CN109762301A - A kind of preparation method of polymer graphite alkene modified epoxy - Google Patents
A kind of preparation method of polymer graphite alkene modified epoxy Download PDFInfo
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- CN109762301A CN109762301A CN201811617360.0A CN201811617360A CN109762301A CN 109762301 A CN109762301 A CN 109762301A CN 201811617360 A CN201811617360 A CN 201811617360A CN 109762301 A CN109762301 A CN 109762301A
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Abstract
The invention discloses a kind of preparation methods of polymer graphite alkene modified epoxy, belong to Epoxy Resin Technology field, by weight including following component: graphene 5-10, epoxy resin 60-80, polyacrylic acid N-butyl 15-20, phthalic anhydride 5-9, azodiisobutyronitrile 3-6, diallyl phthalate 2-4, poly (glycidyl methacrylate) 5-15, resorcinol bisglycidyl ether 28-43, ureaformaldehyde melamine resin 17-29, EDTA10-15, CTBN13-15, organo-silicon coupling agent 6-13, aminomethyl propanol 5-8, water 60-90, carbon dust 4-12, aluminium silicate powder 13-15, antimony oxide 10-15.The advantages of present invention is combined by graphene and epoxy resin, takes into account the two, improves the thermally conductive of compound, toughening and wear-resisting property, achievees the purpose that increase its weatherability.
Description
Technical field
The present invention relates to a kind of preparation methods of modified epoxy, more particularly to a kind of modified ring of polymer graphite alkene
The preparation method of oxygen resin belongs to Epoxy Resin Technology field.
Background technique
Graphene (Graphene) be one kind by carbon atom with sp2Hybridized orbit forms the two dimension that hexangle type is in honeycomb lattice
Carbon nanomaterial.
Graphene have excellent optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and
Drug delivery etc. is with important application prospects, it is considered to be a kind of future revolutionary material.
It successfully prepares two-dimensional graphene within 2004, becomes the carbon material research field after fullerene and carbon nanotube
Another important breakthrough.Graphene has excellent optical property, electromagnetic performance, heating conduction and mechanical property, can be widely applied
In fields such as structural materials.Currently, the application of graphene is concentrated mainly on the preparation research of fluoropolymer resin based composites.English
University of Manchester, state physicist An Deliegaimu and Constantine's Nuo Woxiao love, with micromechanics stripping method success from
Graphene is isolated in graphite, therefore obtains Nobel Prize in physics in 2010 jointly.The side of the common power production of graphene
Method is mechanical stripping method, oxidation-reduction method, SiC epitaxial growth method, and film production method is chemical vapour deposition technique (CVD).With
The gradually breakthrough of the problems such as mass production and large scale, the industrial application paces of graphene accelerating, based on
Some research achievements realize that the field of commercial applications may be mobile device, aerospace, new energy battery neck at first
Domain.
And epoxy resin (EP) be used as common resin matrix, have excellent adhesion energy, mechanical strength, heat resistance and
The features such as dielectricity, but contain a large amount of epoxy groups after its solidification, crosslink density is excessively high, therefore resulting product is in brittleness, and resistance to punching
Hitting property, electric conductivity and thermal conductivity etc. are poor, lead to such as coating, building plastic, rubber product, are applied to outdoor through climate
Test when, comprehensive as caused by illumination, cold and hot, wind and rain, bacterium etc. to destroy, tolerance is poor.
Therefore, it is necessary to a kind of preparation methods, composite material will be made after graphene and EP compounding, improve the resistance to of composite material
Hou Xing.
Summary of the invention
The main object of the present invention is to provide for a kind of preparation method of polymer graphite alkene modified epoxy, passes through
The advantages of graphene and epoxy resin combine, takes into account the two, improves the thermally conductive of compound, toughening and wear-resisting property, reaches increase
The purpose of its weatherability.
