CN110872380B - graphene/MC nylon nano composite material and preparation method thereof - Google Patents
graphene/MC nylon nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of macromolecules, and particularly relates to a preparation method of a graphene/MC nylon nano composite material. The preparation method comprises the steps of physically stripping a graphite raw material by using a dispersing agent to prepare a graphene dispersion liquid; adding a part of caprolactam into the graphene dispersion liquid for pre-dispersion to obtain a premix; and adding the rest caprolactam into the premix, and carrying out dehydration and anion ring-opening in-situ polymerization reaction to obtain the graphene/MC nylon nanocomposite. The method is simple and easy to operate, and can stably and uniformly disperse the graphene in the MC nylon without surface treatment of the graphene, so that the mechanical, electrical and thermal properties of the graphene/MC nylon nanocomposite are improved. In addition, the preparation method has simple process and no pollution, and can be used for large-scale production.
Description
Technical Field
The invention belongs to the technical field of macromolecules, and particularly relates to a graphene/MC nylon nano composite material and a preparation method thereof.
Background
The cast nylon (MC nylon) is an engineering plastic with excellent performance, has excellent properties of light weight, high strength, wear resistance, fatigue resistance and the like, is low in preparation cost and simple in process, and can replace metal to be widely applied to the fields of machinery, chemical engineering, national defense, medicine and the like. However, MC nylon also has the defects of high water absorption, poor dimensional stability, poor thermal stability, poor heat conductivity and the like, cannot meet the application requirements of certain specific fields, and limits the application range of MC nylon.
Graphene is a novel two-dimensional planar nanomaterial, and its emergence has attracted worldwide attention. Due to the special monoatomic layer structure, the graphene has excellent mechanical, electrical and thermal properties. In addition, the graphene has good wave-absorbing performance and lubricating performance, so that the graphene is very suitable for constructing high-performance polymer-based nano composite materials, is often used as a filling phase and a functional phase of the composite materials, and has important application values in the fields of nano electronic devices, energy storage, aerospace military industry, new energy sources and the like. The graphene is used as a reinforcing phase of the MC nylon, and the mechanical property, the electric conductivity, the heat conductivity and the like of the MC nylon can be improved by virtue of the excellent properties of the graphene. However, graphene has the problems of self-aggregation and non-uniform dispersion in the matrix, which severely limits its application in MC nylon.
At present, a research on enhancing the performance of MC nylon by utilizing graphene is advanced to a certain extent, and Wangchunhua and the like, (RSC adv.,2016) report that sulfonated graphene is used for increasing the heat-conducting performance of an MC nylon composite material, wherein the addition amount is 3 wt%, and the heat-conducting performance is doubled. The friction coefficient and the wear rate of the hydroxyl functionalized graphene/MC nylon composite material prepared by Wangquan and the like (Composites Part B: Engineering, 2017) are respectively reduced by 13 percent and 42.3 percent. . Wangyuxin and the like, (high polymer materials science and engineering, 2016) are compounded with high-density polyethylene modified graphene oxide and MC nylon, the graphene oxide is reduced into graphene in the polymerization process, and the mechanical property and the thermal stability of the prepared composite material are improved simultaneously.
The current research shows that graphene without surface treatment is difficult to disperse uniformly in MC nylon, so how to realize uniform dispersion of graphene in MC nylon by a simple, efficient and easy-to-implement method is a key for improving the performance of MC nylon composite materials.
The present invention has been made in view of this situation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a graphene/MC nylon nano composite material and a preparation method thereof.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a graphene/MC nylon nano composite material comprises the following steps: physically stripping a graphite raw material by using a dispersing agent to prepare a graphene dispersion liquid; adding a part of caprolactam into the graphene dispersion liquid for pre-dispersion to obtain a premix; and adding the rest caprolactam into the premix, and carrying out dehydration and anion ring-opening in-situ polymerization reaction to obtain the graphene/MC nylon nanocomposite.
