COFs-modified ammonium polyphosphate flame retardant as well as preparation method and application thereof and flame-retardant epoxy resin

An ammonium polyphosphate and epoxy resin technology, applied in the field of flame retardants, can solve the problems of complex APP modification synthesis process, poor compatibility of epoxy resin, strong water absorption of APP, etc., and achieves broad industrial application prospects, high hydrophobicity Sexual, easy-to-use effects

Active Publication Date: 2022-02-11
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One of the purposes of the present invention is to provide a COFs modified APP flame retardant to solve the current problems of APP with strong water absorption, poor compatibility with epoxy resin, and poor flame retardant efficiency.
[0005] The second object of the present invention is to provide a preparation method of APP flame retardant modified by COFs, to solve the complex problem of the existing APP modification synthesis process

Method used

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  • COFs-modified ammonium polyphosphate flame retardant as well as preparation method and application thereof and flame-retardant epoxy resin
  • COFs-modified ammonium polyphosphate flame retardant as well as preparation method and application thereof and flame-retardant epoxy resin
  • COFs-modified ammonium polyphosphate flame retardant as well as preparation method and application thereof and flame-retardant epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Disperse 1g APP in 200mL methanol to make the concentration 5g / L, stir for 5min; Dissolve formaldehyde in 50mL of methanol to make the concentrations 4.0g / L and 3.0g / L respectively; slowly add the 1,3,5-tris(4-aminophenyl)benzyl alcohol solution into the APP dispersion, dropwise Add 2,5-divinyl terephthalaldehyde solution to the mixed solution slowly dropwise, then add 5mL of 12M acetic acid as a catalyst, continue stirring at 55°C for 1h; centrifuge, and dry in a vacuum oven at 60°C Dry for 24 hours to prepare COFs modified APP flame retardant.

Embodiment 2

[0048] Disperse 1g APP in 125mL ethanol to make the concentration 8g / L, stir for 15min; Dissolve formaldehyde in 50mL of ethanol to make the concentrations 3.0g / L and 2.0g / L respectively; slowly add the 1,3,5-tris(4-aminophenyl)phenylethanol solution into the APP dispersion, dropwise Add 2,5-divinyl terephthalaldehyde solution to the mixed solution slowly and dropwise after the addition is completed, then add 5mL of 12M acetic acid as a catalyst, continue stirring at 35°C for 48h; centrifuge, and dry in a vacuum oven at 60°C Dry for 24 hours to prepare COFs modified APP flame retardant.

Embodiment 3

[0050] Disperse 1g APP in 200mL acetonitrile to make the concentration 5g / L, stir for 30min; Dissolve formaldehyde in 50mL acetonitrile to make the concentrations 2.0g / L and 1.3g / L respectively; slowly add the 1,3,5-tris(4-aminophenyl)phenylacetonitrile solution into the APP dispersion, drop Add 2,5-divinyl terephthalaldehyde solution slowly to the mixed solution dropwise after the addition is complete, then add 5mL of 12M acetic acid as a catalyst, continue stirring at 25°C for 72h; centrifuge, and dry in a vacuum oven at 60°C Dry for 24 hours to prepare COFs modified APP flame retardant.

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Abstract

The invention provides a COFs-modified ammonium polyphosphate flame retardant, a preparation method and application thereof and flame-retardant epoxy resin. The flame retardant is of a core-shell structure with ammonium polyphosphate as a core and a COFs material as a shell, the water contact angle of the flame retardant is larger than 95 degrees, the specific surface area is larger than 5 m<2>/g, and the average pore size is smaller than 6.07 nm. Ammonium polyphosphate, p-phenylenediamine, 1,3,5-tri(4-aminophenyl)benzene and 1,3,5-tri(4-aminophenyl)benzene are used as raw materials, and a one-step method is adopted for synthesis. The flame-retardant epoxy resin is prepared by adding a COFs-modified ammonium polyphosphate flame retardant into epoxy resin. The preparation method is simple to operate and mild in condition, the obtained flame retardant has relatively high hydrophobicity and flame retardance, and a feasible treatment method is provided for the flame retardant with poor stability. The prepared flame retardant is added into the epoxy resin, so that the flame retardant effect of the obtained epoxy resin can be greatly improved, and the flame retardant has a wide industrial application prospect.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a COFs modified ammonium polyphosphate flame retardant, its preparation method, application and flame retardant epoxy resin. Background technique [0002] Epoxy resin (EP) is an important thermosetting polymer with excellent physical and chemical properties, widely used in composite material matrix, coating and other fields. However, EP has high flammability, and current researchers mainly improve the flammability of epoxy resin by adding flame retardants. Currently commonly used EP flame retardants are mainly phosphorus-based flame retardants, among which ammonium polyphosphate (APP) is a compound with both phosphorus and nitrogen, which can be used as an acid source and a gas source at the same time. Therefore, it has broad application prospects in flame retardant EP. However, the strong water absorption of APP leads to its easy precipitation from the matrix in a humid environment. In ad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/10C08K3/32C08L63/00
CPCC08K9/10C08K3/32C08L63/00C08K2003/323C08L2201/02
Inventor 孟伟华毕雪孟雅芳邸航徐建中方立德
Owner HEBEI UNIVERSITY
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