CN114163778A - Solvent-free nano fluid-filled epoxy resin-based self-lubricating composite material - Google Patents
Solvent-free nano fluid-filled epoxy resin-based self-lubricating composite material Download PDFInfo
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- CN114163778A CN114163778A CN202111092329.1A CN202111092329A CN114163778A CN 114163778 A CN114163778 A CN 114163778A CN 202111092329 A CN202111092329 A CN 202111092329A CN 114163778 A CN114163778 A CN 114163778A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to a solvent-free nano fluid filled epoxy resin based self-lubricating composite material, which is prepared by stirring and mixing epoxy resin and solvent-free nano fluid for 15min, adding a curing agent after the mixture is uniform, and continuously stirring and mixing for 10min to obtain a mixed solution; and pouring the mixed solution into a mold, and curing at low temperature to obtain the product. The composite material can effectively overcome the agglomeration problem of nano particles, obviously enhance the bearing capacity and the lubricating property of the epoxy resin-based material, can be used as a sliding friction part of a moving mechanism such as an engine and the like under the condition of oil lubrication to replace a metal-metal friction pair, and has potential application prospect.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a solvent-free nano fluid-filled epoxy resin-based self-lubricating composite material.
Background
With the rapid development of modern automobiles and high-end equipment technology, the service working conditions of a plurality of motion mechanisms are more severe, the friction pair frequently runs in a mixed and boundary lubrication interval, and the solid-solid contact bears considerable or even most of load, so that the abrasion of the traditional friction pair is aggravated, even the occlusion phenomenon is caused, and the service life and the reliability of the motion mechanisms are seriously challenged. Therefore, the friction pair material with long service life and high reliability is developed, the problem of tribology design of a motion mechanism is solved, and the friction pair material has important theoretical and practical significance.
The polymer material has great application potential in the aspect of tribology design of a motion mechanism in the field of high-end equipment due to the advantages of self-lubrication, high chemical stability, designable performance and the like. Epoxy resin is a typical thermosetting polymer engineering material, has excellent chemical stability and good processing performance, and is widely applied to the field of tribology as a self-lubricating matrix material. However, pure epoxy resin has poor mechanical strength, is easy to adhere and seriously abraded, and needs to be added with functional filler to improve the comprehensive performance. The tribology theory and practice show that the nano material is added into the epoxy resin, and the high-performance transfer film with the lubricating property is generated in situ at the polymer-metal friction interface, so that the defect of the liquid film bearing capacity can be effectively made up, and the boundary lubricating effect of the motion mechanism is obviously improved.
Although the tribological performance of the polymer can be improved to a certain extent by the nano material, due to the small-scale effect, the nano material is easy to agglomerate under the action of van der waals force, and is difficult to be uniformly dispersed in the epoxy resin and keep long-term stability in the preparation process, so that the application and popularization of the nano material in the field of the polymer are greatly limited. The solvent-free nano fluid is a special ionic liquid modified nano material, can show liquidity similar to liquid at room temperature without any other solvent, has a core-shell structure, integrates the small size and surface interface effect of monodisperse nano particles and the physicochemical property of shell ionic flexible long-chain molecules, can regulate and control the molecular structures of the nano core and the shell, has the typical characteristics of a novel nano lubricating material, and shows good friction-reducing and wear-resisting properties when used as a lubricant and a lubricating additive. Based on the method, the solvent-free nano fluid is used as a lubricating phase to enhance the tribological performance of the polymer material, and has good application prospect. However, there is no published report on solvent-free nano fluid-filled polymer-based self-lubricating composite material.
Disclosure of Invention
The invention aims to solve the technical problem of providing the solvent-free nano fluid filled epoxy resin based self-lubricating composite material which effectively overcomes the agglomeration problem of nano particles.
In order to solve the problems, the solvent-free nano fluid filled epoxy resin based self-lubricating composite material is characterized in that: the composite material is prepared by stirring and mixing epoxy resin and solvent-free nano fluid for 15min, adding curing agent after the epoxy resin and the solvent-free nano fluid are mixed uniformly, and continuously stirring and mixing for 10min to obtain a mixed solution; and pouring the mixed solution into a mold, and curing at low temperature to obtain the product.
The solvent-free nano fluid is any one of a silicon dioxide nano fluid, a graphene nano fluid, a carbon nanotube fluid, a titanium dioxide nano fluid and a graphene-loaded silicon dioxide nano fluid.
The epoxy resin is bisphenol A type liquid resin.
The curing agent is aliphatic amine curing agent.
