CN109486114B - Graphene epoxy resin high-molecular nano composite material and preparation method thereof - Google Patents
Graphene epoxy resin high-molecular nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of nano materials, and discloses a graphene epoxy resin high-molecular nano composite material and a preparation method thereof. The solvents used in the invention are absolute ethyl alcohol and acetone, so that the environmental pollution is small; the composite material is prepared by adopting an ultrasonic blending method, so that the process is simple; the ultrasonic vibration power is determined, and the dispersibility of the graphene in the epoxy resin matrix can be better improved; the composite material prepared by the process has better conductivity and thermal expansion performance.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a graphene epoxy resin high-molecular nano composite material and a preparation method thereof.
Background
Currently, the current state of the art commonly used in the industry is such that:
in the existing preparation process of the graphene/epoxy resin composite material, a common preparation method is a solution blending method. Wherein the dispersibility of the graphene in the matrix is an important factor influencing the performance of the material. The prior art mainly solves the problem by the following methods:
improving the dispersibility of the graphene by traditional mechanical stirring;
the agglomeration of graphene in a matrix is reduced by connecting an organic group to the surface of the graphene;
the graphene and other fillers cooperatively enhance the performance of the matrix material.
The composite material prepared by the existing process has low enhancement degree of the graphene on the mechanical, electrical and thermal properties of an epoxy resin matrix.
In summary, the problems of the prior art are as follows:
(1) the common traditional mechanical stirring is used for improving the dispersibility of the graphene, and in the process of preparing the graphene/epoxy resin composite material, the dispersibility of the graphene is poor, and the enhancement degree of the graphene on the mechanical, electrical and thermal properties of an epoxy resin matrix is low.
(2) The technical route for adopting the graphene surface to connect the organic group or the graphene and other fillers to cooperatively reinforce the composite material is complex and has low efficiency.
The difficulty and significance for solving the technical problems are as follows:
graphene has excellent mechanical, electrical and thermal properties, but the properties are difficult to show in a composite material, mainly because graphene is easy to agglomerate in a high-molecular matrix and the adhesion with a matrix interface is poor. The existing technology is difficult to improve the dispersibility of graphene in a matrix material and reduce the agglomeration of the graphene.
The technical problem is solved, the enhancement degree of the graphene to various properties of the matrix epoxy resin can be improved, and a simple and effective technical route is provided.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a graphene epoxy resin high-molecular nano composite material and a preparation method thereof. According to the invention, the graphene/epoxy resin composite material is prepared by using an ultrasonic blending method, the aggregation of graphene is reduced by using ultrasonic vibration, the dispersibility of graphene in an epoxy resin matrix is improved, and the uniformly dispersed graphene can better enhance the mechanical, electrical and thermal properties of the epoxy resin matrix.
The invention is realized in such a way that a preparation method of a graphene epoxy resin polymer nanocomposite material comprises the following steps: graphene: 10g of a mixture of graphene, epoxy resin and a curing agent;
step one, graphene soaking and planetary stirring: graphene is prepared by mixing the following components in percentage by mass: adding graphene, epoxy resin and a curing agent in a proportion of 1% -5% into 50-80 ml of absolute ethyl alcohol solution, pre-soaking, and performing planetary stirring on a mixed solution of the soaked graphene and the absolute ethyl alcohol;
step two, mixing and stirring the graphene soaking material: stirring the mixed solution obtained in the first step by using ultrasonic waves, and then stirring by using a planet;
step three, dissolving the epoxy resin material: epoxy resin is prepared by the following steps of: adding 1% -5% of graphene, epoxy resin and curing agent into 40ml of acetone solution, and ultrasonically stirring;
step four, mixing and stirring the nano composite material: mixing the solution obtained in the second step with the solution obtained in the third step, stirring by using ultrasonic waves, and stirring by using a planet;
step five, adding a binder: adding 0.16g of KH-570 solution into the solution obtained in the fourth step, stirring with a stirrer, drying the solution, and volatilizing the solvent;
step six, adding a curing agent: adding a curing agent into the solution obtained in the fifth step, wherein the mass ratio of the curing agent to the epoxy resin is 1: 3, stirring with a parallel star, and removing bubbles;
step seven, curing the nano composite material: and (5) pouring the solution obtained in the step six into a mold, solidifying, cooling and demolding to obtain the graphene epoxy resin nano composite material.
