CN106243618A - A kind of high temperature creep-resisting Graphene modified phenolic foam material and preparation method thereof - Google Patents
A kind of high temperature creep-resisting Graphene modified phenolic foam material and preparation method thereof Download PDFInfo
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- CN106243618A CN106243618A CN201610667220.9A CN201610667220A CN106243618A CN 106243618 A CN106243618 A CN 106243618A CN 201610667220 A CN201610667220 A CN 201610667220A CN 106243618 A CN106243618 A CN 106243618A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08L61/14—Modified phenol-aldehyde condensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/143—Halogen containing compounds
- C08J9/147—Halogen containing compounds containing carbon and halogen atoms only
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
- C08J2203/142—Halogenated saturated hydrocarbons, e.g. H3C-CF3
- C08J2203/144—Perhalogenated saturated hydrocarbons, e.g. F3C-CF3
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08J2361/14—Modified phenol-aldehyde condensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a kind of high temperature creep-resisting Graphene modified phenolic foam material and preparation method thereof, it is formed by the preparation of raw material of following weight portion: phenolic resin 90 100, Graphene 0.5 0.9, phosphoric acid 23, poly-isocyanurate 18 20, Polysorbate 8 10, dichlorotetra-fluoroethane 12 14, isophorone diamine 67, dichloromethyl triethoxysilane 58, diacetyl peroxidase 12 4, calcium stearate 57, tributyl 2-acetylcitrate 35, Propylgallate 79, basic magnesium carbonate 10 12 etc..The present invention uses Graphene phenol-formaldehyde resin modified, the ester bond making the carboxyl around Graphene and the hydroxyl reaction in phenolic resin generate is fixed on phenolic resin, reduce the fragility of foam, the characteristic that Graphene is intrinsic simultaneously enhances the heat absorption capacity of foamed materials, prevent it from occurring high-temerature creep, the basic magnesium carbonate of interpolation and aluminium hydroxide to make foamed materials have good anti-flammability.
Description
Technical field
The present invention relates to a kind of foamed materials, concretely relate to a kind of high temperature creep-resisting Graphene modified phenolic foam
Material and preparation method thereof.
Background technology
Polymer foams, also known as porous material, is that a class is formed in hard resin by a large amount of gas micropore dispersions
Macromolecular material, this kind of material also can be considered with polymer as matrix, the gas composite as filler.Bubble and resin base
The compound of body imparts a series of excellent property such as this kind of density of material is low, specific strength is high, heat-proof quality is excellent, soundproof effect is good
Energy.Most of thermoplastic polymers and thermosetting polymer can be processed into foam of polymers, thus polymer foams
Huge number.Common foamed materials have polystyrene (PS) foam, polyurethane (PU) foam, polrvinyl chloride (PVC) foam,
Phenolic aldehyde (PF) foam, epoxy foams, expanded polyolefin, nitrile rubber foam, thermoplastic elastomer (TPE) foam etc..They are in day
Change the industries such as articles for use, transportation, electronic apparatus, packaging material and weaving to have a wide range of applications.
Phenolic resin has had time of upper a century as the resin of the first industrialized production from coming out.This
Kind resin is simple with its synthesis technique, Stability Analysis of Structures, good mechanical performance, fire protecting performance excellent and is widely used in building, ship
The field such as oceangoing ship, traffic.It is a series of excellent that the phenol formaldehyde foam that Foaming of phenolic resin prepares has processing technique simple, difficult combustion, low cigarette etc.
Point.Owing to insulation material fire protection requirement for building is improved constantly by country in recent years, phenol formaldehyde foam is most possible as it
Substitution material is taken seriously gradually in building material field.Phenol formaldehyde foam is when as wall heat insulation material, due to for a long time
Irradiated by sunlight, its temperature can be made to raise and cause thermal expansion phenomenon, cause body of wall to come off, it is therefore desirable to phenol formaldehyde foam has
There is good Properties of High Temperature Creep.
Summary of the invention
It is an object of the invention to provide a kind of high temperature creep-resisting Graphene modified phenolic foam material and preparation method thereof.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
A kind of high temperature creep-resisting Graphene modified phenolic foam material, is formed by the preparation of raw material of following weight portion: phenolic resin
90-100, Graphene 0.5-0.9, phosphoric acid 2-3, poly-isocyanurate 18-20, Polysorbate 8-10, dichlorotetra-fluoroethane 12-
14, isophorone diamine 6-7, dichloromethyl triethoxysilane 5-8, diacetyl peroxidase 12-4, calcium stearate 5-7, acetyl
Tributyl citrate 3-5, Propylgallate 7-9, basic magnesium carbonate 10-12, zirconium English powder 24-30, asbestos wool 7-9, hydroxide
Aluminum 6-8, Pulvis Talci 5-7, white carbon 4-6, calcined kaolin 8-10, water 20-25.