The mass fractions of the epoxy resin and the solvent-free nano fluid are 85-99.95% and 0.05-15% in sequence.
The using amount of the curing agent is 5-20% of the mass fraction of the epoxy resin.
The stirring and mixing conditions refer to that the vacuum degree is-0.8 multiplied by 105Pa, the initial rotating speed is 500 r/min; after the solvent-free nano fluid is completely immersed into the epoxy resin, the rotating speed is adjusted to 5000 r/min; after the curing agent is added, the rotating speed is adjusted to 5000 r/min.
The low-temperature curing condition is that the pre-curing is carried out for 1-5 h at the temperature of 20-50 ℃, and then the curing is carried out for 1-3 h at the temperature of 80-160 ℃.
Compared with the prior art, the invention has the following advantages:
1. the solvent-free nano fluid used in the invention has a core-shell structure, and the flexible long-chain shell structure of the solvent-free nano fluid can promote the nano fluid to be uniformly dispersed in the epoxy resin, so that the problem of agglomeration of nano particles can be effectively solved while the inherent characteristics of nano materials are exerted.
2. The nano fluid can be released to a friction interface in the friction process of the composite material obtained by the invention, and the formation of a high-strength transfer film is promoted, so that the lubricating property and the bearing capacity of the friction pair interface are improved, the direct contact of a friction pair is inhibited, and the service life and the reliability of the friction pair are improved.
3. The invention provides a new idea for the design of a friction pair under the condition of boundary lubrication, and the obtained solvent-free nano fluid-filled epoxy resin-based self-lubricating composite material has good development prospect as a potential application material of mechanical parts such as engines, internal combustion engines and the like.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a transmission electron microscope image of a slice of an epoxy resin-based composite material in example 2 of the present invention.
Detailed Description
A solvent-free nano-class fluid filled epoxy resin-base self-lubricating composite material with vacuum degree of-0.8X 105Stirring and mixing 85-99.95% of epoxy resin and 0.05-15% of solvent-free nano fluid under the conditions that the initial rotating speed is 500r/min, adjusting the rotating speed to 5000r/min after the solvent-free nano fluid is completely immersed in the epoxy resin, stirring and mixing for 15min, and adding a curing agent after uniform mixing, wherein the using amount of the curing agent is 5% -20% of the mass fraction of the epoxy resin; then the rotating speed is adjusted to 5000r/min, and the mixture is continuously stirred and mixed for 10min to obtain a mixed solution; pouring the mixed solution into a mold, pre-curing at 20-50 ℃ for 1-5 h, and curing at 80-160 ℃ for 1-3 h to obtain the product.
Wherein: the solvent-free nano-fluid is any one of a silica nano-fluid, a graphene nano-fluid, a carbon nanotube-based fluid, a titanium dioxide nano-fluid and a graphene-supported silica nano-fluid.
The epoxy resin is bisphenol A type liquid resin.
The curing agent is aliphatic amine curing agent.
[ PREPARATION OF SILICA NANO-LIKE FLUIDS ]
Dispersing the silicon dioxide nano particles in deionized water, carrying out ultrasonic treatment for 1h, adding 3- (trihydroxysilyl) propyl methyl phosphonic acid monosodium salt aqueous solution, heating and stirring at 70 ℃ for reaction for 24h, and washing and purifying to obtain the phosphonate modified silicon dioxide nano particles; dispersing the product in tetrahydrofuran solution, adding 40mL of concentrated hydrochloric acid, stirring and reacting for 2h at room temperature, centrifuging to remove sodium chloride salt, washing and evaporating the product to dryness to obtain phosphonic acid modified silicon dioxide nanoparticles; and then, dissolving the phosphonic acid modified silica nanoparticles in deionized water, adding an amino-terminated copolymer M2070 aqueous solution, and heating and stirring at 70 ℃ for reaction for 24 hours. And after the reaction is finished, washing and filtering the product by using deionized water, ethanol and tetrahydrofuran, removing impurities, and drying to obtain the silicon dioxide nano fluid.
Example 1
Stirring and mixing 0.05wt% of silicon dioxide nano fluid and 99.95wt% of epoxy resin under the vacuum high-speed condition for 15min, wherein the vacuum degree is-0.8 multiplied by 105Pa, the rotating speed is 500r/min, and the rotating speed is adjusted to 5000r/min after the silicon dioxide nano fluid completely invades the epoxy resin, so as to obtain a mixed liquid A.
And adding a curing agent with the mass being 20wt% of the mass of the epoxy resin into the mixed solution A, and further stirring at a high speed for 10min at the rotating speed of 5000r/min to obtain a mixed solution B.
