CN116535933A - Resin coating liquid suitable for oil lubrication and preparation method and application thereof - Google Patents
Resin coating liquid suitable for oil lubrication and preparation method and application thereof Download PDFInfo
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- CN116535933A CN116535933A CN202310567256.XA CN202310567256A CN116535933A CN 116535933 A CN116535933 A CN 116535933A CN 202310567256 A CN202310567256 A CN 202310567256A CN 116535933 A CN116535933 A CN 116535933A
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- molybdenum disulfide
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- 239000011248 coating agent Substances 0.000 title claims abstract description 165
- 238000000576 coating method Methods 0.000 title claims abstract description 165
- 229920005989 resin Polymers 0.000 title claims abstract description 129
- 239000011347 resin Substances 0.000 title claims abstract description 129
- 239000007788 liquid Substances 0.000 title claims abstract description 91
- 238000005461 lubrication Methods 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 134
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 134
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 50
- 239000010439 graphite Substances 0.000 claims abstract description 50
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- 239000007787 solid Substances 0.000 claims abstract description 37
- 239000000314 lubricant Substances 0.000 claims abstract description 34
- 239000003822 epoxy resin Substances 0.000 claims abstract description 33
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 90
- 239000003921 oil Substances 0.000 claims description 64
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 60
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 60
- 239000003292 glue Substances 0.000 claims description 33
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 26
- 239000000654 additive Substances 0.000 claims description 25
- 238000009210 therapy by ultrasound Methods 0.000 claims description 22
- 239000000853 adhesive Substances 0.000 claims description 20
- 230000001070 adhesive effect Effects 0.000 claims description 20
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 17
- 230000000996 additive effect Effects 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 16
- 238000010008 shearing Methods 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 9
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical group NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- 238000007654 immersion Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 59
- 239000010410 layer Substances 0.000 description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 28
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 22
- 239000000945 filler Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 18
- 239000012071 phase Substances 0.000 description 10
- 238000005299 abrasion Methods 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 229910000975 Carbon steel Inorganic materials 0.000 description 8
- 239000010962 carbon steel Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000002791 soaking Methods 0.000 description 8
- 238000004108 freeze drying Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- 239000006228 supernatant Substances 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 230000001050 lubricating effect Effects 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010687 lubricating oil Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000005036 potential barrier Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 231100000241 scar Toxicity 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000010724 circulating oil Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000012767 functional filler Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
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- 239000002356 single layer Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
- B05D7/16—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies using synthetic lacquers or varnishes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention relates to a resin coating liquid suitable for oil lubrication, and a preparation method and application thereof; the resin coating liquid comprises epoxy resin, 15-25 wt% of bulk solid lubricant, organic solvent and curing agent; the bulk phase solid lubricant consists of bulk molybdenum disulfide and graphite in a mass ratio of 7:4-6; the average grain diameter of the bulk molybdenum disulfide is 0.1-20 mu m, and the average grain diameter of the graphite is 0.1-10 mu m; the preparation method comprises the following steps: uniformly mixing the components according to a certain proportion and a certain feeding sequence to obtain resin coating liquid; the application is as follows: and spraying the resin coating liquid on the surface of the metal substrate, and curing to obtain the coating. The method is simple, and the prepared coating has small friction coefficient, excellent impact resistance and oil resistance and strong bonding capability with a metal substrate.
Description
Technical Field
The invention belongs to the technical field of coating, and relates to a resin coating liquid suitable for oil lubrication, and a preparation method and application thereof.
Background
The solid lubricating coating is widely applied to high-speed and heavy-load friction pairs of gears and the like, and can play an urgent dry lubricating effect in the process of lubricating oil deficiency, so that the friction pairs are prevented from losing efficacy due to high heat generated by friction. The solid lubricating coating of the polymer matrix is adhered to the substrate by the resin matrix and provides guarantee for the mechanical property of the coating, but the dispersion of the wear-resistant filler in the bulk phase in the coating causes the defect impact resistance of the coating to be reduced, and the abrasion of the coating is often too serious to cause the service life to be low. The prior patent (200810203993.7) related to the polymer resin matrix is poor in oil resistance and impact resistance (impact strength is only 50 cm), and in the patent content of attempting to use graphene as an abrasion-resistant additive (such as 201910375103.9), the dry friction coefficient can be as low as 0.2. The negative influence of the bulk filler on the strength of the resin matrix is reduced, and the method has important significance for reinforcing the performance of the coating.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a resin coating liquid suitable for oil lubrication, and a preparation method and application thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a resin coating liquid suitable for oil lubrication comprises epoxy resin, bulk solid lubricant, organic solvent and curing agent;
the content of the bulk solid lubricant is 15-25 wt%; when the content of the bulk solid lubricant is too small (the proportion of the resin matrix is large), the antifriction and wear-resistant performance of the formed coating is poor; when the content of the bulk solid lubricant is too large, the formed coating has insufficient bonding capability with the metal matrix, and cohesive failure is easy to occur, so that the coating is damaged;
the bulk phase solid lubricant consists of bulk molybdenum disulfide and graphite in a mass ratio of 7:4-6; the average grain diameter of the bulk molybdenum disulfide is 0.1-20 mu m, and the average grain diameter of the graphite is 0.1-10 mu m.
