CN113549299A - Preparation method of high-wear-resistance and high-toughness graphene nanosheet/epoxy resin composite material - Google Patents
Preparation method of high-wear-resistance and high-toughness graphene nanosheet/epoxy resin composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a graphene nanosheet/epoxy resin composite material with high wear resistance and high toughness. The organic silicon and polyether flexible chain structure in the epoxy-terminated polyether polysiloxane block structure and graphene synergistically toughen the epoxy resin, and the self-lubricating effect of the graphene obviously improves the wear resistance of the epoxy resin, so that the high-wear-resistance and high-toughness graphene nanosheet/epoxy resin composite material is prepared, and the high wear resistance, high toughness and excellent comprehensive performance of the composite material enable the composite material to have great market application value in the fields of grinding and polishing, packaging and transportation, electronic and electric appliances, aerospace and the like.
Description
Technical Field
The invention belongs to the field of polymer composite materials, and particularly relates to a preparation method of a graphene nanosheet/epoxy resin composite material with high wear resistance and high toughness.
Background
Due to good comprehensive performance, the epoxy resin is widely applied to the fields of electronic packaging, building construction, aerospace and the like. However, the epoxy resin still has some disadvantages in use, such as insufficient mechanical strength, toughness, wear resistance, heat conductivity, etc., which limits its application in various fields. Therefore, the reinforced modification of the epoxy resin is of great significance.
Graphene is considered to be a good filler for improving mechanical properties, wear resistance, flame retardance, heat conduction and electric conduction of high polymer materials due to a two-dimensional nano-layered structure and excellent comprehensive properties (Kim, et al macromolecules 2010,43, 6515-166530; Papageorgiouo, et al prog, Mater, Sci.2017,90, 75-127; Liang, et al, J.Mater, chem.C 2019,7, 2725-2733; Liushu, Sunju, and the like. However, the application of graphene in polymer modification still has a bottleneck to be solved urgently. On one hand, graphene sheets have strong van der waals force between layers, and are difficult to peel off in a high-molecular matrix by using a traditional dispersion method, and are dispersed in a form of single sheets and easy to agglomerate, so that the modification effect of the graphene sheets is reduced. For better dispersion effect, organic solvent is often adopted for dilution and dispersion (Yan red strong, Fangzhui, etc. a preparation method of graphene nanoplatelets/epoxy resin nanocomposite, CN 103396653A; Songhe river, Marmokun, etc. a preparation method of graphene epoxy resin composite, CN 103408895A). However, the introduction of organic solvent not only makes the preparation process complicated and increases energy consumption, but also pollutes environment. Secondly, due to the relative chemical inertness of the surface structure of graphene, the interaction force between graphene and macromolecules is weak, and the modification efficiency of graphene in the aspects of macromolecule mechanical property and heat conduction and electricity conduction is influenced. Therefore, before the graphene modified polymer material is used, the graphene is generally subjected to surface modification treatment (Toulongcheng, Wanyanjun, and the like, a preparation method of a functionalized graphene oxide/epoxy resin composite material, CN103627139AA, Rankine lacquer, Zhaoyuan, and the like, a thermal interface material of surface modified graphene-carbon nitride-epoxy resin and a preparation method thereof, CN 109337291A). However, the chemical surface modification process of graphene is complicated, the operation is complex, the industrial production is difficult, and a strong oxidant and an organic solvent are often used, so that the environment is polluted. Meanwhile, surface chemical modification can destroy the graphitized structure of graphene, so that excellent performances of graphene in the aspects of mechanics, heat conduction and electric conduction are reduced, while a modifier in a physical non-covalent bond modification method is high in cost, and the performance of epoxy resin is reduced by adding the modifier. Therefore, the good graphene dispersing agent and surface modifier are found to have great value for the application of graphene in the modification of high polymer materials.
