Functionalized graphene and its preparation method and its flame-retardant crosslinked polyurethane rigid foam

A technology of rigid foam and graphene, which is applied in the field of rigid polyurethane foam, can solve the problems of decreased dimensional stability and foam strength, and achieve the effects of increasing dimensional stability, increasing cross-linking degree, and uniform dispersion

Active Publication Date: 2018-12-07
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As we all know, the purpose of reducing the density of foam plastics is to achieve the advantages of reducing the use of raw materials, reducing transportation costs, and reducing construction costs brought about by light weight. Polyurethane rigid foam is also prone to decrease in dimensional stability

Method used

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  • Functionalized graphene and its preparation method and its flame-retardant crosslinked polyurethane rigid foam
  • Functionalized graphene and its preparation method and its flame-retardant crosslinked polyurethane rigid foam
  • Functionalized graphene and its preparation method and its flame-retardant crosslinked polyurethane rigid foam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Hummer method to prepare graphene

[0045] Put 10g of expanded graphite, 5g of nitric acid and 230ml of sulfuric acid into a three-necked flask, slowly add 30g of potassium permanganate under mechanical stirring in an ice bath, keep the temperature not exceeding 9°C, remove the water bath, react at 35°C for 4 hours, and dissolve the reactant in 460ml of water Slowly dilute, the temperature rises to about 98°C and keeps for 1h. After continuing to dilute with 1400ml of water, treat the reactant with 3% hydrogen peroxide until bright yellow, filter with suction, wash, reduce with 50ml of hydrazine hydrate, filter with suction, wash and dry.

[0046] (2) Preparation of grafts

[0047]

[0048] Put 30.6g of phosphorus oxychloride in a three-necked flask, and slowly drop in 6.4g of methanol within 30 minutes. The temperature was raised slowly to 50°C, and the chloroform was distilled off after 4 hours of reaction. The temperature was raised until the solution boile...

Embodiment 2

[0059] (1) Hummer method to prepare graphene

[0060]Put 10g of expanded graphite, 5g of nitric acid and 230ml of sulfuric acid into a three-necked flask, slowly add 30g of potassium permanganate under mechanical stirring in an ice bath, keep the temperature not exceeding 9°C, remove the water bath, react at 35°C for 4 hours, and dissolve the reactant in 460ml of water Slowly dilute, the temperature rises to about 98°C and keeps for 1h. After continuing to dilute with 1400ml of water, treat the reactant with 3% hydrogen peroxide until bright yellow, filter with suction, wash, reduce with 50ml of hydrazine hydrate, filter with suction, wash and dry.

[0061] (2) Preparation of grafts

[0062]

[0063] Put 19.4g of phenylphosphoryl dichloride in a three-necked flask, dilute and dissolve 7.4g of glycidyl alcohol with 150ml of acetone under ice bath, and then slowly add it dropwise within 2h. After the dropwise addition, slowly raise the temperature and reflux for 3h.

[0064...

Embodiment 3

[0070] (1) Hummer method to prepare graphene

[0071] Put 10g of expanded graphite, 5g of nitric acid and 230ml of sulfuric acid into a three-necked flask, slowly add 30g of potassium permanganate under mechanical stirring in an ice bath, keep the temperature not exceeding 9°C, remove the water bath, react at 35°C for 4 hours, and dissolve the reactant in 460ml of water Slowly dilute, the temperature rises to about 98°C and keeps for 1h. After continuing to dilute with 1400ml of water, treat the reactant with 3% hydrogen peroxide until bright yellow, filter with suction, wash, reduce with 50ml of hydrazine hydrate, filter with suction, wash and dry.

[0072] (2) Preparation of grafts

[0073]

[0074] Put 25.0g of pyrophosphate chloride in a three-necked flask, dilute and dissolve 7.4g of glycidol with 150ml of acetone, and then slowly add it dropwise in 2 hours under an ice-water bath. After the dropwise addition, slowly raise the temperature and reflux for 5 hours.

[0...

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Abstract

The invention discloses functionalized graphene. A general structural formula of the functionalized graphene is represented in the specification, wherein X is an epoxy group, Y is graphene, Z is any one of alkyl groups of C1-C6, and the functionalized graphene is prepared by grafting graphene oxide onto a product obtained through reaction of a phosphorus and chlorine compound, epoxy structure containing monomers and phenol monomers in an environment without water. After the functionalized graphene is added to rigid polyurethane foam, the functionalized graphene as an intrinsic type flame retardant can better perform functions on the basis of good dispersibility, flame retardancy and compressibility of the rigid polyurethane foam are greatly improved, the density and the heat insulating performance of the rigid polyurethane foam can be equivalent to those of common rigid polyurethane foam, besides, a preparation technology of the functionalized graphene and the rigid polyurethane foam is simple and easy, and large-scale popularization and application can be performed conveniently.

Description

technical field [0001] The invention belongs to the technical field of graphene and its preparation and its flame-retardant polyurethane rigid foam, in particular to a functionalized graphene with high flame-retardant efficiency and its preparation method and its flame-retardant cross-linked polyurethane rigid foam. quality foam. Background technique [0002] Due to the advantages of extremely low thermal conductivity, low density, high specific strength value and good bonding performance, rigid polyurethane foam is welcomed by refrigeration equipment and construction industries that have strict requirements on thermal insulation performance. Its demand is increasing year by year and its The field of application is also expanding. However, polyurethane rigid foam still faces the following problems in practical application: [0003] High flame retardancy of polyurethane rigid foam. Due to the influence of structural factors, polyurethane has low decomposition temperature a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/04C08K3/04C08G18/48C08J9/08
CPCC08G18/4804C08K3/04C08K9/04C08G2110/0025C08G2110/005C08G2110/0058C08G2110/0075C08G2110/0083
Inventor 王玉忠曹志杰廖望杨君驰商珂王水秀
Owner SICHUAN UNIV
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