The graphene dispersion liquid is pre-dispersed with caprolactam and then reacts with caprolactam, so that nano uniform dispersion of graphene in MC nylon is facilitated. The pre-dispersion is physical dispersion, has no influence on the intrinsic structure of the graphene, and is beneficial to the improvement of the overall performance of the composite material.
The method is simple and easy to operate, and can stably and uniformly disperse (achieve nano-scale dispersion) the graphene in the MC nylon without performing surface treatment (such as sulfonation or amination) on the graphene, so that the mechanical, electrical and thermal properties of the graphene/MC nylon nanocomposite are improved. In addition, the preparation process is simple, pollution-free and suitable for large-scale production.
The pre-dispersing means comprises one or more of ultrasonic, high-speed stirring machine, homogenizer, colloid mill grinding, three-roller mill grinding or ball milling.
As an embodiment of the invention, the graphite raw material adopts natural flake graphite with the thickness of a sheet layer of 0.02-0.05 mm or graphite micro-sheets with the thickness of 5-100nm and more than 10 layers.
Preferably, graphite micro-sheets with the number of layers larger than 10 and the thickness of 5-100nm are adopted.
Compared with common graphite, the thickness of the graphite microchip is in the nanoscale range, but the radial width of the graphite microchip can reach several to tens of microns, and the graphite microchip has good heat-conducting property and mechanical property. In addition, under the same stripping condition, the graphite micro-sheets are easier to strip than the graphite flakes, and the obtained graphene has thinner sheet size.
As an embodiment of the present invention, the weight ratio of graphene to caprolactam in the premix is 5: 1-80, preferably 5: 1 to 30.
The weight ratio is selected to facilitate uniform mixing by means of a two-roll, three-roll and/or ball mill mixing, and the like, and sufficient dispersion to allow the premix and the MC nylon to form a nanocomposite of uniform size.
The graphene dispersion liquid comprises graphene, water and a dispersing agent, wherein the weight ratio of the graphene to the dispersing agent is 1: 0.01-30;
further, the weight ratio of the graphene to the dispersing agent is 1: 0.2-20, preferably 1: 0.5-10, and most preferably 1: 1-5.
The final dispersion effect of graphene in nylon is closely related to the ratio of graphene to a dispersant, and the inventor finds that when the amount of the dispersant is small, the graphene is poor in dispersion in a nylon matrix, and when the amount of the dispersant is large, the dispersant influences the polymerization process of MC nylon, and in serious cases, the MC nylon cannot be polymerized.
As an embodiment of the present invention, the dispersant is selected from the group consisting of an aromatic sulfonate formaldehyde condensate, polysulfonic acid calixarenes and derivatives thereof, naphthalene sulfonate formaldehyde condensate, sodium polymethine anthracene sulfonate, polyvinylidene fluoride grafted styrene sulfonic acid ethyl ester, polystyrene sulfonic acid, sodium polystyrene sulfonate, polysulfonyl [4, 8-disubstituted
- (1,2-b:4, 5-b') benzodithiophene ] - [2, 6-substituted bithiophene ] (PBDTTT-S), aromatic poly-thioether ketone, sulfonated poly-p-phenylene ethylene, sulfonated polyaniline or water-soluble propane sulfonic acid aramid fiber.
The dispersing agent can be used as a stripping auxiliary agent to strip graphite raw materials into graphene under certain conditions, can play a role of a compatibilizer, increases interaction between the graphene and MC nylon, enables the graphene to be uniformly dispersed, is beneficial to the mutual overlapping of the graphene to form a heat conduction network chain, effectively transfers heat energy, and improves the thermal conductivity coefficient of the composite material.
As an embodiment of the present invention, the concentration of graphene in the graphene dispersion liquid is not more than 4 wt%, preferably not more than 2 wt%.
