CN103396653A - Preparation method of graphene nanoplatelet/epoxy resin nanocomposite material - Google Patents
Preparation method of graphene nanoplatelet/epoxy resin nanocomposite material Download PDFInfo
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Abstract
The invention provides a preparation method of a graphene nanoplatelet/epoxy resin nanocomposite material. The preparation method comprises the following operating steps of: dispersing graphene nanoplatelets in an organic solvent, putting the organic solvent into an ultrasonic apparatus, carrying out ultrasonic treatment on the materials in an ice bath with power more than or equal to 250W for 1.5 hours, and simultaneously stirring the materials; adding epoxy resins, carrying out ultrasonic treatment in the ice bath with power more than or equal to 250W for 1.5 hours, and simultaneously stirring; putting the materials into an oil bath, raising the temperature to the boiling point of the used organic solvent, simultaneously stirring for 5-15 hours, and then putting the materials into a vacuum oven to be decompressed and heated for 2 hours; cooling to room temperature, adding a curing agent according to the usage amount of the epoxy resins, and stirring the materials for 0.5 hour; and putting the materials in the vacuum oven to be decompressed for 1 hour at normal temperature, then pouring the materials into a forming mold, and putting the forming mold into the oven to be cured, thus obtaining the graphene nanoplatelet/epoxy resin nanocomposite material. In the method, the graphene nanoplatelets are utilized to improve the thermal properties and flame retardance of the epoxy resins, thus solving the problem of dispersion of the graphene nanoplatelets in epoxy resin matrices.
Description
Technical field
The present invention relates to the Nano-composite materials technical field, be specifically related to a kind of preparation method of Graphene microplate/epoxy resin nano composites.
Background technology
Epoxy resin is a kind of extremely important thermosetting polymer.Due to its outstanding physical strength and toughness, good anti-solvent and chemical resistant properties and superior cementability, epoxy resin is widely used as the matrix of coating, tackiness agent, veneer sheet, semiconductor packages and advanced fibre reinforced composites.Yet the oxygen index of the epoxy resin after solidifying only has 15 left and right, is quite low, under air conditions, just can self burn.As can be seen here, inflammableness is a large defect of epoxy resin, has limited greatly its application, and therefore, to epoxy resin, carry out flame-retardant modified is the focus that people endeavour to study always.
The Graphene microplate refers to that the carbon-coating number is more than 10 layers, the ultra-thin Graphene stratiform accumulation body of thickness in the 5-100 nanometer range.The Graphene microplate has kept the original planar carbon six-ring of graphite conjugation crystalline structure, has excellent physical strength, conduction, heat conductivility, and good lubricated, high temperature resistant, high temperature resistant and anticorrosion properties, and production cost is low, and application prospect is extensive.Simultaneously, its laminate structure can stop inflammable gas to escape into flame zone, stop the energy passback and promote into charcoal, is expected to become the BACN of efficient few additive.In order to take full advantage of the potential of Graphene microplate, must make its dispersion that reaches molecular level in matrix and effectively load transmission at the interface.Yet the Graphene microplate has the surface of strong gathering tendency and height inertia, and its scattering problem and the redispersion problem in matrix thereof have limited the performance of its premium properties.Therefore, keeping the nano-grade size of Graphene microplate in matrix, is the key for preparing Graphene microplate nano composite material, is also the difficult problem that preparation high-performance mixture must be captured.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of Graphene microplate/epoxy resin nano composites, the method utilizes the Graphene microplate to improve thermal characteristics and the flame retardant properties of epoxy resin, has solved the scattering problem of Graphene microplate in epoxy resin-base.