Further, in the first step, the pre-soaking is carried out for more than 6 hours, the planet stirring is carried out for 30 minutes, and the rotating speed is 2000 rpm.
Further, in the second step, ultrasonic stirring is carried out for 30 minutes at the ultrasonic power of 900W, and then planetary stirring is carried out for 5 minutes at the rotating speed of 2000 rpm.
Further, in the third step, ultrasonic stirring is carried out for 5 minutes, so that the epoxy resin is fully dissolved;
further, in the fourth step, ultrasonic agitation was used for 30 minutes at a power of 900w, and planetary agitation was used for 5 minutes.
Further, in the fifth step, stirring for 5 minutes in a planet way, putting the solution into a forced air drying oven to volatilize most of the solvent, then putting the solution into a vacuum drying oven to continuously volatilize the solvent, wherein the temperature is 90 ℃, and the drying time is 10 hours.
Further, in the sixth step, stirring was carried out for 3 minutes with a planetary stirrer, and defoaming was carried out for 2 minutes.
Further, in the seventh step, the solution in the sixth step is placed into a mold, and is solidified for 2 hours at the temperature of 80 ℃, and then is solidified for 2 hours at the temperature of 120 ℃, and is cooled along with a furnace.
The invention also aims to provide a graphene epoxy resin high-molecular nano composite material.
The invention also aims to provide an automobile preparation part prepared by using the graphene epoxy resin polymer nanocomposite.
The invention also aims to provide an electronic and electric appliance insulating packaging and functional coating prepared by using the graphene epoxy resin high-molecular nano composite material.
In summary, the advantages and positive effects of the invention are:
the solvents used by the invention are absolute ethyl alcohol and acetone, and the environmental pollution is small.
The composite material is prepared by an ultrasonic blending method, and the process is simple.
The ultrasonic vibration power is determined, and the dispersibility of the graphene in the epoxy resin matrix can be better improved. Fig. 4 is a scanning electron micrograph of the material prepared using only planetary stirring, and it can be seen that graphene is concentrated in several regions and is not well dispersed. Fig. 5 is a scanning electron micrograph of the material prepared using ultrasonic vibration, and it can be seen that graphene is uniformly dispersed in the epoxy matrix. This indicates that the ultrasonic vibration can better improve the dispersibility of the graphene in the epoxy resin matrix.
The composite material prepared by the process has better conductivity and thermal expansion performance.
Due to the excellent mechanical, electrical and thermal properties of graphene, the mechanical property, the thermal property, the corrosion resistance and the electrical property of graphene can be remarkably improved by adding a proper amount of graphene as a reinforcement modified epoxy resin, and the graphene has a wide prospect in the fields of automobile lightweight design, electronic and electrical insulation packaging, functional coatings and the like.
Drawings
Fig. 1 is a flowchart of a method for preparing a graphene epoxy resin polymer nanocomposite according to an embodiment of the present invention.
Fig. 2 is a graph of the ultrasonic stirring vibration power and the thermal expansion coefficient (2 wt%) of the graphene/epoxy resin composite material according to the embodiment of the present invention.
Fig. 3 is a graph of ultrasonic power versus electrical conductivity (3 wt%) for graphene/epoxy composite materials provided by embodiments of the present invention.
FIG. 4 is a scanning electron micrograph of a material prepared using planetary stirring only as provided by an embodiment of the present invention.