The purpose of the present invention can reach by using following technical solution:
A kind of preparation method of polymer graphite alkene modified epoxy, by weight including following component: graphene 5-
10, epoxy resin 60-80, polyacrylic acid N-butyl 15-20, phthalic anhydride 5-9, azodiisobutyronitrile 3-6, O-phthalic
Diallyl phthalate 2-4, poly (glycidyl methacrylate) 5-15, resorcinol bisglycidyl ether 28-43, ureaformaldehyde melamine
Polyimide resin 17-29, EDTA10-15, CTBN13-15, organo-silicon coupling agent 6-13, aminomethyl propanol 5-8, water 60-90, carbon dust 4-
12, aluminium silicate powder 13-15, antimony oxide 10-15.
Further, the CTBN is liquid nbr carboxyl terminal or polyurethane, and the CTBN includes acrylonitrile and two
Silica.
Further, the graphene is nano-graphite particle, micron graphite particle or graphene oxide microplate powder.
Further, the epoxy resin includes bisphenol A epoxide resin, bisphenol F epoxy resin and High Bromine epoxy Resin
It is one or more of.
It further, by weight further include following component: dispersing agent 5-10, defoaming agent 3-5 and disinfectant 2-5.
Further, the organo-silicon coupling agent is gamma-aminopropyl-triethoxy-silane or diethylenetriamine base propyl three
Methoxy silane.
Further, by weight including following component: graphene 8, epoxy resin 72, polyacrylic acid N-butyl 18, neighbour
Phthalate anhydride 6, azodiisobutyronitrile 4, diallyl phthalate 3, poly (glycidyl methacrylate) 10, isophthalic two
Phenol bisglycidyl ether 30, ureaformaldehyde melamine resin 20, EDTA13, CTBN14, organo-silicon coupling agent 8, aminomethyl propanol 7,
Water 80, carbon dust 8, aluminium silicate powder 14, antimony oxide 11.
Compared with prior art, the beneficial effects of the present invention are: polymer graphite alkene modified epoxy tree provided by the invention
The preparation method of rouge, manufactured composite material after graphite there is good thermal conductivity and mechanical strength to compound with epoxy resin
The advantage that the two can be given full play to, improves the performances such as thermal conductivity, tensile strength, fatigue resistance and the toughness of composite material.This hair
The preparation method of the polymer graphite alkene modified epoxy of bright offer, additionally it is possible to improve heat resistance, flame resistance, extend using period
And storage period, and cohesive force is superpower, penetration is extremely strong, can greatly improve in prolonged test of the outdoor through climate
Its weatherability, improves the economic value of the manufactured goods, has positive progress meaning.
Specific embodiment
To make the more clear and clear technical solution of the present invention of those skilled in the art, below with reference to embodiment to this hair
Bright to be described in further detail, embodiments of the present invention are not limited thereto.
Embodiment 1
The preparation method of polymer graphite alkene modified epoxy provided in this embodiment, by weight including such as the following group
Part: graphene 5-10, epoxy resin 60-80, polyacrylic acid N-butyl 15-20, phthalic anhydride 5-9, azodiisobutyronitrile
3-6, diallyl phthalate 2-4, poly (glycidyl methacrylate) 5-15, resorcinol bisglycidyl ether 28-
43, ureaformaldehyde melamine resin 17-29, EDTA10-15, CTBN13-15, organo-silicon coupling agent 6-13, aminomethyl propanol 5-8,
Water 60-90, carbon dust 4-12, aluminium silicate powder 13-15, antimony oxide 10-15, dispersing agent 5-10, defoaming agent 3-5 and disinfectant 2-
5。
CTBN preferred liquid nbr carboxyl terminal or polyurethane in the present embodiment, CTBN include acrylonitrile and titanium dioxide
Silicon, organo-silicon coupling agent are gamma-aminopropyl-triethoxy-silane or diethylenetriamine base propyl trimethoxy silicane.
In the present embodiment, graphene is nano-graphite particle, micron graphite particle or graphene oxide microplate powder, ring
Oxygen resin includes the one or more of bisphenol A epoxide resin, bisphenol F epoxy resin and High Bromine epoxy Resin, if selecting pure ring
Oxygen resin, for dynamic frictional coefficient up to 0.31, graphite oxide is added up to 8.1 × 10-4mm3/ (Nm) in wear rate
The frictionally damage of the composite material of alkene is negligible, and maximum friction resistance has decreased by 70%.
