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Preparation method of phenyl phosphonate grafted graphene-POSS (Polyhedral Oligomeric Silsesquioxane) flame-retardant polyethylene terephthalate material

A technology of polyethylene terephthalate and grafted graphite, which is applied in the field of phenyl phosphonate grafted graphene-POSS flame-retardant polyethylene terephthalate material, which can solve the problem of fire spread and easy fire And other issues

Inactive Publication Date: 2022-04-26
曹帅强
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] One of the disadvantages of glass fiber reinforced polyethylene terephthalate engineering plastics is its fire safety. The low oxygen index value of 16-20% and the large amount of smoke and molten droplets produced during combustion are very easy to burn. Start a fire and cause it to spread quickly

Method used

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  • Preparation method of phenyl phosphonate grafted graphene-POSS (Polyhedral Oligomeric Silsesquioxane) flame-retardant polyethylene terephthalate material

Examples

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Effect test

Embodiment 1

[0030] A kind of preparation method of phenyl phosphonate grafted graphene-POSS flame retardant polyethylene terephthalate material, comprises the following steps:

[0031] Step S1, the preparation of diethanolamine methyl diphenyl phosphonate:

[0032] Add 2.35g of diphenyl phosphite and 1g of diethanolamine in sequence to a 50mL three-necked flask equipped with magnetic stirring, a thermometer, and a reflux condenser, and slowly heat up to 40°C under stirring, then add 0.9g of paraformaldehyde, and continue to heat up To 85°C, stir to dissolve all the paraformaldehyde, stop the reaction after 30 minutes of reaction, and cool to room temperature;

[0033] The above liquid was dissolved in chloroform, washed several times with distilled water, the organic layer was collected and dried with anhydrous sodium sulfate, the desiccant was filtered off and the chloroform was removed by rotary evaporation to obtain diphenyl diethanolamine methylphosphonate;

[0034] Step S2, preparat...

Embodiment 2

[0041] A kind of preparation method of phenyl phosphonate grafted graphene-POSS flame retardant polyethylene terephthalate material, comprises the following steps:

[0042] Step S1, the preparation of diethanolamine methyl diphenyl phosphonate:

[0043] Add 1g of diphenyl phosphite and 0.5g of diethanolamine in sequence to a 50mL three-neck flask equipped with magnetic stirring, a thermometer, and a reflux condenser, and slowly heat up to 60°C under stirring, then add 0.5g of paraformaldehyde, and continue to heat up to 80°C, stir to dissolve all the paraformaldehyde, stop the reaction after 60 minutes of reaction, and cool to room temperature;

[0044] The above liquid was dissolved in chloroform, washed several times with distilled water, the organic layer was collected and dried with anhydrous sodium sulfate, the desiccant was filtered off and the chloroform was removed by rotary evaporation to obtain diphenyl diethanolamine methylphosphonate;

[0045] Step S2, preparation...

Embodiment 3

[0052] A kind of preparation method of phenyl phosphonate grafted graphene-POSS flame retardant polyethylene terephthalate material, comprises the following steps:

[0053] Step S1, the preparation of diethanolamine methyl diphenyl phosphonate:

[0054] Add 5g of diphenyl phosphite and 1.5g of diethanolamine in sequence in a 50mL three-necked flask equipped with a magnetic stirrer, a thermometer, and a reflux condenser, slowly heat up to 80°C under stirring, then add 2g of paraformaldehyde, and continue to heat up to Stir at 95°C to dissolve all the paraformaldehyde, stop the reaction after 40 minutes, and cool to room temperature;

[0055] The above liquid was dissolved in chloroform, washed several times with distilled water, the organic layer was collected and dried with anhydrous sodium sulfate, the desiccant was filtered off and the chloroform was removed by rotary evaporation to obtain diphenyl diethanolamine methylphosphonate;

[0056] Step S2, preparation of hydroxyl-...

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Abstract

The invention relates to the technical field of flame retardance of polyethylene terephthalate, and discloses a preparation method of a phenyl phosphonate grafted graphene-POSS (Polyhedral Oligomeric Silsesquioxane) flame-retardant polyethylene terephthalate material, which comprises the following steps: firstly, bridging an imino group of diethanol amine with a phosphorus element of diphenyl phosphite through a methylene group under the action of paraformaldehyde; the alcohol hydroxyl group end capped amine methyl diphenyl phosphonate is obtained; then, an alcoholic hydroxyl group at one end of alcoholic hydroxyl group-terminated aminomethyl diphenyl phosphonate is firstly reacted with a hydroxyl group on the graphene oxide, and then the alcoholic hydroxyl group at one end of the alcoholic hydroxyl group-terminated aminomethyl diphenyl phosphonate is reacted with a chloropropyl functional group on 3-chloropropyl POSS, so that the phenyl phosphonate grafted graphene-POSS flame retardant is obtained. The phenyl phosphonate grafted graphene-POSS flame retardant is applied to flame-retardant polyethylene terephthalate, and the beneficial technical effect of remarkably improving the flame retardant property of polyethylene terephthalate is achieved.

Description

technical field [0001] The invention relates to the technical field of flame-retardant polyethylene terephthalate, in particular to a method for preparing a phenylphosphonate-grafted graphene-POSS flame-retardant polyethylene terephthalate material. Background technique [0002] One of the disadvantages of glass fiber reinforced polyethylene terephthalate engineering plastics is its fire safety. The low oxygen index value of 16-20% and the large amount of smoke and molten droplets produced during combustion are very easy to burn. Start a fire and cause the fire to spread rapidly. [0003] At present, it has been disclosed in the literature that the synergistic effect of aluminum hypophosphite (AHP) and graphene (RGO) is applied to the flame retardant treatment of polybutylene terephthalate (PBT), and the combination of phosphorus flame retardants and POSS is synergistically applied to the flame retardant treatment of PET; [0004] The present invention quotes the following...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/02C08K9/04C08K9/06C08K3/04
CPCC08K9/04C08K9/08C08K3/042C08L2201/02C08L67/02
Inventor 曹帅强
Owner 曹帅强
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