Fig. 5 is a scanning electron micrograph of a material prepared using ultrasonic vibration according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the existing preparation process of the graphene/epoxy resin composite material, the traditional mechanical stirring is commonly used to improve the dispersibility of graphene, and the dispersibility of graphene in the composite material is poor.
The composite material prepared by the existing process has low enhancement degree of the graphene on the mechanical, electrical and thermal properties of an epoxy resin matrix.
Fig. 1 is a preparation method of a graphene epoxy resin polymer nanocomposite provided in an embodiment of the present invention, including:
s101, graphene soaking and planetary stirring: adding a proper amount of absolute ethyl alcohol solution into graphene with specified mass, pre-soaking for more than 6 hours, and then carrying out planetary stirring on the soaked mixed solution of the graphene and the absolute ethyl alcohol for 30 minutes at the rotating speed of 2000 rpm;
s102, mixing and stirring the graphene soaking material: stirring the mixed solution obtained in the step S101 for 30 minutes by using ultrasonic waves, wherein the ultrasonic power is 900W, and then stirring for 5 minutes by using a planet at the rotating speed of 2000 rpm;
s103, dissolving an epoxy resin material: adding epoxy resin with specified mass into an appropriate amount of acetone solution, and ultrasonically stirring for 5 minutes to fully dissolve the epoxy resin;
s104, mixing and stirring the nano composite material: mixing the solution of the step S102 and the solution of the step S103, stirring for 30 minutes by using ultrasonic waves with the power of 900w, and stirring for 5 minutes by using a planet;
s105, adding a binder: stirring a specified amount of KH-570 solution in the solution obtained in the step S104 for 5 minutes, putting the solution in an air-blowing drying oven to volatilize most of the solvent, putting the solution in a vacuum drying oven to continuously volatilize the solvent, wherein the temperature is 90 ℃, and the drying time is 10 hours;
s106, adding a curing agent: adding a curing agent into the solution obtained in the step S105, wherein the mass ratio of the curing agent to the epoxy resin is 1: 3, stirring for 3 minutes with a parallel star, and removing bubbles for 2 minutes;
s107, curing the nano composite material: and (4) pouring the solution obtained in the step (S106) into a mold, curing for 2 hours at the temperature of 80 ℃, curing for 2 hours at the temperature of 120 ℃, furnace-cooling, and demolding to obtain the graphene/epoxy resin nanocomposite.
The mass ratio of the graphene to the epoxy resin to the curing agent is as follows: graphene: 1% -5% of graphene, epoxy resin and curing agent.
The embodiment of the invention provides a graphene epoxy resin high-molecular nano composite material.
The following uses of the invention are further described in conjunction with specific assays.
According to the invention, the graphene/epoxy resin composite material is prepared by adopting an ultrasonic blending method, the size of the graphene can be ensured by ultrasonic vibration with the power of 900w, the agglomeration of the graphene in an epoxy resin matrix is obviously reduced, and the dispersibility of the graphene is improved.
The thermal expansion coefficient of the composite material prepared by the method is obviously reduced compared with that of pure epoxy resin. When the content of the graphene is 5 wt%, the thermal expansion coefficient of the composite material between 30 ℃ and 120 ℃ is 35% lower than that of pure epoxy resin. And the composite material prepared by the ultrasonic power of 900w has smaller thermal expansion rate than that prepared by the ultrasonic power of 840w, the convergence of the thermal expansion rate is good, and the fluctuation of each temperature point is small. As in table 1.
TABLE 1 coefficient of thermal expansion of graphene/EP composites (900W/2h)
Table1 CTE of graphene/EP nanocomposites(900W/2h)
Fig. 2 is a graph of the ultrasonic stirring vibration power and the thermal expansion coefficient (2 wt%) of the graphene/epoxy resin composite material according to the embodiment of the present invention. The composite material prepared by the method has better conductivity compared with ultrasonic power (840w, 960w and 1020 w).