The technical solution adopted in the present invention is:
A kind of preparation method of Graphene microplate/epoxy resin nano composites comprises following operation steps:
(1) getting the Graphene microplate is dispersed in organic solvent and forms suspension, suspension is put into to ultrasonic apparatus, the mixture of ice and water of packing in ultrasonic apparatus simultaneously, the power ice-bath ultrasonic of use >=250W 1.5 hours, stir suspension with the mechanical stirring instrument in the time of ultrasonic;
(2) in step (1) gained liquid, add epoxy resin, the power ice-bath ultrasonic of continuation use >=250W 1.5 hours, stir with the mechanical stirring instrument in the time of ultrasonic;
(3) gained mixture in step (2) is put into to oil bath, oil bath is warming up to the boiling point of organic solvent used, uses simultaneously magnetic stirrer 5-15 hour, makes organic solvent evaporation, put into subsequently vacuum drying oven, decompression heats up and removed residual organic solvent in 2 hours;
(4) step (3) gained mixture is cooled to room temperature, according to the usage quantity of epoxy resin, adds solidifying agent, with magnetic stirrer, made to mix in 0.5 hour;
(5) step (4) gained mixture is put into to vacuum drying oven, the bubble that under normal temperature, decompression was removed in mixture in 1 hour, pour into subsequently in forming mould, forming mould is put into to baking oven to be solidified, condition of cure is 50 ℃ of Procuring 5-10 hours, 110 ℃ of curing 2-5 hour, namely obtains Graphene microplate/epoxy resin nano composites of the present invention.
The concentration that the middle Graphene microplate of described step (1) is dispersed in the suspension that forms in organic solvent is 0.01-10mg/ml.
Organic solvent is a kind of in acetone, ethanol, tetrahydrofuran (THF), DMF in described step (1).
In described step (2), the add-on of epoxy resin is 20-100 times (being preferably 20 times) of Graphene microplate usage quantity in step (1) (calculating by weight), namely according to listed as parts by weight, the epoxy resin of 100 parts of weight parts need to add the Graphene microplate of 1-5 part weight part (being preferably 5 parts of weight parts).
In described step (2), the viscosity of epoxy resin is 1.13-1.15 g/cm
3.
In described step (3) and step (5) method of decompression be specially use water pump to take out to make into negative pressure-0.1 ~-0.08MPa.
The kind of organic solvent used in the temperature that in described step (3), temperature-rise period reaches depending on step (1), when organic solvent is acetone, be warming up to 56 ℃, when the ethanol 80 ℃, during for tetrahydrofuran (THF) 65 ℃, during for DMF 153 ℃.
In described step (4), the add-on of solidifying agent is the 30-50% of epoxy resin usage quantity in step (2) (calculating by weight).
In described step (4), solidifying agent is amine curing agent.
Compared with prior art, the present invention has following remarkable advantage and beneficial effect:
1. the present invention is from the angle of the dispersiveness of raising Graphene microplate, adopt solution blending and secondary ice-bath ultrasonic method, prepared Graphene microplate/epoxy resin nano composites, made the Graphene microplate that exists sheet to peel off in the epoxy resin of the matrix material that is prepared into.The method that this promotion disperses is entirely the Physical Processing method, and universality is strong, to system, does not introduce any other additive or chemical composition, can make the Graphene microplate in epoxy resin-base, reach the nano level dispersion effect.
Graphene microplate addition just can significantly improve seldom the time epoxy resin thermostability, improve matrix material limiting oxygen index(LOI), improve the charring property of combustion of epoxy resin, reduce the melting drippage.When Graphene microplate addition is 0.5 weight part (epoxy resin is 100 mass parts) of weight epoxy, just can restrain the melting drip phenomenon of epoxy resin fully.
The accompanying drawing explanation
Figure 1 shows that the perspective Electronic Speculum figure of the Graphene microplate/epoxy resin nano composites of the embodiment of the present invention 1 preparation;
Shown in Figure 2 is the schematic appearance of sample after the test of oxygen index tester prepared by various embodiments of the present invention and Comparative Examples;
The TG graphic representation of matrix material, Graphene microplate and epoxy resin prepared by various embodiments of the present invention that shown in Figure 3 is, wherein ER is that epoxy resin, GNS are that Graphene microplate, ER/GNS0.3 are that matrix material, the ER/GNS0.5 of embodiment 5 preparations is that matrix material, the ER/GNS1 of embodiment 4 preparations is that matrix material, the ER/GNS3 of embodiment 3 preparations is that matrix material, the ER/GNS5 of embodiment 2 preparations is the matrix material of embodiment 1 preparation.
Embodiment
Below in conjunction with embodiment, the present invention is further described in detail, but is not limited to this.
Embodiment 1:
Graphene microplate/epoxy resin nano composites prepared by the present embodiment, its epoxy resin, solidifying agent, Graphene microplate weight proportion are 100:33:5.