Sundao 38495and the like utilize a block copolymer, i.e., isobutylene-b-propylene ethanol-b-isobutylene, as a dispersant to achieve good dispersion of graphene in an oily solvent (sundao 38495, litdan, a slurry and a preparation method and application thereof, CN 110484020A). Limeitai and the like adopt a polyether-polystyrene and other block copolymers as a dispersing agent to prepare a graphene solution (limeitai, sunzurchi, and the like, the block copolymers and a method for preparing graphene by using the block copolymers, CN107182213B) with good dispersion. The block copolymer has obvious toughening effect on epoxy resin (Huang Yajiang, Tang Dynasty, and the like, a reinforcing toughening agent, a toughened epoxy resin composite material and a preparation method thereof, CN107459612B, and amphiphilic block copolymer and inorganic nano filler for reinforcing the performance of thermosetting polymer, CN 101772546B).
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a graphene nanosheet/epoxy resin composite material with high wear resistance and high toughness, the preparation method adopts a commercially available liquid fabric finishing agent, namely epoxy-terminated polyether polysiloxane, as a dispersing agent, and an organic silicon-oxygen chain in the structure of the polyether polysiloxane has strong interaction with a graphitized structure in graphene and can be used as a dispersing agent and a surface modifier of the graphene. Meanwhile, epoxy-terminated polyether can participate in epoxy resin curing, so that graphene and epoxy resin have strong interface interaction force. Therefore, the epoxy-terminated polyether polysiloxane and the graphene synergistically reinforce the modified epoxy resin.
In order to achieve the above purpose, the solution of the invention is:
a preparation method of a graphene nanosheet/epoxy resin composite material with high wear resistance and high toughness comprises the following steps:
1) adding graphite powder into epoxy-terminated polyether polysiloxane according to a certain mass ratio, and filling the mixture into a ball milling tank for ball milling to obtain graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry.
2) The above steps are carried out. And mixing the graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry with a certain amount of curing agent and epoxy resin, and stirring at a high speed for 30 minutes to obtain an epoxy resin mixture.
3) And vacuumizing the epoxy resin mixture, removing bubbles, pouring into a mold, and carrying out curing reaction to prepare the graphene nanosheet/epoxy resin composite material with high wear resistance and high toughness.
The mesh number of the graphite powder is 300-5000 meshes.
The epoxy-terminated polyether polysiloxane is colorless transparent or light yellow transparent liquid, and the viscosity is 100-3000 cP.
The midblock in the structure of the epoxy-terminated polyether polysiloxane is one or more copolymers of polydimethylsiloxane, polymethylphenylsiloxane and polydiphenylsiloxane. The molecular weight of the midblock is 500-5000 g/mol.
Two side blocks in the epoxy terminated polyether polysiloxane structure are one or two copolymers of polyoxyethylene ether and polyoxyethylene oxypropylene ether. The molecular weight of the two-side block is 500-10000 g/mol.
The end group in the epoxy terminated polyether polysiloxane structure is an epoxy group.
The mass ratio of the graphite powder to the epoxy-terminated polyether polysiloxane is 1: (3-200).
The ball milling equipment is a planetary ball mill, the grinding balls are zirconium dioxide balls, the ball milling rotating speed is 100-1000 rpm, and the ball milling time is 2-6 hours.
The epoxy resin is liquid epoxy resin, and specifically is one or a combination of more of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, alicyclic epoxy resin, heterocyclic epoxy resin and aliphatic epoxy resin.
The curing agent is one or a combination of several of polyether amine, aliphatic amine, alicyclic amine, aromatic amine, methylhexahydrophthalic anhydride, methyltetrahydrophthalic anhydride, methylnadic anhydride and polythiol.
The epoxy resin composite material comprises the following components in percentage by mass: epoxy resin: 100 parts by mass; graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry: 5-100 parts by mass; a curing agent; 10 to 120 parts by mass.
The curing process comprises the step-by-step heating curing, wherein the curing temperature of the first stage is 20-140 ℃, and the curing time is 30-90 minutes; the curing temperature of the second stage is 60-180 ℃, and the time is 60-300 minutes.