The graphene concentration is more than 4 wt%, which is not favorable for dispersion. 4 wt% is already at the edge where dispersion is difficult, and the graphene dispersion is in a slurry state, which is not favorable for keeping the state stable. And the dispersion liquid with the concentration is easier to strip from the graphite raw material. As an embodiment of the present invention, the preparation method of the graphene/MC nylon nanocomposite comprises the following steps:
(1) adding a graphite raw material and a dispersing agent into water according to a certain ratio, and treating by one or more methods of colloid grinding, ultrasound, a high-speed stirrer, a homogenizer, ball milling and two-roller or three-roller grinding to obtain a graphene dispersion liquid;
(2) adding a part of caprolactam into the graphene dispersion liquid, mixing, and performing colloid grinding and ultrasonic treatment for pre-dispersion to obtain a premix;
(3) adding the rest caprolactam into the premix, grinding for a period of time, heating and vacuumizing to constant temperature and constant pressure, adding an alkaline catalyst, continuing heating and vacuumizing to constant temperature and constant pressure, adding a cocatalyst, casting into a preheated mold, preserving heat, cooling and demolding to obtain the graphene/MC nylon nanocomposite.
Another object of the present invention is to provide a graphene/MC nylon nanocomposite obtained by any one of the above preparation methods.
As an embodiment of the present invention, the weight ratio of graphene is not more than 2 wt%, preferably not more than 1 wt%.
During the polymerization of MC nylon, caprolactam is in liquid state in the reaction liquid system, and when the vacuum is pumped, the liquid in the whole device is continuously boiled and reflows for mutual exchange, so that the aim of removing bubbles and water in the system is fulfilled. The addition amount of graphene is increased, the viscosity of a reaction system is increased, the vacuumizing and dewatering effect is poor, and the polymerization reaction is influenced.
As an embodiment of the invention, the thermal conductivity is 0.5-1.5W/mK, and the conductivity is 10-14-10-8S/m, tensile strength of 90-150MPa, bending strength of 100-180MPa, and impact strength of 3.1-5kJ/m2。
The graphene/MC nylon nanocomposite can reduce the wear rate and increase the wear resistance.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention, are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is an SEM image of a graphene/MC nylon nanocomposite prepared in example 1 of the present invention;
FIG. 2 is an enlarged view of a portion of FIG. 1;
FIG. 3 is an SEM image of a graphene/MC nylon nanocomposite prepared in comparative example 1;
fig. 4 is a partially enlarged view of fig. 3.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention are described in detail and completely with reference to some examples, which are only used for illustrating the present invention and are not used for limiting the scope of the present invention.
Example 1
(1) Adding 40g of graphite micro-sheets with the number of layers being more than 10 and the thickness being 5-100nm and 80g of naphthalene sulfonate formaldehyde condensate (FDN) into 880g of water, and carrying out colloid grinding and ultrasonic treatment to obtain 4 wt% of graphene dispersion liquid;
(2) mixing 100g of the graphene dispersion liquid with 20g of caprolactam, grinding for 30min by a colloid mill (the rotating speed is 750r/min), and then carrying out ultrasonic treatment (150W, the frequency is 20000Hz) for 30min to obtain a premix;
(3) adding the rest 376g of caprolactam into the obtained premix, continuously grinding for 10min, transferring the mixture to a three-neck flask, heating, vacuumizing, dehydrating to constant temperature and constant pressure, adding 0.6g of sodium hydroxide serving as a catalyst, continuously heating, vacuumizing, adding 2g of diphenylmethane diisocyanate (MDI) serving as a cocatalyst after constant temperature and constant pressure, finally quickly casting into a preheated mold, preserving heat for 80min, cooling and demolding to obtain the graphene/MC nylon nanocomposite.
The weight ratio of graphene in the obtained graphene/MC nylon nano composite material is 1 wt%, the thermal conductivity of the graphene/MC nylon nano composite material is 1W/m.K, and the conductivity is 10-10S/m, tensile strength 90MPa, bending strength 120MPa, impact strength 4.6kJ/m2。
SEM images of the graphene/MC nylon nanocomposite are shown in fig. 1 and 2, from which it can be seen that the graphene is uniformly distributed, no significant agglomeration occurs and the sheet is thin.