From figure 2 it can be seen that the composite material has a thermal expansion rate of 50-80 c, the lower the thermal expansion rate, indicating a lower degree of thermal expansion. It is obvious that when the ultrasonic power is 900w, the thermal expansion rate of the material at a given temperature point is lower, and the fluctuation of each temperature point is small. This indicates that the material prepared using an ultrasonic power of 900w possesses better thermal expansion properties.
Fig. 3 is a graph of ultrasonic power versus electrical conductivity (3 wt%) for graphene/epoxy composite materials provided by embodiments of the present invention. As can be seen from fig. 3, the conductance increases and then decreases with the increase of the vibration power, and reaches a peak value at the vibration power of 900w, so that the magnitude of the vibration power directly determines the conductivity of the composite material. When the ultrasonic stirring vibration power is smaller, the dispersion of graphene in the matrix does not reach the best state, and poor conductivity is caused due to the possible poor phenomena such as agglomeration. The vibration power gradually improves with the increase of the vibration power, and finally reaches a peak value. However, when the vibration power is increased continuously and the vibration power is too large (960W) or too large (1020W), the dispersion of graphene is improved well, but graphene sheets may be broken, and the effect of large surface area of graphene is lost, which may result in the performance degradation of the material.
The invention determines the ultrasonic vibration power and can better improve the dispersibility of the graphene in the epoxy resin matrix. Fig. 4 is a scanning electron micrograph of the material prepared using only planetary stirring, and it can be seen that graphene is concentrated in several regions and is not well dispersed. Fig. 5 is a scanning electron micrograph of the material prepared using ultrasonic vibration, and it can be seen that graphene is uniformly dispersed in the epoxy matrix. This indicates that the ultrasonic vibration can better improve the dispersibility of the graphene in the epoxy resin matrix.
The application of the invention is further described below with reference to specific examples.
Example 1:
the method comprises the following steps: weighing 3g of graphene, adding 50-80 ml of absolute ethyl alcohol solution, pre-soaking for more than 6 hours, and stirring the soaked mixed solution of the graphene and the absolute ethyl alcohol for 30 minutes in a planetary way at the rotating speed of 2000 rpm; the mixed solution was stirred with 900w ultrasonic waves for 30 minutes and then stirred with a planetary mixer at 2000 rpm for 5 minutes.
Step two: weighing 5.25g of epoxy resin, adding the epoxy resin into a proper amount of 40ml of acetone solution, and ultrasonically stirring for 5 minutes to fully dissolve the epoxy resin;
step three: mixing the solution of the first step and the solution of the second step, and ultrasonically stirring the mixture for 30 minutes by using 900w of power, and further stirring the mixture for 5 minutes by using a planet. Then 0.16g of KH-570 solution is added, stirring is carried out for 5 minutes, then part of solution is put into an air-blowing drying oven to volatilize most of solution, and then the solution is put into a vacuum drying oven to continuously mix and volatilize the solvent, wherein the temperature is 90 ℃, and the drying time is 10 hours; adding 1.75g of curing agent and stirring for 3 minutes in a planet way, and removing bubbles for two minutes; and finally, placing the composite into a drying oven for curing at 80 ℃ for 2 hours, and curing at 120 ℃ for two hours to obtain the graphene/epoxy resin composite material with the content of 3 wt%.