The preparation method of a kind of high temperature creep-resisting Graphene modified phenolic foam material, comprises the following steps:
(1) phenolic resin, Graphene, phosphoric acid mixing are poured into stirring 20-25min in agitator and be allowed to mix homogeneously, then add
Heat, to 175-180 DEG C, is incubated 50-60min, obtains Graphene phenol-formaldehyde resin modified；
(2) basic magnesium carbonate, zirconium English powder, asbestos wool, aluminium hydroxide, Pulvis Talci, white carbon, calcined kaolin are together put into ball
Fine grinding in grinding machine, the Task-size Controlling of mixture mixture siccative after 1-2mm, fine grinding is put in mixing plant, and is added
The water of half is sufficiently stirred for, and obtains mixed slurry；
(3) Graphene phenol-formaldehyde resin modified and mixed slurry are added the 3-that begins to pratise at a temperature of 100-110 DEG C in mill
5min, is subsequently adding poly-isocyanurate, Polysorbate, dichlorotetra-fluoroethane, isophorone diamine, dichloromethyl triethoxy
Raw material and the remaining water such as silane, diacetyl peroxide, calcium stearate, tributyl 2-acetylcitrate, Propylgallate,
At a temperature of 90-100 DEG C, continue mill 5-8min, obtain compound；
(4) inject a mixture in foaming mould foamable reaction 40-60min in the environment of 60-80 DEG C, obtain described phenolic aldehyde bubble
Foam material.
Beneficial effects of the present invention:
The present invention uses Graphene phenol-formaldehyde resin modified, makes the carboxyl around Graphene generate with the hydroxyl reaction in phenolic resin
Ester bond be fixed on phenolic resin, reduce foam fragility, the characteristic that Graphene is intrinsic simultaneously enhances foam material
The heat absorption capacity of material, prevents it from occurring high-temerature creep, the basic magnesium carbonate of interpolation and aluminium hydroxide to make foamed materials have very well
Anti-flammability.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1:
A kind of high temperature creep-resisting Graphene modified phenolic foam material, is formed by the preparation of raw material of following weight portion (kg): phenolic aldehyde
Resin 90, Graphene 0.5, phosphoric acid 2, poly-isocyanurate 18, Polysorbate 8, dichlorotetra-fluoroethane 12, isophorone diamine 6,
Dichloromethyl triethoxysilane 5, diacetyl peroxidase 12, calcium stearate 5, tributyl 2-acetylcitrate 3, gallic acid third
Ester 7, basic magnesium carbonate 10, zirconium English powder 24, asbestos wool 7, aluminium hydroxide 6, Pulvis Talci 5, white carbon 4, calcined kaolin 8, water 20.
The preparation method of a kind of high temperature creep-resisting Graphene modified phenolic foam material, comprises the following steps:
(1) phenolic resin, Graphene, phosphoric acid mixing are poured into stirring 20-25min in agitator and be allowed to mix homogeneously, then add
Heat, to 175-180 DEG C, is incubated 50-60min, obtains Graphene phenol-formaldehyde resin modified；
(2) basic magnesium carbonate, zirconium English powder, asbestos wool, aluminium hydroxide, Pulvis Talci, white carbon, calcined kaolin are together put into ball
Fine grinding in grinding machine, the Task-size Controlling of mixture mixture siccative after 1-2mm, fine grinding is put in mixing plant, and is added
The water of half is sufficiently stirred for, and obtains mixed slurry；
(3) Graphene phenol-formaldehyde resin modified and mixed slurry are added the 3-that begins to pratise at a temperature of 100-110 DEG C in mill
5min, is subsequently adding poly-isocyanurate, Polysorbate, dichlorotetra-fluoroethane, isophorone diamine, dichloromethyl triethoxy
Raw material and the remaining water such as silane, diacetyl peroxide, calcium stearate, tributyl 2-acetylcitrate, Propylgallate,
At a temperature of 90-100 DEG C, continue mill 5-8min, obtain compound；
(4) inject a mixture in foaming mould foamable reaction 40-60min in the environment of 60-80 DEG C, obtain described phenolic aldehyde bubble
Foam material.
Embodiment 2:
A kind of high temperature creep-resisting Graphene modified phenolic foam material, is formed by the preparation of raw material of following weight portion (kg): phenolic aldehyde
Resin 95, Graphene 0.7, phosphoric acid 2.5, poly-isocyanurate 19, Polysorbate 9, dichlorotetra-fluoroethane 13, isophorone diamine
6.5, dichloromethyl triethoxysilane 6.5, diacetyl peroxide 3, calcium stearate 6, tributyl 2-acetylcitrate 4, five times
Sub-propyl propionate 8, basic magnesium carbonate 11, zirconium English powder 27, asbestos wool 8, aluminium hydroxide 7, Pulvis Talci 6, white carbon 5, calcined kaolin
9, water 22.5.
