CN109912924B - Preparation and application method of graphene-nano polytetrafluoroethylene composite modified filler - Google Patents
Preparation and application method of graphene-nano polytetrafluoroethylene composite modified filler Download PDFInfo
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Abstract
The invention discloses a preparation method and an application method of a graphene-nano polytetrafluoroethylene composite modified filler, wherein the modified graphene is compounded with a nanosphere polytetrafluoroethylene filler, and simultaneously, a spray drying method is adopted to uniformly compound the nanosphere polytetrafluoroethylene filler and a flake graphene filler by using a binder, so that the prepared composite filler has the wear resistance of the graphene and the lubricating property of the nano polytetrafluoroethylene.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a preparation method and an application method of a graphene-nano polytetrafluoroethylene composite modified filler.
Background
With the development of science and technology and the development of industry, at present, automation equipment is applied more and various industries, the automation process cannot leave the operation and action of a mechanical part mechanism, and the mechanical part inevitably generates friction and abrasion in the operation process. Research indicates that the friction consumes more than 1/3 primary energy sources in the world, and 60% of mechanical parts are damaged due to abrasion, so that the research on the wear-resistant lubricating composite material has important practical significance, and the development of the abrasion-reducing and friction-reducing filler is particularly critical. The friction reducing and reducing material is always a key research object in the field of tribology, and is mainly used for processing into transmission parts in actual industry and life; the friction reduction means that the service life of the part is prolonged, the resource utilization rate is improved, and the friction reduction means that energy is saved and the energy loss is reduced. The high molecular polymer material can be conveniently processed into various shapes by virtue of the excellent plasticity and has incomparable advantages compared with the traditional metal in some aspects.
At present, the friction reducing filler in the polymer is mainly limited to some traditional fillers, such as graphite, molybdenum disulfide, polytetrafluoroethylene and the like. These conventional fillers can improve some tribological properties of the polymeric material to a certain extent, but their improvement is rather limited and they require a large amount of filling, which causes a significant reduction in the mechanical properties of the matrix material. Compared with the traditional material, the graphene serving as a two-dimensional nano material has excellent mechanical property, can obviously improve the wear resistance of the material under the condition of extremely small filling amount, and is an efficient friction reducing filler. However, the lubricating performance is poor, and graphene needs to be improved to have a certain lubricating function. The polytetrafluoroethylene has excellent lubricating property, and the composite material has better self-lubricating property by adding the nano polytetrafluoroethylene into the polymer. Therefore, if the graphene and the nano polytetrafluoroethylene can be compounded to exert a synergistic effect, the lubricating and wear-resisting properties of the polymer material can be improved.
Since graphene and nano polytetrafluoroethylene are both nanoscale materials and are added into a polymer material by a conventional mechanical mixing method, the graphene and the nano polytetrafluoroethylene are easy to agglomerate and difficult to realize uniform and stable dispersion, and therefore, the effect is difficult to reach an ideal level. The invention patent 201410088554.1 indicates that the surfaces of graphene and polytetrafluoroethylene are respectively aminated and carboxylated, and then the covalent bond connection between graphene and nano polytetrafluoroethylene can be realized through condensation reaction, so as to prepare the uniform graphene-nano polytetrafluoroethylene composite filler. Although the method can uniformly disperse the graphene and the nano polytetrafluoroethylene, a plurality of chemical reagents are required to be introduced, the environmental protection performance is uncertain, the process is complex, the impurity removal and reaction efficiency is low, and the industrial production is difficult to realize at present. Therefore, the preparation and application methods of the graphene-nano polytetrafluoroethylene composite modified filler with the functions of reducing abrasion and friction are provided
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the preparation method and the application method of the graphene-nano polytetrafluoroethylene composite modified filler, which are simple and practical in operation, obvious in effect and capable of realizing mass production, and the abrasion and friction reducing characteristics of the resin matrix material can be effectively improved by solving the dispersion and combination problems of graphene and nano polytetrafluoroethylene.