Embodiment 2
The preparation method of polymer graphite alkene modified epoxy provided in this embodiment, by weight including such as the following group
Part: graphene 8, epoxy resin 72, polyacrylic acid N-butyl 18, phthalic anhydride 6, azodiisobutyronitrile 4, phthalic acid
Diallyl 3, poly (glycidyl methacrylate) 10, resorcinol bisglycidyl ether 30, ureaformaldehyde melamine resin 20,
EDTA13, CTBN14, organo-silicon coupling agent 8, aminomethyl propanol 7, water 80, carbon dust 8, aluminium silicate powder 14, antimony oxide 11.
Embodiment 3
The preparation method of polymer graphite alkene modified epoxy provided in this embodiment, by weight including such as the following group
Part: the preparation method of polymer graphite alkene modified epoxy provided in this embodiment, by weight including following component: graphite
Alkene 9, epoxy resin 75, polyacrylic acid N-butyl 17, phthalic anhydride 8, azodiisobutyronitrile 6, diallyl phthalate third
Ester 4, poly (glycidyl methacrylate) 13, resorcinol bisglycidyl ether 35, ureaformaldehyde melamine resin 24,
EDTA14, CTBN15, organo-silicon coupling agent 11, aminomethyl propanol 5, water 77, carbon dust 11, aluminium silicate powder 13, antimony oxide 13,
Dispersing agent 7, defoaming agent 4 and disinfectant 4.
In the above-described embodiments, by graphene modified epoxy, the advantages of both taking into account, various performances is improved and are referred to
Mark, graphene has very big table specific area, in addition the dispersion of the molecular level of graphene, can form very strong between polymer
Interface interaction, the functional groups such as hydroxyl and manufacturing process can make graphene become the state of fold, these nanoscale out-of-flatnesses
The interaction between graphene and polymer chain can be enhanced, hydroxyl, the chemistry base such as carboxyl are contained in functional group's graphite alkene surface
Group can form stronger hydrogen bond with polarity macromolecule such as polymethyl methacrylate, and epoxy resin has excellent anti-rotten candle
Performance, adhesive property and electrical insulation capability, but but enbrittle after epoxy resin cure big, Anticrack ability is poor,
The disadvantages of poor heat resistance, causes weatherability poor, and the present embodiment improves epoxy resin by introducing reinforced phase in the epoxy
Performance be added to graphite is dilute in polymeric matrix as reinforcement, improve poly- for the excellent properties for making full use of graphene
The performance of object matrix is closed, the composite material being had excellent performance improves its weather resistance.
In some embodiments, the preparation process of the composite material of polymer graphite alkene modified epoxy are as follows:
Step (1) weighs a certain amount of epoxy resin and graphene mixing first；
Step (2), graphene is mixed with polyacrylic acid N-butyl and ultrasound (temperature is 25 DEG C, and power is within 5 hours
300W, frequency 50KHZ), epoxy resin is preheated into 30min in 90 DEG C of water-baths；
Modified graphene and polyacrylic acid N-butyl mixture are added in epoxy resin and in 90 DEG C of water-baths step (3)
During which raw material provided by the above embodiment is added in middle mechanical stirring 5 hours；
Mixed system is put into vacuum oven and vacuumizes 15 hours (temperature be 90 DEG C) by step (4)；
Curing agent addition mixed system after preheating is placed in gentle agitation 15min in 60 DEG C of water-baths by step (5), so
After be put into vacuum oven and vacuumize 15min (temperature be 50 DEG C)；
Step (6) pours into mixed system in warmed-up mold, and juxtaposition in a vacuum drying oven, solidifies 2 at 50 DEG C
Hour, solidify 2 hours and 120 DEG C at 90 DEG C at solidify 89 hours, sampled after being cooled to room temperature.