After the technical scheme is adopted, the invention has the following beneficial effects: 1) the invention adopts a commercial block copolymer-epoxy terminated polyether polysiloxane, wherein an organic silicon oxygen chain in the structure has strong interaction with a graphitized structure in graphene, and the block copolymer-epoxy terminated polyether polysiloxane can be used as a dispersing agent and a surface modifier of the graphene. Meanwhile, epoxy-terminated polyether can participate in epoxy resin curing, so that epoxy-terminated polyether polysiloxane modified graphene can be uniformly dispersed in epoxy resin and has strong interfacial interaction force with the epoxy resin. 2) The epoxy-terminated polyether polysiloxane is a block copolymer with high flexibility, has an obvious toughening effect on epoxy resin, and can be used for toughening the epoxy resin together with graphene. 3) The preparation method disclosed by the invention is simple in process, free of organic solvent, green and environment-friendly, and can meet the requirements of industrial production; 4) the epoxy resin composite material prepared by the invention not only has high wear resistance and high toughness, but also has other excellent performances such as heat conduction and the like, and has great application value in the fields of electronic packaging, building construction, aerospace and the like.
Drawings
FIG. 1 shows the chemical structure of epoxy-terminated polyether polysiloxane.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
Example 1
500-mesh graphite powder and epoxy terminated polyether polysiloxane (polydimethylsiloxane chain segment: 1000g/mol, epoxy polyether chain segment: 500g/mol) are mixed according to the mass ratio of 1: 199, and filling the mixture into a ball milling tank to perform ball milling for 2 hours at the rotating speed of 500rpm to prepare the graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry. Then, 20g of the mixed slurry was mixed with 100g of bisphenol A epoxy resin (bisphenol A glycidyl ether), 85g of methyl hexahydrophthalic anhydride as a curing agent and 1.5g of 2, 4, 6-tris (dimethylaminomethyl) phenol as parts by mass, and stirred at a high speed for 30 minutes to obtain a black slurry epoxy resin mixture. A black paste epoxy resin mixture was obtained. And putting the mixture into an oven, vacuumizing for 10 minutes, removing bubbles introduced by stirring, pouring into a mold, and carrying out a curing reaction. The curing conditions were: curing for 60 minutes at 120 ℃, heating to 140 ℃ and curing for 4 hours to obtain the graphene nanosheet/epoxy resin composite material.
Example 2
Mixing 800-mesh graphite powder and epoxy terminated polyether polysiloxane (polydimethylsiloxane chain segment: 2000g/mol, epoxy polyether chain segment: 500g/mol) according to a mass ratio of 1: 99, and filling the mixture into a ball milling tank to perform ball milling for 4 hours at the rotating speed of 800rpm to prepare the graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry. Then, 10g of the mixed slurry was mixed with 100g of bisphenol A epoxy resin (bisphenol A glycidyl ether), 85g of methyl hexahydrophthalic anhydride as a curing agent and 1.5g of 2, 4, 6-tris (dimethylaminomethyl) phenol as parts by mass, and stirred at high speed for 30 minutes to obtain a black slurry epoxy resin mixture. A black paste epoxy resin mixture was obtained. And putting the mixture into an oven, vacuumizing for 10 minutes, removing bubbles introduced by stirring, pouring into a mold, and carrying out a curing reaction. The curing conditions were: curing for 60 minutes at 120 ℃, heating to 140 ℃ and curing for 4 hours to obtain the graphene nanosheet/epoxy resin composite material.
Example 3
1500-mesh graphite powder and epoxy terminated polyether polysiloxane (polydimethylsiloxane chain segment: 3000g/mol, epoxy polyether chain segment: 500g/mol) are mixed according to the mass ratio of 1: 19, mixing, and ball-milling in a ball-milling tank at the rotating speed of 600rpm for 5 hours to prepare the graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry. Then, 10g of the mixed slurry was mixed with 100g of bisphenol A epoxy resin (bisphenol A glycidyl ether), 85g of methyl hexahydrophthalic anhydride as a curing agent and 1.5g of 2, 4, 6-tris (dimethylaminomethyl) phenol as parts by mass, and stirred at high speed for 30 minutes to obtain a black slurry epoxy resin mixture. A black paste epoxy resin mixture was obtained. And putting the mixture into an oven, vacuumizing for 10 minutes, removing bubbles introduced by stirring, pouring into a mold, and carrying out a curing reaction. The curing conditions were: curing for 60 minutes at 120 ℃, heating to 140 ℃ and curing for 4 hours to obtain the graphene nanosheet/epoxy resin composite material.