In order to solve the problems of dispersion and combination of graphene and nano polytetrafluoroethylene, the invention provides a preparation method of a graphene-nano polytetrafluoroethylene composite modified filler, which comprises the following steps,
step I, adding graphene into deionized water, and heating and stirring under a water bath condition to obtain a solution A;
step II, taking the coupling agent, ethanol and deionized water, stirring and mixing to obtain a solution B
Step III, mixing the solution A and the solution B, performing coupling reaction under the condition of water bath to enable the surface of the material to be lipophilic, cooling, filtering and washing to obtain a modified graphene filler M;
step IV, adding a proper amount of modified graphene filler M and nano polytetrafluoroethylene into a water-ethanol mixed solution for mixing, adding a proper amount of aqueous binder, and performing dispersive mixing to obtain an emulsion N;
and step V, maintaining the dispersibility of the emulsion N, and dehydrating and drying to obtain the graphene-nano polytetrafluoroethylene composite modified filler.
Preferably, the weight ratio of each component in the step I is as follows: 800 parts of deionized water and 10 parts of graphene, wherein the water bath temperature is 80 ℃, and the graphene is powdery water-based graphene;
the weight ratio of each component in the step II is as follows: 2 parts of coupling agent, 15 parts of ethanol and 1 part of deionized water;
the weight ratio of the solution A to the solution B in the step III is as follows: 810 parts of solution A and 5 parts of solution B, and the coupling reaction is carried out for 3 hours in a water bath at the temperature of 80 ℃.
Preferably, the coupling agent is one or more of organic chromium complex, silanes, titanates and aluminate compounds.
Preferably, the weight ratio of the graphene filler M to the polytetrafluoroethylene in the step IV is in a range of 1:5 to 1: 25.
Preferably, the aqueous binder in the step IV is one or more of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) and erythritol, and the weight content of the aqueous binder is 1% -5% of the graphene-nano polytetrafluoroethylene composite modified filler.
Preferably, the drying manner in step V is spray drying, and the parameters of the spray drying are that the temperature at the opening is 120-150 ℃, the feeding speed is 5-35%, the air pressure is 10-25 atmospheric pressure, and the temperature at the outlet is controlled within the range of 70-90 ℃.
Preferably, the weight ratio of the water-ethanol mixed solution in the step IV is 3 parts of water and 2 parts of ethanol.
The invention provides an application method of a graphene-nano polytetrafluoroethylene composite modified filler, which is characterized in that in order to improve the wear resistance and lubricity of a polymer matrix and reduce the friction coefficient and wear rate of a material, the graphene-nano polytetrafluoroethylene composite modified filler obtained in the step V is added into the polymer matrix material in a weight ratio of 5-30%, meanwhile, a small molecular oily substance with the weight fraction of 0.1-1% is added, then, the mixture is stirred and mixed, and extruded and granulated to obtain a graphene-nano polytetrafluoroethylene modified polymer composite granule, and the composite granule is subjected to injection molding or hot pressing to obtain a product with a required structure.
Preferably, the small molecular oily matter is paraffin oil, and the polymer matrix material is one or more of polyformaldehyde, nylon, polyether ether ketone and ultrahigh molecular weight polyethylene.
The beneficial effects of the invention are: the invention adopts the coupling agent for pretreatment, on one hand, the mutual accumulation of the fillers due to Van der Waals force can be avoided, and the filling property of the fillers is reduced; on the other hand, the pretreatment of the coupling agent can also improve the compatibility of the filler and the matrix, reduce the defects caused by incompatibility in the composite material, and is simpler and simpler in process flow compared with the existing method adopting chemical functional groups such as amination treatment, carboxylation treatment and the like; the graphene and the nano polytetrafluoroethylene are uniformly dispersed by adopting a liquid phase mixing mode, the agglomeration is avoided, the dispersion effect is better compared with that of a common mechanical mixing method, in addition, the existing industrially mature and efficient spray drying equipment is utilized, the cost is low, the industrial application prospect is larger, meanwhile, the spray drying mode is adopted, the composite slurry is dried, the large-scale agglomeration of the nano material is avoided, and the nano polytetrafluoroethylene is adhered to the surface of the graphene through the action of a binder, so that the composite filler obtained by the preparation method provided by the invention has the wear resistance of the graphene and the lubricating property of the nano polytetrafluoroethylene, and the combination of the graphene and the nano polytetrafluoroethylene in a matrix material can play a synergistic effect. The composite material prepared by the preparation method can be mixed with various polymer base materials such as polyformaldehyde, nylon, polyether-ether-ketone and ultra-high molecular weight polyethylene, can improve the lubricating and wear-resisting properties of the composite material, can be suitable for injection molding and hot-press molding, and has wide application range.