And pouring the mixed solution B into a mould, curing at the low temperature of 20 ℃ for 5 hours, and curing at the temperature of 80 ℃ for 3 hours to obtain the solvent-free silicon dioxide nano fluid filled epoxy resin based nano composite material.
Example 2
Stirring and mixing 15wt% of silicon dioxide nano fluid and 85wt% of epoxy resin under the vacuum high-speed condition for 15min, wherein the vacuum degree is-0.8 multiplied by 105Pa, the rotating speed is 500r/min, and the rotating speed is adjusted to 5000r/min after the solvent-free silicon dioxide nano fluid is completely immersed in the epoxy resin, so as to obtain a mixed liquid A.
And adding a curing agent with the mass of 5wt% of the epoxy resin into the mixed solution A, and further stirring at a high speed of 5000r/min for 10min to obtain a mixed solution B.
And pouring the mixed solution B into a mould, curing at 50 ℃ for 1h, and curing at 160 ℃ for 1h to obtain the solvent-free silicon dioxide nano fluid filled epoxy resin based nano composite material.
The obtained solvent-free silicon dioxide nano fluid filled epoxy resin matrix composite material slice is observed by a transmission electron microscope, as shown in figure 1, the silicon dioxide nano fluid can be seen to be uniformly dispersed in the epoxy resin, and the agglomeration phenomenon of the conventional nano filler in a resin matrix is effectively avoided. The analysis shows that the flexible shell layer of the nano fluid is used as a molecular bridge, one end of the flexible shell layer is linked with the nano inner core, and the other end of the flexible shell layer is grafted with the epoxy resin matrix molecules to jointly form a three-dimensional network structure.
[ PREPARATION OF SOLVENT-FREE CARBON NANOTUBE FLUID ]
Dispersing carbon nanotubes in mixed acid, performing ultrasonic treatment for 2 hours, washing with deionized water, centrifuging to remove residual mixed acid, performing vacuum drying to obtain oxidized carbon nanotubes with functionalized oxygen-containing groups, dispersing the oxidized carbon nanotubes in deionized water, performing ultrasonic treatment for 2 hours to obtain a carbon nanotube suspension, dropwise adding silane coupling agent 3- (trihydroxy silicon-based) propanesulfonic acid, performing heating reflux reaction at 80 ℃ for 24 hours, and performing purification and drying to obtain the silane coupling agent grafted carbon nanotubes. And then ultrasonically dissolving the treated carbon nano tube in deionized water at room temperature, dropwise adding an amino-terminated block copolymer M2070 aqueous solution under mechanical stirring, reacting for 24 hours at 50 ℃, and purifying and drying the product to obtain the solvent-free carbon nano tube fluid.
Example 3
5wt% of solvent-free carbon nanotube fluid and 95wt% of epoxy resin are stirred and mixed under the vacuum high-speed condition, the stirring time is 15min, and the vacuum degree is-0.8 multiplied by 105Pa, the rotating speed is 500r/min, and the rotating speed is adjusted to 5000r/min after the similar fluid completely invades the epoxy resin, so as to obtain a mixed liquid A.
Adding a curing agent with the mass of 15wt% of the epoxy resin into the mixed solution A, and further stirring at a high speed of 5000r/min for 10min to obtain a mixed solution B.
And pouring the mixed solution B into a mould, curing at the low temperature of 30 ℃ for 2h, and curing at the temperature of 100 ℃ for 2h to obtain the solvent-free carbon nanotube fluid-filled epoxy resin-based nanocomposite.
Example 4
Stirring and mixing 10wt% of solvent-free carbon nanotube fluid and 90wt% of epoxy resin under the vacuum high-speed condition for 15min, wherein the vacuum degree is-0.8 multiplied by 105Pa, the rotating speed is 500r/min, and the rotating speed is adjusted to 5000r/min after the solvent-free nano fluid completely invades the epoxy resin, so as to obtain a mixed liquid A.
And adding a curing agent with the mass being 10wt% of the mass of the epoxy resin into the mixed solution A, and further stirring at a high speed for 10min at the rotating speed of 5000r/min to obtain a mixed solution B.
And pouring the mixed solution B into a mould, curing at 40 ℃ for 1.5h, and curing at 120 ℃ for 2h to obtain the solvent-free nano fluid filled epoxy resin-based nano composite material.
Comparative example 1
Adding a curing agent with the mass of 20wt% of the epoxy resin into the epoxy resin, and stirring at a high speed of 5000r/min for 10min to obtain a mixed solution; pouring the mixed solution into a mold, curing at the low temperature of 20 ℃ for 5 hours, and then curing at the temperature of 80 ℃ for 3 hours to obtain the epoxy resin material.