The preparation method is as follows:
Get 5g Graphene microplate and be dispersed in acetone and form suspension, making suspension concentration is 10mg/ml.This suspension is put into to ultrasonic apparatus, and the mixture of ice and water of packing in ultrasonic apparatus simultaneously, stirred 1.5 hours simultaneously with the power ice-bath ultrasonic of 250W.In gained solution, add 100g epoxy monomer JY-256, continue to stir simultaneously 1.5 hours with the power ice-bath ultrasonic of 250W.The gained mixture is put into to 60 ℃ of oil baths, stirred 5 hours.Put into subsequently vacuum drying oven, vacuumize 2 hours under 60 ℃.The gained mixture is cooled to room temperature, adds 33g solidifying agent D230, stirred 0.5 hour.The gained mixture is put into to vacuum drying oven, under normal temperature, vacuumize 1 hour bubble removing, pour in mould subsequently.Mould is put into to baking oven, and 50 ℃ of Procuring are after 5 hours, and 110 ℃ solidified 2 hours, and the demoulding namely obtains Graphene microplate/epoxy resin nano composites sample.
This sample is cut into slices and utilized transmission electron microscope observing, and as shown in Figure 1, the Graphene microplate that sheet is peeled off is present in epoxy resin-base result.Thermal gravimetric analyzer shows this sample analysis result, and the remaining carbon of Graphene microplate/epoxy resin nano composites is 9.0 %.With the oxygen index tester, this sample is carried out to limiting oxygen index(LOI) mensuration, LOI reaches 21.4, and when the batten after test can be found out burning, without the molten drop phenomenon, the batten after test was as shown in Fig. 2 (f).
Embodiment 2:
Graphene microplate/epoxy resin nano composites prepared by the present embodiment, its epoxy resin, solidifying agent, Graphene microplate weight proportion are 100:33:3.
The preparation method is as follows:
Get 3g Graphene microplate and be dispersed in acetone and form suspension, making suspension concentration is 10mg/ml.This suspension is put into to ultrasonic apparatus, and the mixture of ice and water of packing in ultrasonic apparatus simultaneously, stirred 1.5 hours simultaneously with the power ice-bath ultrasonic of 250W.In gained solution, add 100g epoxy monomer JY-256, continue to stir simultaneously 1.5 hours with the power ice-bath ultrasonic of 250W.The gained mixture is put into to 60 ℃ of oil baths, stirred 5 hours.Put into subsequently vacuum drying oven, vacuumize 2 hours under 60 ℃.The gained mixture is cooled to room temperature, adds 33g solidifying agent D230, stirred 0.5 hour.The gained mixture is put into to vacuum drying oven, under normal temperature, vacuumize 1 hour bubble removing, pour in mould subsequently.Mould is put into to baking oven, and 50 ℃ of Procuring are after 5 hours, and 110 ℃ solidified 2 hours, and namely obtained Graphene microplate/epoxy resin nano composites sample.
Thermal gravimetric analyzer shows this sample analysis result, and the remaining carbon of Graphene microplate/epoxy resin nano composites is 7.2 %.With the oxygen index tester, this sample is carried out to limiting oxygen index(LOI) mensuration, LOI reaches 21.0, and when the batten after test can be found out burning, without the molten drop phenomenon, the batten after test was as shown in Fig. 2 (e).
Embodiment 3:
Graphene microplate/epoxy resin nano composites prepared by the present embodiment, its epoxy resin, solidifying agent, Graphene microplate weight proportion are 100:33:1.
The preparation method is as follows:
Get 1g Graphene microplate and be dispersed in acetone, making suspension concentration is 10mg/ml.This suspension is put into to ultrasonic apparatus, and the mixture of ice and water of packing in ultrasonic apparatus simultaneously, stirred 1.5 hours simultaneously with the power ice-bath ultrasonic of 250W.In gained solution, add 100g epoxy monomer JY-256, continue to stir simultaneously 1.5 hours with the power ice-bath ultrasonic of 250W.The gained mixture is put into to 60 ℃ of oil baths, stirred 5 hours.Put into subsequently vacuum drying oven, vacuumize 2 hours under 60 ℃.The gained mixture is cooled to room temperature, adds 33g solidifying agent D230, stirred 0.5 hour.The gained mixture is put into to vacuum drying oven, under normal temperature, vacuumize 1 hour bubble removing, pour in mould subsequently.Mould is put into to baking oven, and 50 ℃ of Procuring are after 5 hours, and 110 ℃ solidified 2 hours, and namely obtained Graphene microplate/epoxy resin nano composites.Thermal gravimetric analyzer shows this sample analysis result, and the remaining carbon of Graphene microplate/epoxy resin nano composites is 3.8 %.With the oxygen index tester, this sample is carried out to limiting oxygen index(LOI) mensuration, LOI reaches 19.5, and when the batten after test can be found out burning, without the molten drop phenomenon, the batten after test as shown in Figure 2 (d) shows.