In conclusion in the embodiment above, the polymer graphite alkene modified epoxy that some embodiments above provides
Preparation method, introduce graphene and epoxy resin be modified, modified composite material obtained not only has leads well
Hot coefficient, mechanical performance are also greatly improved, and can be improved heat resistance, flame resistance, extend using period and storage period, and
And cohesive force is superpower, penetration is extremely strong, can substantially increase its weatherability in prolonged test of the outdoor through climate,
Have the effect of positive.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (7)
1. a kind of preparation method of polymer graphite alkene modified epoxy, which is characterized in that by weight including following component:
Graphene 5-10, epoxy resin 60-80, polyacrylic acid N-butyl 15-20, phthalic anhydride 5-9, azodiisobutyronitrile 3-6,
Diallyl phthalate 2-4, poly (glycidyl methacrylate) 5-15, resorcinol bisglycidyl ether 28-43, urea
Aldehyde melamine resin 17-29, EDTA10-15, CTBN13-15, organo-silicon coupling agent 6-13, aminomethyl propanol 5-8, water 60-
90, carbon dust 4-12, aluminium silicate powder 13-15, antimony oxide 10-15.
2. a kind of preparation method of polymer graphite alkene modified epoxy according to claim 1, which is characterized in that institute
Stating CTBN is liquid nbr carboxyl terminal or polyurethane, and the CTBN includes acrylonitrile and silica.
3. a kind of preparation method of polymer graphite alkene modified epoxy according to claim 1, which is characterized in that institute
Stating graphene is nano-graphite particle, micron graphite particle or graphene oxide microplate powder.
4. a kind of preparation method of polymer graphite alkene modified epoxy according to claim 1, which is characterized in that institute
State the one or more that epoxy resin includes bisphenol A epoxide resin, bisphenol F epoxy resin and High Bromine epoxy Resin.
5. a kind of preparation method of polymer graphite alkene modified epoxy according to claim 1, which is characterized in that press
Weight ratio further includes following component: dispersing agent 5-10, defoaming agent 3-5 and disinfectant 2-5.
6. a kind of preparation method of polymer graphite alkene modified epoxy according to claim 1, which is characterized in that institute
Stating organo-silicon coupling agent is gamma-aminopropyl-triethoxy-silane or diethylenetriamine base propyl trimethoxy silicane.
7. a kind of preparation method of polymer graphite alkene modified epoxy described in -6 according to claim 1, which is characterized in that
By weight including following component: graphene 8, epoxy resin 72, polyacrylic acid N-butyl 18, phthalic anhydride 6, azo two
Isobutyronitrile 4, diallyl phthalate 3, poly (glycidyl methacrylate) 10, resorcinol bisglycidyl ether 30,
Ureaformaldehyde melamine resin 20, EDTA13, CTBN14, organo-silicon coupling agent 8, aminomethyl propanol 7, water 80, carbon dust 8, alumina silicate
Powder 14, antimony oxide 11.
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Cited By (5)
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| CN111286292A (en) * | 2020-02-11 | 2020-06-16 | 广西大学 | Strong-weathering limestone dangerous rock joint filling agent and preparation method thereof |
| CN111440544A (en) * | 2020-03-24 | 2020-07-24 | 广西民族大学 | Holding agent for integrity of weakly weathered limestone cracks |
| CN112250999A (en) * | 2020-10-21 | 2021-01-22 | 广德龙泰电子科技有限公司 | Heat-resistant epoxy resin composition, halogen-free middle-Tg copper-clad plate and preparation method thereof |
| CN112608598A (en) * | 2020-10-30 | 2021-04-06 | 西南科技大学 | Microencapsulated graphene foam silicone rubber dielectric composite material and preparation method thereof |
| CN113004812A (en) * | 2021-03-30 | 2021-06-22 | 刘新宽 | Graphene modified resin packaging material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111286292A (en) * | 2020-02-11 | 2020-06-16 | 广西大学 | Strong-weathering limestone dangerous rock joint filling agent and preparation method thereof |
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| CN112250999A (en) * | 2020-10-21 | 2021-01-22 | 广德龙泰电子科技有限公司 | Heat-resistant epoxy resin composition, halogen-free middle-Tg copper-clad plate and preparation method thereof |
| CN112608598A (en) * | 2020-10-30 | 2021-04-06 | 西南科技大学 | Microencapsulated graphene foam silicone rubber dielectric composite material and preparation method thereof |
| CN113004812A (en) * | 2021-03-30 | 2021-06-22 | 刘新宽 | Graphene modified resin packaging material and preparation method thereof |
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