In examples 1 to 4 and comparative example 1, the epoxy resin was a bisphenol A type liquid resin. The curing agent is aliphatic amine curing agent. The mass unit is g.
The cured polymer samples of examples 1 to 4 and comparative example 1 were processed into 50mm × 10mm × 4mm block-shaped test specimens, and a friction test was performed using a high-speed ring-block tester to examine the tribological properties thereof. GCr15 steel ring is used as friction couple, the lubricating medium is poly-alpha-olefin (PAO 4), the polymer block and the coupling material are both polished by sand paper with the same mesh number to obtain the same roughness of 0.1-0.2 μm, the test load is 300N, the sliding speed is 0.05m/s, and the friction and wear test time is 3 h. And after the friction experiment is finished, measuring the width of the grinding crack by using an optical microscope, and calculating the characteristic wear rate by using a formula.
The calculation formula of the wear rate is as follows:
in the formula: l' is the width (mm) of the sample, R is the diameter (mm) of the dual steel ring, W is the width (mm) of the grinding mark, F is the normal force (N), and L is the sliding distance (m).
The average friction coefficient and the characteristic wear rate of the materials prepared in examples 1-4 and comparative example 1 were measured and calculated, and the results are shown in table 1. The friction test result shows that the tribological performance of the composite material in the boundary and the mixed lubrication area is greatly improved by adding the nano fluid, and the antifriction and wear-resistant performance of the epoxy resin material can be obviously enhanced even if a trace amount of the nano fluid is added. In the friction process, the solvent-free nano fluid is released on a friction interface, is adsorbed on the surface of a friction pair through electrostatic action, changes the structure of an adsorption film, promotes the in-situ growth of the friction film with a hybrid structure, inhibits the direct contact of the friction pair, and obviously enhances the bearing capacity and the lubricating property of the epoxy resin-based material. Therefore, the self-lubricating composite material can be used as a sliding friction part of a moving mechanism such as an engine and the like under the condition of oil lubrication to replace a metal-metal friction pair, and has potential application prospect.
TABLE 1 measurement and calculation results of average friction coefficient and wear rate of materials prepared in examples 1-4 and comparative example 1
Claims (8)
1. A solvent-free nano fluid filled epoxy resin based self-lubricating composite material is characterized in that: the composite material is prepared by stirring and mixing epoxy resin and solvent-free nano fluid for 15min, adding curing agent after the epoxy resin and the solvent-free nano fluid are mixed uniformly, and continuously stirring and mixing for 10min to obtain a mixed solution; and pouring the mixed solution into a mold, and curing at low temperature to obtain the product.
2. The solvent-free nano fluid-filled epoxy-based self-lubricating composite material as claimed in claim 1, wherein: the solvent-free nano fluid is any one of a silicon dioxide nano fluid, a graphene nano fluid, a carbon nanotube fluid, a titanium dioxide nano fluid and a graphene-loaded silicon dioxide nano fluid.
3. The solvent-free nano fluid-filled epoxy-based self-lubricating composite material as claimed in claim 1, wherein: the epoxy resin is bisphenol A type liquid resin.
4. The solvent-free nano fluid-filled epoxy-based self-lubricating composite material as claimed in claim 1, wherein: the curing agent is aliphatic amine curing agent.
5. The solvent-free nano fluid-filled epoxy-based self-lubricating composite material as claimed in claim 1, wherein: the mass fractions of the epoxy resin and the solvent-free nano fluid are 85-99.95% and 0.05-15% in sequence.
6. The solvent-free nano fluid-filled epoxy-based self-lubricating composite material as claimed in claim 1, wherein: the using amount of the curing agent is 5-20% of the mass fraction of the epoxy resin.
7. The solvent-free nano fluid-filled epoxy-based self-lubricating composite material as claimed in claim 1, wherein: the stirring and mixing conditions refer to that the vacuum degree is-0.8 multiplied by 105Pa, the initial rotating speed is 500 r/min; after the solvent-free nano fluid is completely immersed into the epoxy resin, the rotating speed is adjusted to 5000 r/min; after the curing agent is added, the rotating speed is adjusted to 5000 r/min.
8. The solvent-free nano fluid-filled epoxy-based self-lubricating composite material as claimed in claim 1, wherein: the low-temperature curing condition is that the pre-curing is carried out for 1-5 h at the temperature of 20-50 ℃, and then the curing is carried out for 1-3 h at the temperature of 80-160 ℃.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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