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Preparation method for nitrogen-phosphorus-silicon modified graphene/self-repaired polyurethane flame-retardant composite material

A flame retardant composite material and graphene technology, applied in the field of intelligent coating and packaging, can solve the problems of unreported research on functionalized graphene/polyurethane composite materials, no flame retardant function, general flame retardant efficiency, etc. Excellent flame retardant and self-healing function, easy operation, environment-friendly effect

Inactive Publication Date: 2019-05-10
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patent (CN108299653A) discloses a phosphorus-nitrogen flame retardant functionalized graphene and its preparation method, which is composed of branched polyethyleneimine (BPEI) and 9,10-dihydro- 9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) modified graphene oxide, the prepared functionalized graphene has flame retardant effect, and has a strong molecular chain with polycaprolactone (PLA) affinity, but the invention only uses polymers containing nitrogen and phosphorus to modify graphene oxide, the flame retardant efficiency is average, and it has not been practically applied to polymer matrix materials, especially polymer materials with intelligent responsiveness
Chinese patent (CN106117486A) discloses a dihydric alcohol containing an acylhydrazone bond, a dihydric alcohol containing an acylhydrazone bond and a disulfide bond, a self-healing polyurethane elastomer and a preparation method thereof. It is prepared from polyhydric alcohol or dihydric alcohol containing acylhydrazone bond and disulfide bond and polyurethane prepolymer. It has self-healing function, but it does not have flame retardant function and has potential safety hazards.
[0006] So far, there have been no reports on the research on functionalized graphene / polyurethane composites in terms of flame retardancy and self-healing at home and abroad.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: Disperse 500 g of graphene oxide in deionized water (1 mg / mL) in a single-necked flask, slowly add 1 g of polyethyleneimine (M n ≈600), nitrogen protection, reaction at room temperature for 24 h, centrifugation, and drying to obtain nitrogen-modified graphene; disperse 250 mg nitrogen-modified graphene in butanone (3 mg / mL), add 1.08 g of 9,10-dihydro -9-oxa-10-phosphaphenanthrene-10-oxide, 0.53 g triethylamine and 0.77 g carbon tetrachloride, under nitrogen protection, reacted at room temperature for 24 h, centrifuged and dried to obtain nitrogen-phosphorus-modified graphene; 200 1 g of nitrogen-phosphorus-modified graphene was dispersed in methyl ethyl ketone (3 mg / mL), 2 g of isocyanate-propyltrimethoxysilane was added, under nitrogen protection, and reacted at 80 °C for 24 h. After centrifugation, nitrogen-phosphorus-silicon-modified graphene was obtained. spare. 10 g polytetrahydrofuran diol (M n=1000) was placed in a three-necked flask equipped with a...

Embodiment 2

[0017] Example 2: Disperse 500 g of graphene oxide in deionized water (1 mg / mL) in a single-necked flask, and slowly add 1 g of polyethyleneimine (M n ≈600), nitrogen protection, reaction at room temperature for 24 h, centrifugation, and drying to obtain nitrogen-modified graphene; disperse 250 mg nitrogen-modified graphene in butanone (3 mg / mL), add 1.08 g of 9,10-dihydro -9-oxa-10-phosphaphenanthrene-10-oxide, 0.53 g triethylamine and 0.77 g carbon tetrachloride, under nitrogen protection, reacted at room temperature for 24 h, centrifuged and dried to obtain nitrogen-phosphorus-modified graphene; 200 1 g of nitrogen-phosphorus-modified graphene was dispersed in methyl ethyl ketone (3 mg / mL), 2 g of isocyanate-propyltrimethoxysilane was added, under nitrogen protection, and reacted at 80 °C for 24 h. After centrifugation, nitrogen-phosphorus-silicon-modified graphene was obtained. spare. 10 g polytetrahydrofuran diol (M n =1000) placed in a three-necked flask equipped with ...

Embodiment 3

[0018] Example 3: Disperse 500 g of graphene oxide in deionized water (1 mg / mL) in a single-necked flask, and slowly add 1 g of polyethyleneimine (M n ≈600), nitrogen protection, reaction at room temperature for 24 h, centrifugation, and drying to obtain nitrogen-modified graphene; disperse 250 mg nitrogen-modified graphene in butanone (3 mg / mL), add 1.08 g of 9,10-dihydro -9-oxa-10-phosphaphenanthrene-10-oxide, 0.53 g triethylamine and 0.77 g carbon tetrachloride, under nitrogen protection, reacted at room temperature for 24 h, centrifuged and dried to obtain nitrogen-phosphorus-modified graphene; 200 1 g of nitrogen-phosphorus-modified graphene was dispersed in methyl ethyl ketone (3 mg / mL), 2 g of isocyanate-propyltrimethoxysilane was added, under nitrogen protection, and reacted at 80 °C for 24 h. After centrifugation, nitrogen-phosphorus-silicon-modified graphene was obtained. spare. 10 g polytetrahydrofuran diol (M n =1000) placed in a three-necked flask equipped with ...

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PUM

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Abstract

The invention discloses a preparation method for a nitrogen-phosphorus-silicon modified graphene / self-repaired polyurethane flame-retardant composite material. The composite material is prepared by nitrogen-phosphorus-silicon modified functional graphene and a self-repaired polyurethane precursor containing double-selenium through suspension polymerization, wherein the functional graphene is obtained by covalent modification of oxidized graphene with polyethyleneimine, a phosphorated flame retardant and isocyanate silane. The composite material is capable of synergistically developing functions of the graphene and nitrogen-phosphorus-silicon-containing polymers on the surface thereof, and a polyurethane material is endowed with good fire resistance. At the same time, a polyurethane main chain contains a dynamic double-selenium bond, so damage, such as a broke section and a scratch, of the material can be repaired under visible light. The provided preparation method is simple and convenient in operation, and environment-friendly. The prepared composite material has good flame retardant and self-repaired functions, and can be applied to the fields of an intelligent coating and package and the like.

Description

technical field [0001] The invention relates to the field of intelligent coating and packaging, in particular to the preparation of a nitrogen-phosphorus-silicon-modified graphene / self-repairing polyurethane flame-retardant composite material. Background technique [0002] Polyurethane materials are low in cost, easy to process, and have excellent performance, and are widely used in smart materials, optical materials, biomedical materials, and other fields (Angewandte Chemie International Edition, 2013, 52(36): 9422-9441). Due to the nature of the material itself, microcracks and aging are prone to damage during processing and use, which greatly limits the safety and practicability of the material (Polymer, 2015, 69: 369-383). Therefore, how to prolong the service life of polyurethane materials so that their own functions can be fully exerted has become a research hotspot in the field of material science. As a relatively new field, self-healing materials can be divided into...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L75/08C08K9/06C08K9/08C08K9/04C08K3/04
Inventor 金勇杜卫宁金泓宇
Owner SICHUAN UNIV