Example 2:
the procedure was as in example 1, except that the graphene content was 2 wt%, i.e., 2g of graphene, 6g of epoxy resin, and 2g of curing agent were weighed.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A preparation method of a graphene epoxy resin polymer nanocomposite is characterized by comprising the following steps:
step one, graphene soaking and planetary stirring: graphene according to the mass ratio: adding graphene, epoxy resin and a curing agent in a proportion of 1% -5% into 50-80 ml of absolute ethyl alcohol solution, pre-soaking, and performing planetary stirring on a mixed solution of the soaked graphene and the absolute ethyl alcohol;
step two, mixing and stirring the graphene soaking material: stirring the mixed solution obtained in the first step by using ultrasonic waves, and then stirring by using a planet;
step three, dissolving the epoxy resin material: and (3) mixing the graphene with the specified mass ratio: adding 1% -5% of graphene, epoxy resin and curing agent into 40ml of acetone solution, and ultrasonically stirring;
step four, mixing and stirring the nano composite material: mixing the solution obtained in the second step with the solution obtained in the third step, stirring by using ultrasonic waves, and stirring by using a planet;
step five, adding a binder: adding 0.16g of KH-570 solution into the solution obtained in the fourth step, stirring with a stirrer, drying the solution, and volatilizing the solvent;
step six, adding a curing agent: adding a curing agent into the solution obtained in the fifth step, wherein the mass ratio of the curing agent to the epoxy resin is 1: 3, stirring with a parallel star, and removing bubbles;
step seven, curing the nano composite material: placing the solution obtained in the step six into a mold, solidifying, cooling and demolding to obtain the graphene epoxy resin nano composite material;
in the first step, 10g of a mixture of graphene, epoxy resin and a curing agent is used; pre-soaking for more than 6 hours, stirring for 30 minutes in a planet way, and rotating speed of 2000 r/min;
and in the second step, stirring for 30 minutes by using ultrasonic waves, wherein the ultrasonic power is 900W, and stirring for 5 minutes by using a planet at the rotating speed of 2000 rpm.
2. The method for preparing the graphene-epoxy resin polymer nanocomposite material according to claim 1, wherein in the third step, the epoxy resin is sufficiently dissolved by ultrasonic stirring for 5 minutes.
3. The method for preparing the graphene-epoxy resin polymer nanocomposite material according to claim 1, wherein in the fourth step, ultrasonic stirring is performed for 30 minutes at a power of 900w, and then planetary stirring is performed for 5 minutes.
4. The preparation method of the graphene epoxy resin polymer nanocomposite material as claimed in claim 1, wherein in the fifth step, the solution is stirred for 5 minutes in a planet way, the solution is placed in a forced air drying oven to volatilize most of the solvent, and then the solution is placed in a vacuum drying oven to continuously volatilize the solvent, wherein the temperature is 90 ℃, and the drying time is 10 hours;
in the sixth step, stirring is carried out for 3 minutes in a planet way, and bubbles are removed for 2 minutes.
5. The method for preparing the graphene-epoxy-resin polymer nanocomposite material as claimed in claim 1, wherein in the seventh step, the solution obtained in the sixth step is poured into a mold, cured at a temperature of 80 ℃ for 2 hours, cured at a temperature of 120 ℃ for 2 hours, and furnace-cooled.
6. The graphene epoxy resin polymer nanocomposite prepared by the preparation method of the graphene epoxy resin polymer nanocomposite as claimed in claim 1.
7. An automotive formulation part prepared using the graphene epoxy polymer nanocomposite material of claim 6.
8. An electronic and electric appliance insulation packaging and functional coating prepared by using the graphene epoxy resin polymer nanocomposite material of claim 6.
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Citations (4)
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| CN102286189A (en) * | 2011-06-24 | 2011-12-21 | 中国科学院理化技术研究所 | Preparation method of graphene oxide/epoxy resin nanocomposite |
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| CN106009514A (en) * | 2016-06-20 | 2016-10-12 | 山东欧铂新材料有限公司 | Preparation method for graphene/epoxy resin composite material |
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| CN102286189A (en) * | 2011-06-24 | 2011-12-21 | 中国科学院理化技术研究所 | Preparation method of graphene oxide/epoxy resin nanocomposite |
| CN104448704A (en) * | 2014-11-14 | 2015-03-25 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of high-toughness carboxylated graphene-epoxy resin composite material |
| CN106009514A (en) * | 2016-06-20 | 2016-10-12 | 山东欧铂新材料有限公司 | Preparation method for graphene/epoxy resin composite material |
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