Drawings
FIG. 1 is an electron micrograph I of graphene-nano polytetrafluoroethylene/polyoxymethylene prepared by the method of the present invention;
FIG. 2 is an electron micrograph II of the graphene-nano polytetrafluoroethylene/polyoxymethylene prepared by the method of the invention.
Detailed Description
The present invention will be further described with reference to specific examples, but it should be understood that the examples described are only a few examples of the present invention, and not all examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1, the graphene-nano polytetrafluoroethylene composite modified filler is prepared by the following process:
firstly, adding 10 parts by weight of powdered graphene into 800 parts by weight of deionized water, heating to 80 ℃ through a water bath, mixing and stirring to fully dissolve the graphene to obtain a solution A; taking 2 parts by weight of silane coupling agent, 15 parts by weight of ethanol and 1 part by weight of deionized water, mixing and fully stirring for 30min to obtain a solution B, adding 5 parts by weight of silane coupling agent into the solution A, then keeping the reaction temperature at 80 ℃, carrying out water bath reaction for 3 hours, then cooling to room temperature, filtering and washing with deionized water to obtain the modified graphene filler M with oleophylic property, wherein the fillers can be prevented from being stacked and aggregated due to Van der Waals force by adopting the pretreatment of the coupling agent. The preparation method comprises the steps of preparing materials according to the weight ratio of 1:15 of the graphene filler M to the nano polytetrafluoroethylene, adding a proper amount of water-ethanol mixed solution with the mass ratio of 3:2, stirring and mixing, and simultaneously adding the erythritol accounting for 2% of the total mass of the graphene filler M and the nano polytetrafluoroethylene, wherein the amount of the water-ethanol mixed solution requires that the graphene filler M and the nano polytetrafluoroethylene can be fully dispersed in the water-ethanol mixed solution, and when the volume of the ethanol accounts for 10% -20% of the mixed solution, the erythritol has a good effect as a binder, and the nano polytetrafluoroethylene can be effectively prevented from being overlapped in a subsequent process after being bonded on the surface of the graphene, so that the agglomeration of the composite filler in a polymer is avoided.
And stirring the mixture at the temperature of 60 ℃ to form emulsion N, wherein in order to provide the dispersion effect of the emulsion N, an ultrasonic dispersion device can be adopted to disperse the emulsion N.
Then, the emulsion N is treated in a spray drying mode, various parameters of a spray drying tester are adjusted, the inlet temperature is kept at 130 ℃, the feeding speed is kept at 15, and the air pressure is 20m 3 H, jet velocity of 5S -1 And when the outlet temperature is 70-80 ℃, after the equipment is preheated and stabilized, the emulsion is subjected to spray drying by a spray dryer under the transmission of an N injection pump, and the treated dry powder P, namely the graphene-nano polytetrafluoroethylene composite modified filler, is collected.
The prepared graphene-nano polytetrafluoroethylene composite modified filler can effectively improve the wear rate of the existing polymer matrix, the obtained dry powder P20 parts by weight and 80 parts by weight of polyformaldehyde powder are mixed, paraffin oil accounting for 0.2 percent of the total weight is added, the mixture is stirred for 5min under the condition of 1000r/min by adopting a traditional shearing type mechanical stirring method, and then the polyformaldehyde composite modified by the graphene-nano polytetrafluoroethylene can be obtained.
To testThe effect of improving the wear resistance of the graphene-nano polytetrafluoroethylene composite modified filler on the polyformaldehyde matrix is proved, a structural part prepared from graphene-nano polytetrafluoroethylene modified polyformaldehyde composite granules and a structural part prepared from pure polyformaldehyde are respectively obtained in an injection molding mode, and a friction and wear test is carried out on the comparative materials, so that experimental data show that the friction coefficient of the structural part prepared by the preparation and application methods is 0.11, and the wear rate is 1.1 x 10 -6 mm 3 V (N × m); while pure polyoxymethylene has a coefficient of friction of 0.19 and a wear rate of 2.3 x 10 -6 mm 3 V (N × m). The results prove that the preparation and application methods of the graphene-nano polytetrafluoroethylene composite modified filler provided by the invention can effectively combine the wear resistance of graphene and the lubricating property of nano polytetrafluoroethylene, and the combination of the graphene-nano polytetrafluoroethylene composite modified filler and the nano polytetrafluoroethylene can be applied to the existing polymer matrix to obviously improve the lubricating wear resistance of the polymer matrix;
in addition, microscopic interface observation is carried out on a member made of graphene-nano polytetrafluoroethylene/polyformaldehyde through an electron microscope, and a Hitachi cold field emission scanning electron microscope SU8010(MDTC-EQ-M18-01) is adopted, and the type specification is as follows: the HITACHI SU8010 has the electron microscope images as shown in fig. 1 and fig. 2 (the magnifications of fig. 1 and fig. 2 are different), the substrate material in the images is graphene, the spherical particles are polytetrafluoroethylene micro-nano powder particles, and it can be seen that except a small amount of agglomeration in a local area, the nano polytetrafluoroethylene is distributed uniformly, which indicates that the nano polytetrafluoroethylene is successfully bonded on the surface of the graphene, thereby proving the effectiveness of the microscopic morphology of the invention.
