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Preparation method of phenyl phosphine oxide synergistic graphene-POSS flame-retardant polycarbonate material

A technology of flame retardant polycarbonate and phenyl phosphine oxide, which is applied in the field of polycarbonate flame retardant and can solve the problems of unsatisfactory flame retardant effect and the like

Pending Publication Date: 2022-03-25
曹苗苗
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Although the main chain of polycarbonate contains benzene rings, it can be condensed into aromatic carbon substances during its combustion reaction, with a relatively high char formation rate and self-extinguishing, and its flame retardant grade can reach the standard of UL94V-2 , but when applied to many high-tech fields, its flame retardant effect is still not ideal.

Method used

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  • Preparation method of phenyl phosphine oxide synergistic graphene-POSS flame-retardant polycarbonate material
  • Preparation method of phenyl phosphine oxide synergistic graphene-POSS flame-retardant polycarbonate material

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Effect test

Embodiment 1

[0035] A kind of preparation method of phenylphosphine oxide cooperative graphene-POSS flame-retardant polycarbonate material, comprises the following steps:

[0036] Step S1, preparation of amino-terminated imidized graphene:

[0037] Place 0.1 g of graphene in 120 mL of H 2 SO 4 and HNO 3 (volume ratio 3: 1), ultrasonication at room temperature for 4h, filtered after dilution, washed with distilled water to neutrality, and vacuum-dried to obtain carboxylated graphene;

[0038] The carboxylated graphene is placed in a flask filled with 3g of 3,3'-diaminodipropylamine, ultrasonicated for 30min at room temperature, and 0.1g of N,N'-dicyclohexylcarbodiimide is added, mixed uniformly, Reflux in an oil bath at 110°C for 48 hours, and the product is ultrasonically removed with absolute ethanol to remove the remaining N,N'-dicyclohexylcarbodiimide and 3,3'-diaminodipropylamine, and the final product is washed several times with distilled water , after drying, obtain amino-termin...

Embodiment 2

[0048] A kind of preparation method of phenylphosphine oxide cooperative graphene-POSS flame-retardant polycarbonate material, comprises the following steps:

[0049] Step S1, preparation of amino-terminated imidized graphene:

[0050] 0.12 g of graphene was placed in 120 mL of H 2 SO 4 and HNO 3(volume ratio 3: 1), ultrasonication at room temperature for 5h, filtered after dilution, washed with distilled water to neutrality, and vacuum-dried to obtain carboxylated graphene;

[0051] The carboxylated graphene is placed in a flask filled with 5g of 3,3'-diaminodipropylamine, ultrasonicated for 60min at room temperature, and 0.12g of N,N'-dicyclohexylcarbodiimide is added, mixed uniformly, Reflux in an oil bath at 150°C for 36 hours, and the product is ultrasonically removed with absolute ethanol to remove the remaining N,N'-dicyclohexylcarbodiimide and 3,3'-diaminodipropylamine, and the final product is washed several times with distilled water , after drying, obtain amino-...

Embodiment 3

[0061] A kind of preparation method of phenylphosphine oxide cooperative graphene-POSS flame-retardant polycarbonate material, comprises the following steps:

[0062] Step S1, preparation of amino-terminated imidized graphene:

[0063] 0.05 g of graphene was placed in 120 mL of H 2 SO 4 and HNO 3 (volume ratio 3: 1), ultrasonication at room temperature for 2h, filtered after dilution, washed with distilled water to neutrality, and vacuum-dried to obtain carboxylated graphene;

[0064] The carboxylated graphene is placed in a flask filled with 1g of 3,3'-diaminodipropylamine, ultrasonicated at room temperature for 20min, and 0.05g of N,N'-dicyclohexylcarbodiimide is added, mixed uniformly, Reflux in an oil bath at 130°C for 40 hours, and the product is ultrasonicated with absolute ethanol to remove the remaining N,N'-dicyclohexylcarbodiimide and 3,3'-diaminodipropylamine, and the final product is washed several times with distilled water , after drying, obtain amino-termina...

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Abstract

The invention relates to the technical field of flame retardance of polycarbonate, and discloses a preparation method of a phenylphosphine oxide synergistic graphene-POSS (Polyhedral Oligomeric Silsesquioxane) flame-retardant polycarbonate material, which comprises the following steps: firstly, carrying out amino-terminated imidization modification on graphene; then carrying out epoxy ring-opening reaction on a single epoxy group on the POSS and an amino-terminated group on the graphene to generate imidization graphene-POSS; then carrying out a reaction on an alcoholic hydroxyl group on 6-chloro-1-hexanol and a chlorine functional group of diphenyl phosphinyl chloride to generate chlorine-terminated diphenyl phosphine oxide; finally, grafting of the phenyl phosphine oxide and the graphene-POSS is achieved through a chlorine functional group on the chlorine-terminated diphenyl phosphine oxide and an imine group on the imidization graphene-POSS, so that the phenyl phosphine oxide synergistic graphene-POSS flame retardant is prepared, and the phenyl phosphine oxide synergistic graphene-POSS flame retardant is applied to flame-retardant polycarbonate, so that the flame-retardant performance of the flame-retardant polycarbonate is improved, and the flame-retardant performance of the flame-retardant polycarbonate is improved. The effective technical effect of remarkably improving the flame retardant property is achieved.

Description

technical field [0001] The invention relates to the technical field of polycarbonate flame retardancy, in particular to a method for preparing a phenylphosphine oxide synergistic graphene-POSS flame-retardant polycarbonate material. Background technique [0002] Although the main chain of polycarbonate contains benzene rings, it can be condensed into aromatic carbon substances during its combustion reaction, with a relatively high char formation rate and self-extinguishing, and its flame retardant grade can reach the standard of UL94V-2 , but when applied to many high-tech fields, its flame retardant effect is still not ideal. [0003] At present, the research on the flame retardancy of polycarbonate by the silicon-containing flame retardant POSS has been disclosed in the literature, and the literature also discloses that graphene and organophosphorus compounds can be applied to flame-retardant organic polymer materials. [0004] The following references are cited in the pr...

Claims

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Application Information

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IPC IPC(8): C08L69/00C08L87/00C08K5/5397C08G83/00
CPCC08L69/00C08G83/001C08L2201/02C08L87/005C08K5/5397Y02E60/10
Inventor 曹苗苗
Owner 曹苗苗
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