrile resin.

Method used

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  • Phthalonitrile, benzoxazine and tetraaminophthalocyanine lead-based anti-radiation composite material and preparation method
  • Phthalonitrile, benzoxazine and tetraaminophthalocyanine lead-based anti-radiation composite material and preparation method
  • Phthalonitrile, benzoxazine and tetraaminophthalocyanine lead-based anti-radiation composite material and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 2-methoxy-4-allylphenoxyphthalonitrile (10g), phenol-anilinobenzoxazine (1g) and lead tetraaminophthalocyanine (0.7g) into a beaker, Slowly heat to 100°C under stirring, when the solid is completely melted, continue to stir for 20-30 minutes, add it to the preheated (about 100°C) mold while it is still hot, vacuum defoam at 100°C for 3 hours, and then place it in the air to dry Segmented curing in the box, the heating process of segmented curing is: 180°C / 2h+220°C / 4h+260°C / 4h+300°C / 2h, and finally phthalonitrile / benzoxazine / tetraaminophthalocyanine Lead-based composites. The composite sample was placed in the 60 In the Co irradiation device, the samples were taken out after 20 h, and the composite materials before and after irradiation were tested. Infrared spectra of 2-methoxy-4-allylphenoxyphthalonitrile / phenol-anilinobenzoxazine / tetraaminophthalocyanine lead-based composites before and after irradiation ( image 3 ) shows that after the sample is irradiated by...

Embodiment 2

[0026] Except that 2-methoxy-4-allylphenoxyphthalonitrile was changed to bisphenol A-based phthalonitrile, and the dosage of phenol-anilinobenzoxazine was changed from 1g to 2g, the same Example 1. The E' of the composite before and after irradiation were 2265 and 2249 MPa, T g 376 and 373°C, respectively, T 5 463 and 461°C, respectively, Y c 66.7% and 66.5%, respectively.

Embodiment 3

[0028] The amount of phenol-anilinobenzoxazine was changed from 2g to 4g, the amount of lead tetraaminophthalocyanine was changed from 0.7g to 1.5g, the melt blending temperature was changed from 100°C to 80°C, and the heating process of segmented curing was changed from 180°C Except that / 2h+220°C / 4h+260°C / 4h+300°C / 2h is changed to 170°C / 2h+210°C / 3h+250°C / 3h+280°C / 2h, the others are the same as in Example 2. The E′ of the composite before and after irradiation were 2527 and 2531 MPa, T g 348 and 351°C, respectively, T 5 443 and 447°C, respectively, Y c 70.2% and 70.5%, respectively.

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Abstract

The invention provides a phthalonitrile-benzoxazine-tetramine phthalocyanine lead based anti-radiation composite material and a preparation method thereof. The preparation method comprises the steps of carrying out melt blending on phthalonitrile, benzoxazine and tetramine phthalocyanine lead at 70-120 DEG C, uniformly mixing to obtain a mixture, putting the mixture into a preheated mold, carrying out vacuum defoaming at the temperature of 100 DEG C, and carrying out sectional curing at 160-350 DEG C for 6-20 hours, so as to obtain the phthalonitrile-benzoxazine-tetramine phthalocyanine lead based anti-radiation composite material, wherein the mass ratio of phthalonitrile to benzoxazine is 1 to (0.1-1), and the mass ratio of a blend of phthalonitrile and benzoxazine to tetramine metal phthalocyanine lead is 1 to (0.03-0.3). The composite material has excellent gamma ray irradiation resistance, and the dynamic mechanical property, thermal property and structure of a polymer are not obviously changed before and after radiation. The type of the materials can meet requirement on material properties in an extreme environment and can be used for preparing high-performance structural materials, electronic packaging materials, high-temperature-resistant adhesives, ablation-resistant materials and the like.

Description

technical field [0001] The present invention relates to a radiation protection material resistant to high-energy ray radiation, and also relates to a preparation method of a radiation protection material resistant to high-energy ray radiation, in particular to a gamma-ray radiation-resistant ophthalmic The dicyanonitrile / benzoxazine / tetraaminophthalocyanine lead-based anti-radiation composite material and its preparation method. Background technique [0002] At present, a large number of polymer materials and resin-based composite materials are used in nuclear power plants, aerospace vehicles, hospitals and other environments. These polymer materials and composite materials are easily irradiated by high-energy rays such as gamma and x-rays in the above-mentioned environments. Radiation The free radicals produced will cause reverse crosslinking and degradation of polymer materials, resulting in changes in the mechanical properties and thermal properties of polymer materials, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/04C08L61/34C08K5/00G21F1/10
CPCC08L79/04C08L2201/08G21F1/10C08L61/34C08K5/0091
Inventor 王军刘文彬马瑞坤宋莎王安然
Owner HARBIN ENG UNIV