Example 2
Firstly, adding 10 parts by weight of powdered graphene into 800 parts by weight of deionized water, heating to 80 ℃ through a water bath, mixing and stirring to fully dissolve the graphene to obtain a solution A; taking 2 parts by weight of silane coupling agent, 15 parts by weight of ethanol and 1 part by weight of deionized water, mixing and fully stirring for 30min to obtain solution B, taking 5 parts by weight, adding into the solution A, keeping the reaction temperature at 80 ℃, carrying out water bath reaction for 3 hours, cooling to room temperature, filtering, washing with deionized water to obtain modified stone with oleophylic propertyThe graphene fillers M are pretreated by the coupling agent, so that the fillers can be prevented from being stacked and agglomerated due to van der Waals force. Preparing materials according to the weight ratio of 1:5 of the graphene filler M to the nano polytetrafluoroethylene, adding a proper amount of water-ethanol mixed solution with the mass ratio of 3:2, stirring and mixing, simultaneously adding polyvinylpyrrolidone and erythritol accounting for 1% of the total mass of the graphene filler M and the nano polytetrafluoroethylene, wherein the amount of the water-ethanol mixed solution requires that the graphene filler M and the nano polytetrafluoroethylene can be fully dispersed in the water-ethanol mixed solution, stirring to form emulsion N under the condition of keeping 60 ℃, then treating the emulsion N in a spray drying mode, adjusting various parameters of a spray drying testing machine, keeping the inlet temperature at 130 ℃, the feeding speed at 15 and the air pressure at 20M 3 H, jet velocity of 5S -1 And when the outlet temperature is 70-80 ℃, after the equipment is preheated and stabilized, the emulsion is subjected to spray drying by a spray dryer under the transmission of an N injection pump, and the treated dry powder, namely the graphene-nano polytetrafluoroethylene composite modified filler, is collected.
The prepared graphene-nano polytetrafluoroethylene composite modified filler can effectively improve the wear rate of the existing polymer matrix, 5 parts by weight of the obtained dry powder is mixed with 95 parts by weight of ultra-high molecular weight polyethylene, paraffin oil accounting for 0.2 percent of the total weight is added, the mixture is stirred for 5min under the condition of 1000r/min by adopting a traditional shear type mechanical stirring method, and then the graphene-nano polytetrafluoroethylene modified polyethylene composite material can be obtained.
In order to verify the effect of the graphene-nano polytetrafluoroethylene composite modified filler on improving the wear resistance of the polyethylene matrix, a structural member prepared from graphene-nano polytetrafluoroethylene modified polyethylene composite granules and a structural member prepared from pure polyethylene are respectively obtained in an injection molding mode, and the comparative materials are subjected to a friction and wear test. The specific friction test condition is tested by adopting a reciprocating friction mode, the specific equipment model is an HSR-2M high-speed reciprocating friction abrasion tester of Kaikaya Hua Ke technology development Limited company in Lanzhou, and the test parameters are as follows; the ground surface is GCr15 steel ball with diameter of 6.35mm, load is 20N, reciprocating speed is 500rpm, reciprocating length is 5mm, test time is 2h, a structural member made of pure ultra-high molecular weight polyethylene is used as a comparison test, and the result is that the friction coefficient of the pure ultra-high molecular weight polyethylene is 0.12, and the wear rate is:
5.6*10 -6 mm 3 v (N × m), and the coefficient of friction of the graphene-nano polytetrafluoroethylene composite filler added with the present invention is 0.09, the wear rate: 3.2*10 -6 mm 3 V (N × m), the wear rate is reduced by 42% compared to a significant effect.