Example 4
3000-mesh graphite powder and epoxy terminated polyether polysiloxane (polydimethylsiloxane chain segment: 2000g/mol, epoxy polyether chain segment: 500g/mol) are mixed according to the mass ratio of 1: 9, mixing, and putting the mixture into a ball milling tank to perform ball milling for 6 hours at the rotating speed of 1000rpm to prepare the graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry. Then, 10g of the mixed slurry was mixed with 100g of bisphenol A epoxy resin (bisphenol A glycidyl ether), 85g of methyl hexahydrophthalic anhydride as a curing agent and 1.5g of 2, 4, 6-tris (dimethylaminomethyl) phenol as parts by mass, and stirred at high speed for 30 minutes to obtain a black slurry epoxy resin mixture. A black paste epoxy resin mixture was obtained. And putting the mixture into an oven, vacuumizing for 10 minutes, removing bubbles introduced by stirring, pouring into a mold, and carrying out a curing reaction. The curing conditions were: curing for 60 minutes at 120 ℃, heating to 140 ℃ and curing for 4 hours to obtain the graphene nanosheet/epoxy resin composite material.
Comparative example 1
1g of 3000-mesh graphite powder was added to 100g of bisphenol A epoxy resin (bisphenol A glycidyl ether), and the mixture was uniformly mixed, then 85g of a curing agent methylhexahydrophthalic anhydride and 1.5g of 2, 4, 6-tris (dimethylaminomethyl) phenol by mass were added and mixed, and the mixture was stirred at high speed for 30 minutes to obtain a black slurry epoxy resin mixture. A black paste epoxy resin mixture was obtained. And putting the mixture into an oven, vacuumizing for 10 minutes, removing bubbles introduced by stirring, pouring into a mold, and carrying out a curing reaction. The curing conditions were: curing for 60 minutes at 120 ℃, heating to 140 ℃ and curing for 4 hours to prepare the epoxy resin composite material.
Comparative example 2
100g of bisphenol A epoxy resin (bisphenol A glycidyl ether), 85g of a curing agent methylhexahydrophthalic anhydride and 1.5g of 2, 4, 6-tris (dimethylaminomethyl) phenol by mass were mixed and stirred at high speed for 30 minutes to obtain a black slurry epoxy resin mixture. A black paste epoxy resin mixture was obtained. And putting the mixture into an oven, vacuumizing for 10 minutes, removing bubbles introduced by stirring, pouring into a mold, and carrying out a curing reaction. The curing conditions were: curing for 60 minutes at 120 ℃, heating to 140 ℃ and curing for 4 hours to prepare the epoxy resin composite material.
In order to better illustrate the effects of the present invention, samples of examples and comparative examples were tested. The impact strength test is carried out according to the ASTM D6110-2017 standard, the abrasion resistance test is carried out according to the ASTM G9905 standard, and the thermal conductivity test is carried out according to the ASTM D5930-2017 standard. As can be seen from Table 1, the epoxy-terminated polyether polysiloxane and the carbon nanotubes cooperate to significantly improve the impact strength of the epoxy resin, which indicates that the toughness of the epoxy resin is significantly improved. Meanwhile, the wear resistance and the heat conductivity of the epoxy resin are improved. Therefore, the graphene nanosheet/epoxy resin composite material prepared by the method disclosed by the invention has the advantages of high wear resistance, high toughness and excellent comprehensive performance.
Table 1 results of performance testing
The above embodiments are not intended to limit the form and style of the present invention, and any suitable changes or modifications may be made by one of ordinary skill in the art without departing from the present invention.
Claims (10)
1. The preparation method of the graphene nanosheet/epoxy resin composite material with high wear resistance and high toughness is characterized by comprising the following steps of: the method comprises the following steps:
1) adding graphite powder into epoxy-terminated polyether polysiloxane, and filling the mixture into ball milling equipment for ball milling to prepare graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry;
2) mixing the graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry with a curing agent and epoxy resin, and stirring to obtain an epoxy resin mixture;
3) and vacuumizing the epoxy resin mixture, removing bubbles, pouring into a mold, and carrying out curing reaction to prepare the graphene nanosheet/epoxy resin composite material with high wear resistance and high toughness.
2. The preparation method of the high wear-resistant and high toughness graphene nanoplatelet/epoxy composite material according to claim 1, characterized in that: the mesh number of the graphite powder is 300-5000 meshes, and the viscosity of the epoxy-terminated polyether polysiloxane is 100-3000 cP.