Embodiment 4:
Graphene microplate/epoxy resin nano composites prepared by the present embodiment, its epoxy resin, solidifying agent, Graphene microplate weight proportion are 100:33:0.5.
The preparation method is as follows:
Get 0.5g Graphene microplate and be dispersed in acetone, making suspension concentration is 10mg/ml.This suspension is put into to ultrasonic apparatus, and the mixture of ice and water of packing in ultrasonic apparatus simultaneously, stirred 1.5 hours simultaneously with the power ice-bath ultrasonic of 250W.In gained solution, add 100g epoxy monomer JY-256, continue to stir simultaneously 1.5 hours with the power ice-bath ultrasonic of 250W.The gained mixture is put into to 60 ℃ of oil baths, stirred 5 hours.Put into subsequently vacuum drying oven, vacuumize 2 hours under 60 ℃.The gained mixture is cooled to room temperature, adds 33g solidifying agent D230, stirred 0.5 hour.The gained mixture is put into to vacuum drying oven, under normal temperature, vacuumize 1 hour bubble removing, pour in mould subsequently.Mould is put into to baking oven, and 50 ℃ of Procuring are after 5 hours, and 110 ℃ solidified 2 hours, and namely obtained Graphene microplate/epoxy resin nano composites sample.
Thermal gravimetric analyzer shows this sample analysis result, and the remaining carbon of Graphene microplate/epoxy resin nano composites is 3.2 %.With the oxygen index tester, this sample is carried out to limiting oxygen index(LOI) mensuration, LOI reaches 19.1, and when the batten after test can be found out burning, without the molten drop phenomenon, the batten after test was as shown in Fig. 2 (c).
Embodiment 5:
Graphene microplate/epoxy resin nano composites prepared by the present embodiment, its epoxy resin, solidifying agent, Graphene microplate weight proportion are 100:33:0.3.
The preparation method is as follows:
Get 0.3g Graphene microplate and be dispersed in acetone, making suspension concentration is 10mg/ml.This suspension is put into to ultrasonic apparatus, and the mixture of ice and water of packing in ultrasonic apparatus simultaneously, stirred 1.5 hours simultaneously with the power ice-bath ultrasonic of 250W.In gained solution, add 100g epoxy monomer JY-256, continue to stir simultaneously 1.5 hours with the power ice-bath ultrasonic of 250W.The gained mixture is put into to 60 ℃ of oil baths, stirred 5 hours.Put into subsequently vacuum drying oven, vacuumize 2 hours under 60 ℃.The gained mixture is cooled to room temperature, adds 33g solidifying agent D230, stirred 0.5 hour.The gained mixture is put into to vacuum drying oven, under normal temperature, vacuumize 1 hour bubble removing, pour in mould subsequently.Mould is put into to baking oven, and 50 ℃ of Procuring are after 5 hours, and 110 ℃ solidified 2 hours, and namely obtained Graphene microplate/epoxy resin nano composites sample.
Thermal gravimetric analyzer shows this sample analysis result, and the remaining carbon of Graphene microplate/epoxy resin nano composites is 3.1 %.With the oxygen index tester, this sample is carried out to limiting oxygen index(LOI) mensuration, LOI reaches 18.0, and there is the molten drop phenomenon in the batten after test in the time of can finding out burning, and the batten after test is as shown in Fig. 2 (b).
Comparative Examples:
This Comparative Examples is not added the Graphene microplate, directly prepares epoxy resin.
The preparation method is as follows:
By 100g epoxy monomer JY-256,33g solidifying agent D230 mixes, and with magnetic stirrer, makes it even mixing in 0.5 hour.The gained mixture is put into to vacuum drying oven, the bubble removed in mixture in 1 hour of decompression under normal temperature, careful pouring in mould, put into baking oven by mould and solidify subsequently.Condition of cure is: 50 ℃ of Procuring are after 5 hours, and 110 ℃ solidified 2 hours, and namely obtained epoxide resin polymer.