Example 2
(1) Adding 40g of graphite micro-sheets and 0.4g of naphthalene sulfonate formaldehyde condensate (FDN) into 1959.6g of water, and carrying out colloid grinding and ultrasonic treatment to obtain 2 wt% of graphene dispersion liquid;
(2) mixing 100g of the graphene dispersion liquid with 0.4g of caprolactam, grinding for 30min by a colloid mill (the rotating speed is 750r/min), and then carrying out ultrasonic treatment (150W, the frequency is 20000Hz) for 30min to obtain a premix;
(3) adding the rest 397.6g of caprolactam into the obtained premix, continuously grinding for 10min, transferring the mixture into a three-neck flask, heating, vacuumizing, removing water to constant temperature and constant pressure, adding 0.5g of sodium hydroxide serving as a catalyst, continuously heating, vacuumizing, adding 2.2g of diphenylmethane diisocyanate (MDI) serving as a cocatalyst after constant temperature and constant pressure, finally quickly casting into a preheated mold, preserving heat for 80min, cooling, and demolding to obtain the graphene/MC nylon nanocomposite.
The weight ratio of graphene in the obtained graphene/MC nylon nano composite material is 0.5 wt%, the thermal conductivity of the graphene/MC nylon nano composite material is 0.8W/m.K, and the conductivity is 10-12S/m, tensile strength of 80MPa, bending strength of 100MPa, and impact strength of 3.7kJ/m2。
The SEM image of the graphene/MC nylon nanocomposite is similar to that of example 1, the graphene is uniformly distributed, no obvious agglomeration exists, and the sheet layer is thin.
Example 3
(1) Adding 4g of graphite micro-sheets and 120g of naphthalene sulfonate formaldehyde condensate (FDN) into 876g of water (the weight ratio of graphene to a dispersing agent is controlled to be 1:30), and carrying out colloid grinding and ultrasonic treatment to obtain 0.4 wt% of graphene dispersion liquid;
(2) mixing 100g of the graphene dispersion liquid with 6.4g of caprolactam, grinding for 30min by a colloid mill (the rotating speed is 750r/min), and then carrying out ultrasonic treatment (150W, the frequency is 20000Hz) for 30min to obtain a premix;
(3) adding the rest 393.2g of caprolactam into the obtained premix, continuously grinding for 10min, transferring the mixture to a three-neck flask, heating, vacuumizing, removing water to constant temperature and constant pressure, adding 0.5g of sodium hydroxide serving as a catalyst, continuously heating, vacuumizing, adding 2.2g of diphenylmethane diisocyanate (MDI) serving as a cocatalyst after constant temperature and constant pressure, finally quickly casting into a preheated mold, preserving heat for 80min, cooling, and demolding to obtain the graphene/MC nylon nanocomposite.
The weight ratio of graphene in the obtained graphene/MC nylon nano composite material is 0.1 wt%, the thermal conductivity of the graphene/MC nylon nano composite material is 0.4W/m.K, and the conductivity is 10-14S/m, tensile strength of 75MPa, bending strength of 95MPa, and impact strength of 3.4kJ/m2。
The SEM image of the graphene/MC nylon nanocomposite is similar to that of example 1, the graphene is uniformly distributed, no obvious agglomeration exists, and the sheet layer is thin.
Example 4
(1) Adding 4g of graphite microchip and 80g of sulfonated poly-p-phenylene ethylene and naphthalene sulfonate formaldehyde condensate (FDN) into 916g of water (the weight ratio of graphene to a dispersing agent is controlled to be 1:20), and carrying out colloid grinding and ultrasonic treatment to obtain 0.4 wt% of graphene dispersion liquid;
(2) mixing 100g of the graphene dispersion liquid with 2.4g of caprolactam, grinding for 30min by a colloid mill (the rotating speed is 750r/min), and then carrying out ultrasonic treatment (150W, the frequency is 20000Hz) for 30min to obtain a premix;
(3) adding the rest 397.2g of caprolactam into the obtained premix, continuously grinding for 10min, transferring the mixture into a three-neck flask, heating, vacuumizing, removing water to constant temperature and constant pressure, adding 0.5g of sodium hydroxide serving as a catalyst, continuously heating, vacuumizing, adding 2.2g of diphenylmethane diisocyanate (MDI) serving as a cocatalyst after constant temperature and constant pressure, finally quickly casting into a preheated mold, preserving heat for 80min, cooling, and demolding to obtain the graphene/MC nylon nanocomposite.