Claims (6)
1. A preparation method of graphene-nano polytetrafluoroethylene composite modified filler is characterized by comprising the following steps:
step I, adding graphene into deionized water, and heating and stirring under a water bath condition to obtain a solution A;
step II, taking the coupling agent, ethanol and deionized water, and stirring and mixing to obtain a solution B;
step III, mixing the solution A and the solution B, carrying out coupling reaction under the condition of water bath to enable the surface of the material to present lipophilicity, cooling, filtering and washing to obtain a modified graphene filler M;
step IV, adding a proper amount of modified graphene filler M and nano polytetrafluoroethylene into a water-ethanol mixed solution for mixing, adding a proper amount of aqueous binder, and performing dispersive mixing to obtain an emulsion N;
step V, maintaining the dispersibility of the emulsion N, and dehydrating and drying to obtain the graphene-nano polytetrafluoroethylene composite modified filler;
the coupling agent is one or more of organic chromium complex, silanes, titanates and aluminate compounds;
the weight ratio of the graphene filler M to the polytetrafluoroethylene in the step IV is 1: 5-1: 25;
the water-based binder in the step IV is one or more of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) and erythritol, the weight content of the water-based binder is 1% -5% of that of the graphene-nano polytetrafluoroethylene composite modified filler, and the graphene is powdery water-based graphene.
2. The preparation method of the graphene-nano polytetrafluoroethylene composite modified filler according to claim 1, wherein the weight ratio of each component in the step I is as follows: 800 parts of deionized water and 10 parts of graphene, wherein the water bath temperature is 80 ℃;
the weight ratio of each component in the step II is as follows: 2 parts of coupling agent, 15 parts of ethanol and 1 part of deionized water;
the weight ratio of the solution A to the solution B in the step III is as follows: 810 parts of solution A and 5 parts of solution B, and the coupling reaction is carried out for 3 hours in a water bath at the temperature of 80 ℃.
3. The method as claimed in claim 2, wherein the drying manner in step v is spray drying, and the parameters of the spray drying include an inlet temperature of 120-.
4. The method for preparing the graphene-nano polytetrafluoroethylene composite modified filler according to claim 2, wherein the weight ratio of the water-ethanol mixed solution in the step IV is 3 parts of water and 2 parts of ethanol.
5. The application method of the composite modified filler prepared by the preparation method of any one of claims 1 to 4 is characterized in that the graphene-nano polytetrafluoroethylene composite modified filler obtained in the step V is added into a polymer matrix material in a weight ratio of 5-30%, meanwhile, a small molecular oily substance with the weight fraction of 0.1-1% is added, then, the mixture is stirred and mixed, extrusion granulation is carried out to obtain graphene-nano polytetrafluoroethylene modified polymer composite granules, and the composite granules are subjected to injection molding or hot pressing to obtain a product with a required structure, wherein the small molecular oily substance is paraffin oil.
6. The method for applying the composite modified filler according to claim 5, wherein the polymer matrix material is one or more of polyoxymethylene, nylon, polyetheretherketone and ultra-high molecular weight polyethylene.
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| CN110918007B (en) * | 2019-11-04 | 2022-04-22 | 江苏一夫新材料产业技术研究院有限公司 | PVP polymerized SnO2-graphene aerogels and method for the production thereof |
| CN112300521B (en) * | 2020-11-09 | 2022-03-11 | 河北中科同创科技发展有限公司 | High-thermal-conductivity polytetrafluoroethylene composite material and preparation method and application thereof |
| CN112574585A (en) * | 2020-12-11 | 2021-03-30 | 安徽中翰高分子科技有限公司 | Low-hardness thermoplastic vulcanized elastomer material formed by polypropylene three-dimensional blow molding and preparation method thereof |
| CN114752265A (en) * | 2022-04-25 | 2022-07-15 | 中国航空发动机研究院 | Fluorine-containing coating and preparation method and application thereof |
| CN114875393B (en) * | 2022-05-13 | 2023-03-21 | 上海涓微新材料科技有限公司 | High-hardness wear-resistant nickel-phosphorus Teflon plating solution and plating layer |
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