Thermal gravimetric analyzer shows this sample analysis result, and the remaining carbon of epoxy resin is 2.1 %.With the oxygen index tester, this sample is carried out to limiting oxygen index(LOI) mensuration, LOI reaches 15.9, and the batten after test has obvious molten drop phenomenon in the time of can finding out burning, and the batten after test as shown in Figure 2 (a) shows.
Figure 3 shows that it is the TG graphic representation of the various embodiments of the present invention matrix material, Graphene microplate and the epoxy resin that prepare.As seen from Figure 3, the Graphene microplate add the charring property of combustion that can improve epoxy resin, and the addition of Graphene microplate is larger, the carbon residue amount of Graphene microplate/epoxy resin nano composites is larger.
The testing standard that limiting oxygen index(LOI) of the present invention is tested institute's foundation is GB2406-80.
The above embodiment of the present invention is to explanation of the present invention and can not be used to limiting the present invention, and the implication suitable with claims of the present invention and any change in scope, all should think to be included in the scope of claims.
Claims (9)
1. the preparation method of a Graphene microplate/epoxy resin nano composites is characterized in that comprising following operation steps:
(1) getting the Graphene microplate is dispersed in organic solvent and forms suspension, suspension is put into to ultrasonic apparatus, the mixture of ice and water of packing in ultrasonic apparatus simultaneously, the power ice-bath ultrasonic of use >=250W 1.5 hours, stir suspension with the mechanical stirring instrument in the time of ultrasonic;
(2) in step (1) gained liquid, add epoxy resin, the power ice-bath ultrasonic of continuation use >=250W 1.5 hours, stir with the mechanical stirring instrument in the time of ultrasonic;
(3) gained mixture in step (2) is put into to oil bath, oil bath is warming up to the boiling point of organic solvent used, uses simultaneously magnetic stirrer 5-15 hour, makes organic solvent evaporation, put into subsequently vacuum drying oven, decompression heats up and removed residual organic solvent in 2 hours;
(4) step (3) gained mixture is cooled to room temperature, according to the usage quantity of epoxy resin, adds solidifying agent, with magnetic stirrer, made to mix in 0.5 hour;
(5) step (4) gained mixture is put into to vacuum drying oven, the bubble that under normal temperature, decompression was removed in mixture in 1 hour, pour into subsequently in forming mould, forming mould is put into to baking oven to be solidified, condition of cure is 50 ℃ of Procuring 5-10 hours, 110 ℃ of curing 2-5 hour, namely obtains Graphene microplate/epoxy resin nano composites of the present invention.
2. the preparation method of a kind of Graphene microplate/epoxy resin nano composites according to claim 1 is characterized in that: in described step (1), to be dispersed in the concentration of the suspension that forms in organic solvent be 0.01-10mg/ml to the Graphene microplate.
3. the preparation method of a kind of Graphene microplate/epoxy resin nano composites according to claim 1 is characterized in that: in described step (1), organic solvent is a kind of in acetone, ethanol, tetrahydrofuran (THF), DMF.
4. the preparation method of a kind of Graphene microplate/epoxy resin nano composites according to claim 1 is characterized in that: in described step (2) add-on of epoxy resin be Graphene microplate usage quantity in step (1) 20-100 doubly.
5. the preparation method of a kind of Graphene microplate/epoxy resin nano composites according to claim 4 is characterized in that: in described step (2), the add-on of epoxy resin is 20 times of Graphene microplate usage quantity in step (1).
6. the preparation method of a kind of Graphene microplate/epoxy resin nano composites according to claim 1 is characterized in that: in described step (2), the viscosity of epoxy resin is 1.13-1.15 g/cm
3.
7. the preparation method of a kind of Graphene microplate/epoxy resin nano composites according to claim 1 is characterized in that: in described step (3) and step (5) method of decompression be specially use water pump to take out to make into negative pressure-0.1 ~-0.08MPa.
8. the preparation method of a kind of Graphene microplate/epoxy resin nano composites according to claim 1 is characterized in that: in described step (4), the add-on of solidifying agent is the 30-50% of epoxy resin usage quantity in step (2).
9. the preparation method of a kind of Graphene microplate/epoxy resin nano composites according to claim 1 is characterized in that: in described step (4), solidifying agent is amine curing agent.
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| CN110373140A (en) * | 2019-08-12 | 2019-10-25 | 江南大学 | A kind of epoxy adhesive and preparation method thereof |
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