The weight ratio of graphene in the obtained graphene/MC nylon nano composite material is 0.1 wt%, the thermal conductivity of the graphene/MC nylon nano composite material is 0.45W/m.K, and the conductivity is 10-14S/m, tensile strength of 80MPa, bending strength of 100MPa, and impact strength of 3.6kJ/m2。
The SEM image of the graphene/MC nylon nanocomposite is similar to that of example 1, the graphene is uniformly distributed, no obvious agglomeration exists, and the sheet layer is thin.
Example 5
(1) Adding 40g of graphite micro-sheets and 400g of naphthalene sulfonate formaldehyde condensate (FDN) into 1560g of water (the weight ratio of graphene to the dispersing agent is controlled to be 1:10), and carrying out colloid grinding and ultrasonic treatment to obtain 2 wt% of graphene dispersion liquid;
(2) mixing 200g of the graphene dispersion liquid with 16.8g of caprolactam, grinding for 30min by a colloid mill (the rotating speed is 750r/min), and then carrying out ultrasonic treatment (150W, the frequency is 20000Hz) for 30min to obtain a premix;
(3) adding the rest 379.2g of caprolactam into the obtained premix, continuously grinding for 10min, transferring the mixture into a three-neck flask, heating, vacuumizing, removing water to constant temperature and constant pressure, adding 0.6g of sodium hydroxide serving as a catalyst, continuously heating, vacuumizing, adding 2g of diphenylmethane diisocyanate (MDI) serving as a cocatalyst after constant temperature and constant pressure, finally quickly casting into a preheated mold, preserving heat for 80min, cooling and demolding to obtain the graphene/MC nylon nanocomposite.
The weight ratio of graphene in the obtained graphene/MC nylon nano composite material is 1 wt%, the thermal conductivity of the graphene/MC nylon nano composite material is 1.2W/m.K, and the conductivity is 10-9S/m, tensile strength 95MPa, bending strength 130MPa, impact strength 5kJ/m2。
The SEM image of the graphene/MC nylon nanocomposite is similar to that of example 1, the graphene is uniformly distributed, no obvious agglomeration exists, and the sheet layer is thin.
Example 6
(1) Adding 40g of graphite microchip and 200g of poly sulfonyl [4, 8-disubstituted- (1,2-b:4, 5-b') benzodithiophene ] - [2, 6-substituted bithiophene ] (PBDTTT-S) into 1760g of water (the weight ratio of graphene to a dispersing agent is controlled to be 1:5), and carrying out colloid grinding and ultrasonic treatment to obtain 2 wt% of graphene dispersion liquid;
(2) mixing 200g of the graphene dispersion liquid with 13.6g of caprolactam, grinding for 30min by a colloid mill (the rotating speed is 750r/min), and then carrying out ultrasonic treatment (150W, the frequency is 20000Hz) for 30min to obtain a premix;
(3) adding the remaining 382.4g of caprolactam into the obtained premix, continuously grinding for 10min, transferring the mixture into a three-neck flask, heating, vacuumizing, removing water to constant temperature and constant pressure, adding 0.6g of sodium hydroxide serving as a catalyst, continuously heating, vacuumizing, adding 2g of diphenylmethane diisocyanate (MDI) serving as a cocatalyst after constant temperature and constant pressure, finally quickly casting into a preheated mold, preserving heat for 80min, cooling, and demolding to obtain the graphene/MC nylon nanocomposite.
The weight ratio of graphene in the obtained graphene/MC nylon nano composite material is 1 wt%, the thermal conductivity of the graphene/MC nylon nano composite material is 1.5W/m.K, and the conductivity is 10-8S/m, tensile strength 100MPa, bending strength 140MPa, impact strength 5.1kJ/m2。
The SEM image of the graphene/MC nylon nanocomposite is similar to that of example 1, the graphene is uniformly distributed, no obvious agglomeration exists, and the sheet layer is thin.