3. The preparation method of the high wear-resistant and high toughness graphene nanoplatelet/epoxy composite material according to claim 1, characterized in that: in the structure of the epoxy-terminated polyether polysiloxane, the midblock is one or more copolymers of polydimethylsiloxane, polymethylphenylsiloxane and polydiphenylsiloxane, and the molecular weight of the midblock is 500-5000 g/mol;
the two-side block is one or two copolymers of polyoxyethylene ether and polyoxyethylene oxypropylene ether, and the molecular weight of the two-side block is 500-10000 g/mol;
the end group is an epoxy group.
4. The preparation method of the high wear-resistant and high toughness graphene nanoplatelet/epoxy composite material according to claim 1, characterized in that: the mass ratio of the graphite powder to the epoxy-terminated polyether polysiloxane is 1: 3 to 200.
5. The preparation method of the high wear-resistant and high toughness graphene nanoplatelet/epoxy composite material according to claim 1, characterized in that: the ball milling equipment is a planetary ball mill, the grinding balls are zirconium dioxide balls, the ball milling rotating speed is 100-1000 rpm, and the ball milling time is 2-6 hours.
6. The preparation method of the high wear-resistant and high toughness graphene nanoplatelet/epoxy composite material according to claim 1, characterized in that: the epoxy resin is liquid epoxy resin, and specifically is one or a combination of more of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, alicyclic epoxy resin, heterocyclic epoxy resin and aliphatic epoxy resin.
7. The preparation method of the high wear-resistant and high toughness graphene nanoplatelet/epoxy composite material according to claim 1, characterized in that: the curing agent is one or a combination of several of polyether amine, aliphatic amine, alicyclic amine, aromatic amine, methylhexahydrophthalic anhydride, methyltetrahydrophthalic anhydride, methylnadic anhydride and polythiol.
8. The preparation method of the high wear-resistant and high toughness graphene nanoplatelet/epoxy composite material according to claim 1, characterized in that: the components in the step 2) are as follows in parts by mass: epoxy resin: 100 parts by mass; graphene nanosheet/epoxy-terminated polyether polysiloxane mixed slurry: 5-100 parts by mass; a curing agent; 10 to 120 parts by mass.
9. The preparation method of the high wear-resistant and high toughness graphene nanoplatelet/epoxy composite material according to claim 1, characterized in that: the curing reaction is heating curing step by step, the curing temperature of the first stage is 20-140 ℃, and the curing time is 30-90 minutes; the curing temperature of the second stage is 60-180 ℃, and the time is 60-300 minutes.
10. The graphene nanosheet/epoxy resin composite material with high wear resistance and high toughness, which is obtained by the preparation method according to any one of claims 1 to 9.
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Cited By (4)
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| CN113881051A (en) * | 2021-11-05 | 2022-01-04 | 无锡东润电子材料科技有限公司 | Preparation method and application of multifunctional toughening agent for epoxy resin |
| CN115197540A (en) * | 2022-08-01 | 2022-10-18 | 哈尔滨工业大学（深圳） | Preparation method of modified epoxy composite material suitable for marine environment and product |
| CN116284655A (en) * | 2023-01-10 | 2023-06-23 | 中威北化科技有限公司 | Preparation method of graphene-organosilicon synergistically-reinforced polyurethane grafted modified epoxy resin |
| WO2023197698A1 (en) * | 2022-04-14 | 2023-10-19 | 华南理工大学 | Heat-conduction-enhanced phase-change nanocapsule composite material, and preparation method therefor and use thereof |
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| CN115197540A (en) * | 2022-08-01 | 2022-10-18 | 哈尔滨工业大学（深圳） | Preparation method of modified epoxy composite material suitable for marine environment and product |
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| CN116284655A (en) * | 2023-01-10 | 2023-06-23 | 中威北化科技有限公司 | Preparation method of graphene-organosilicon synergistically-reinforced polyurethane grafted modified epoxy resin |
| CN116284655B (en) * | 2023-01-10 | 2024-01-09 | 中威北化科技有限公司 | Preparation method of graphene-organosilicon synergistically-reinforced polyurethane grafted modified epoxy resin |
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