Preparation method is with embodiment 1.
Embodiment 3:
A kind of high temperature creep-resisting Graphene modified phenolic foam material, is formed by the preparation of raw material of following weight portion (kg): phenolic aldehyde
Resin 100, Graphene 0.9, phosphoric acid 3, poly-isocyanurate 20, Polysorbate 10, dichlorotetra-fluoroethane 14, isophorone diamine
7, dichloromethyl triethoxysilane 8, diacetyl peroxide 4, calcium stearate 7, tributyl 2-acetylcitrate 5, gallic acid
Propyl ester 9, basic magnesium carbonate 12, zirconium English powder 30, asbestos wool 9, aluminium hydroxide 8, Pulvis Talci 7, white carbon 6, calcined kaolin 10, water
25。
Preparation method is with embodiment 1.
The performance test results of the phenolic foam material that above-described embodiment 1-3 prepares is as shown in the table:
The performance test results of the phenolic foam material that table 1 embodiment 1-3 prepares
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Heat distortion temperature, DEG C | 245 | 258 | 253 |
| Rate of weight loss, % | 4.75 | 5.16 | 4.53 |
| Bending strength, MPa | 55 | 58 | 53 |
| Bending modulus, MPa | 475 | 416 | 453 |
Claims (2)
1. a high temperature creep-resisting Graphene modified phenolic foam material, it is characterised in that by the preparation of raw material of following weight portion
Form: phenolic resin 90-100, Graphene 0.5-0.9, phosphoric acid 2-3, poly-isocyanurate 18-20, Polysorbate 8-10, dichloro
Tetrafluoroethane 12-14, isophorone diamine 6-7, dichloromethyl triethoxysilane 5-8, diacetyl peroxidase 12-4, tristearin
Acid calcium 5-7, tributyl 2-acetylcitrate 3-5, Propylgallate 7-9, basic magnesium carbonate 10-12, zirconium English powder 24-30, asbestos
Floss 7-9, aluminium hydroxide 6-8, Pulvis Talci 5-7, white carbon 4-6, calcined kaolin 8-10, water 20-25.
The preparation method of a kind of high temperature creep-resisting Graphene modified phenolic foam material the most according to claim 1, it is special
Levy and be, comprise the following steps:
(1) phenolic resin, Graphene, phosphoric acid mixing are poured into stirring 20-25min in agitator and be allowed to mix homogeneously, then add
Heat, to 175-180 DEG C, is incubated 50-60min, obtains Graphene phenol-formaldehyde resin modified；
(2) basic magnesium carbonate, zirconium English powder, asbestos wool, aluminium hydroxide, Pulvis Talci, white carbon, calcined kaolin are together put into ball
Fine grinding in grinding machine, the Task-size Controlling of mixture mixture siccative after 1-2mm, fine grinding is put in mixing plant, and is added
The water of half is sufficiently stirred for, and obtains mixed slurry；
(3) Graphene phenol-formaldehyde resin modified and mixed slurry are added the 3-that begins to pratise at a temperature of 100-110 DEG C in mill
5min, is subsequently adding poly-isocyanurate, Polysorbate, dichlorotetra-fluoroethane, isophorone diamine, dichloromethyl triethoxy
Raw material and the remaining water such as silane, diacetyl peroxide, calcium stearate, tributyl 2-acetylcitrate, Propylgallate,
At a temperature of 90-100 DEG C, continue mill 5-8min, obtain compound；
(4) inject a mixture in foaming mould foamable reaction 40-60min in the environment of 60-80 DEG C, obtain described phenolic aldehyde bubble
Foam material.
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| CN201610667220.9A CN106243618A (en) | 2016-08-15 | 2016-08-15 | A kind of high temperature creep-resisting Graphene modified phenolic foam material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107955325A (en) * | 2017-12-02 | 2018-04-24 | 范运昌 | A kind of processing method for reducing phenolic foam board thermal conductivity factor |
| CN108822488A (en) * | 2018-05-29 | 2018-11-16 | 中建深业建设发展有限公司 | Fibre-reinforced environmentally friendly phenolic aldehyde thermal insulation material of raw bamboo and preparation method thereof |
| CN112454955A (en) * | 2020-10-30 | 2021-03-09 | 陕西科技大学 | Wear-resistant flame-retardant TPU sole and one-step forming method thereof |
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| CN108822488A (en) * | 2018-05-29 | 2018-11-16 | 中建深业建设发展有限公司 | Fibre-reinforced environmentally friendly phenolic aldehyde thermal insulation material of raw bamboo and preparation method thereof |
| CN112454955A (en) * | 2020-10-30 | 2021-03-09 | 陕西科技大学 | Wear-resistant flame-retardant TPU sole and one-step forming method thereof |
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Application publication date: 20161221 |