Example 7
(1) Adding 40g of graphite micro-sheets and 8g of aromatic sulfonate formaldehyde condensate into 1952g of water (the weight ratio of graphene to the dispersing agent is controlled to be 1:0.2), and carrying out colloid grinding and ultrasonic treatment to obtain 2 wt% of graphene dispersion liquid;
(2) mixing 100g of the graphene dispersion liquid with 4.4g of caprolactam, grinding for 30min by a colloid mill (the rotating speed is 750r/min), and then carrying out ultrasonic treatment (150W, the frequency is 20000Hz) for 30min to obtain a premix;
(3) adding the remaining 393.6g of caprolactam into the obtained premix, continuously grinding for 10min, transferring the mixture into a three-neck flask, heating, vacuumizing, removing water to constant temperature and constant pressure, adding 0.6g of sodium hydroxide serving as a catalyst, continuously heating, vacuumizing, adding 2g of diphenylmethane diisocyanate (MDI) serving as a cocatalyst after constant temperature and constant pressure, finally quickly casting into a preheated mold, preserving heat for 80min, cooling, and demolding to obtain the graphene/MC nylon nanocomposite.
The weight ratio of graphene in the obtained graphene/MC nylon nano composite material is 0.5 wt%, the thermal conductivity of the graphene/MC nylon nano composite material is 0.8W/m.K, and the conductivity is 10-11S/m, tensile strength 85MPa, bending strength 118MPa, impact strength 3.8kJ/m2。
The SEM image of the graphene/MC nylon nanocomposite is similar to that of example 1, the graphene is uniformly distributed, no obvious agglomeration exists, and the sheet layer is thin.
Comparative example 1
This comparative example differs from example 1 in that the graphene dispersion was not pre-dispersed with caprolactam.
(1) Adding graphite micro-sheets and a naphthalene sulfonate formaldehyde condensate (FDN) into water according to a certain proportion, and carrying out colloid grinding and ultrasonic treatment to obtain a 4 wt% graphene dispersion liquid;
(2) mixing 100g of the graphene dispersion liquid with 396g of caprolactam, grinding for 40min by a colloid mill (the rotation speed is 750r/min), then carrying out ultrasonic treatment (150W, the frequency is 20000Hz) for 30min, transferring the mixture to a three-neck flask, heating, vacuumizing, removing water to a constant temperature and a constant pressure, adding 0.6g of sodium hydroxide serving as a catalyst, continuing heating, vacuumizing, adding 2g of diphenylmethane diisocyanate (MDI) serving as a cocatalyst after the constant temperature and the constant pressure, finally quickly casting into a preheated mold, carrying out heat preservation for 80min, cooling, and demolding to obtain the graphene/MC nylon nanocomposite.
The thermal conductivity of the obtained graphene/MC nylon nano composite material is 0.2W/m.K, and the conductivity is 0.2 multiplied by 10- 10S/m, tensile strength 65MPa, bending strength 91MPa, impact strength 3.3kJ/m2. Referring to fig. 3 and 4, SEM images of the graphene/MC nylon nanocomposite show that graphene is unevenly distributed, and is seriously agglomerated, thick in sheet layer and numerous in layer number.
Comparative example 1 differs from example 1 only in that the graphene dispersion liquid and a part of caprolactam are not pre-dispersed, other steps and parameters are consistent, but the thermal, electrical and mechanical properties of the obtained graphene/MC nylon nanocomposite are poor, and the dispersion effect is poor as can be seen from the SEM image.
Comparative examples 2 to 3
The differences between the comparative examples 2-3 and the example 1 are that the used graphite raw material is not graphite micro-sheets, but is the same, and the relevant performance parameters of the graphite raw material in each comparative example and the obtained graphene/MC nylon nano composite material are shown in the following table.
TABLE 1
According to the numerical values in the table, the comparative examples 2-3 do not adopt the graphite microchip of the invention, and the electrical, thermal and mechanical properties of the corresponding graphene/MC nylon nano composite material are relatively poor.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (12)
1. A preparation method of a graphene/MC nylon nano composite material is characterized in that a dispersing agent is used for physically stripping a graphite raw material to prepare a graphene dispersion liquid; adding a part of caprolactam into the graphene dispersion liquid for pre-dispersion to obtain a premix; adding the rest caprolactam into the premix, and carrying out dehydration and anion ring-opening in-situ polymerization reaction to obtain the graphene/MC nylon nanocomposite;
comprises the following steps:
(1) adding a graphite raw material and a dispersing agent into water according to a certain ratio, and carrying out colloid grinding and ultrasonic treatment to obtain a graphene dispersion liquid;
(2) adding a part of caprolactam into the graphene dispersion liquid, mixing, and pre-dispersing the mixture by one or more methods of colloid grinding, ultrasonic treatment, a high-speed stirrer, a homogenizer, ball milling and two-roller or three-roller grinding to obtain a premix;
(3) adding the rest caprolactam into the premix, grinding for a period of time, heating and vacuumizing to constant temperature and constant pressure, adding an alkaline catalyst, continuing heating and vacuumizing to constant temperature and constant pressure, adding a cocatalyst, casting into a preheated mold, preserving heat, cooling and demolding to obtain the graphene/MC nylon nanocomposite;
the weight ratio of graphene to caprolactam in the premix is 5: 1-80;
the dispersing agent is selected from one or more of aromatic sulfonate formaldehyde condensate, polysulfonic acid calixarene and derivatives thereof, naphthalene sulfonate formaldehyde condensate, polymethine anthracene sodium sulfonate, polyvinylidene fluoride grafted styrene sulfonic acid, polyvinylidene fluoride grafted styrene ethyl sulfonate, polystyrene sulfonic acid, polystyrene sodium sulfonate, polysulfonyl [4, 8-disubstituted- (1,2-b:4, 5-b') benzodithiophene ] - [2, 6-substituted benzothiophene ], aromatic poly-thioether ketone, sulfonated poly-p-phenylene ethylene, sulfonated polyaniline or water-soluble propane sulfonic acid aramid;
the concentration of graphene in the graphene dispersion liquid is not more than 4 wt%.
2. The preparation method of claim 1, wherein the graphite raw material is natural flake graphite with a flake thickness of 0.02-0.05 mm or/and graphite micro-flakes with a layer number of more than 10 and a thickness of 5-100 nm.
3. The method according to claim 1 or 2, wherein the weight ratio of graphene to caprolactam in the premix is 5: 1 to 30.
4. The preparation method of claim 3, wherein the graphene dispersion liquid comprises graphene, water and a dispersing agent, and the weight ratio of the graphene to the dispersing agent is 1: 0.01-30.
5. The preparation method according to claim 4, wherein the weight ratio of the graphene to the dispersing agent is 1: 0.2-20.
6. The preparation method according to claim 4, wherein the weight ratio of the graphene to the dispersing agent is 1: 0.5-10.
7. The preparation method according to claim 4, wherein the weight ratio of the graphene to the dispersing agent is 1: 1-5.
8. The production method according to any one of claims 4 to 7, wherein the concentration of graphene in the graphene dispersion liquid is not more than 2 wt%.
9. graphene/MC nylon nanocomposite obtained by the preparation method according to any one of claims 1 to 8.
10. The graphene/MC nylon nanocomposite of claim 9, wherein the weight proportion of graphene is no greater than 2 wt%.
11. The graphene/MC nylon nanocomposite of claim 10, wherein the weight proportion of graphene is no greater than 1 wt%.
12. The graphene/MC nylon nanocomposite as claimed in claim 10 or 11, wherein the thermal conductivity is 0.5-1.5W/m.K, and the electrical conductivity is 10-14-10-8S/m, tensile strength of 90-150MPa, bending strength of 100-180MPa, and impact strength of 3.1-5kJ/m2。
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