One of the purposes of the invention is to reduce the friction coefficient of the coating, and the invention is specifically solved by designing a bulk phase solid lubricant composed of bulk molybdenum disulfide and graphite with specific proportions and specific sizes, and the principle is as follows:
the mechanism of lubrication macroscopic for solid fillers is explained by the small interlayer van der waals forces of graphite and bulk molybdenum disulfide, which are subject to slip by shear forces and form a continuous transfer film, but the interlayer slip barriers of the two are different. According to researches, in the process of forming ase:Sub>A lubricating film by mixing solid lubricating fillers, the number of layers of bulk molybdenum disulfide and graphite is continuously reduced along with sliding, when two graphite surfaces are in contact with each other in ase:Sub>A metric state (every 60 degrees of rotation), the friction force is greatly reduced when the two graphite surfaces are in relative rotation to be in contact with each other in ase:Sub>A non-metric state (the term is derived from structural super lubrication, the concept is proposed in 1991, experiments prove between nano graphite sheets in 2004, carbon atoms in the graphite are periodically arranged in ase:Sub>A hexagonal mode to form an atomic scale 'peak-valley' landscape, the appearance is like an egg tray in life, when the two graphite surfaces are in contact with each other in ase:Sub>A metric state (every 60 degrees of rotation), the friction force between the two graphite surfaces is greatly reduced when the two graphite surfaces are in relative rotation to be in contact with each other in ase:Sub>A non-metric state, the friction force is like an egg tray in which two mutually contacted, when the two graphite surfaces are rotated to be incapable of being in mutual 'occlusion', the relative sliding is easier to occur, the reduction of the friction force is realized when the two graphite surfaces are in rotation, the interlayer potential barrier is smaller than the bulk molybdenum disulfide-bulk molybdenum disulfide or graphite sheets (the bulk molybdenum disulfide layers are in the number of layers A and B layers are in contact with each other, the friction coefficient is easy to be reduced when the friction coefficient is reduced in the process of the whole layer A-B is similar to the playing card, and the friction coefficient is obviously reduced when the friction coefficient is in the process is compared with the layer B layer is in the shear layer.
To date, structural super-lubrication is still formed under severe conditions, macroscopic friction cannot perfectly show the super-lubrication defined at present, but reduction of particle size and reasonable proportion are still helpful for improving the possibility of heterogeneous non-metric contact in macroscopic friction and reducing friction coefficient theoretically;
the invention controls the average grain diameter of the bulk molybdenum disulfide to be 0.1-20 mu m, and the average grain diameter of the graphite to be 0.1-10 mu m; if the average particle size of the bulk molybdenum disulfide and graphite is too large, the filler is obviously settled in the resin curing process, and finally, the coating is uneven, so that the friction coefficient of the coating is not reduced; if the average particle size of the bulk molybdenum disulfide and graphite is too small, agglomeration is easy to occur, and the quality of the coating is not facilitated;
under the microscopic condition, if graphite and block molybdenum disulfide slide mutually, the sliding potential barrier between layers can be reduced, but under the macroscopic condition, the ratio of the two substances added is different and directly influences the probability of occurrence of the phenomenon under the microscopic condition, so that the value of a specific parameter is required to be found to be an optimal value or a reasonable value through testing; the mass ratio of the bulk molybdenum disulfide to the graphite is controlled to be 7:4-6; if the proportion of the block molybdenum disulfide is too large, the brittleness of the coating is increased, the probability of fatigue wear in the friction process is increased, the texture is softened, the probability of adhesive wear is increased, and the wear resistance of the coating is rapidly reduced; the friction coefficient of the coating is not reduced, and the long service life of the coating is ensured.
In addition, the bulk molybdenum disulfide and graphite have synergistic effect, pure bulk molybdenum disulfide is better in high-vacuum environment but is easily oxidized into molybdenum trioxide by water and oxygen (high in friction coefficient), the friction coefficient of graphite is lower under atmospheric conditions, in the shearing sliding process, the filler is sheared and dispersed on the surface, and the sheared graphite can protect the surface of the bulk molybdenum disulfide from being contacted with water and oxygen if transferred to the upper part of the bulk molybdenum disulfide, and finally can avoid being oxidized.
As a preferable technical scheme:
the resin coating liquid suitable for oil lubrication has the advantages that the average particle size of the bulk molybdenum disulfide is 0.1-5 mu m, and the average particle size of the graphite is 0.1-5 mu m, so that the distribution of the bulk molybdenum disulfide and the graphite in the resin is more uniform, and the occurrence probability of defects on the surface of the coating and internal defects is reduced.
The resin coating liquid suitable for oil lubrication further comprises 3-8wt% of a few-layer molybdenum disulfide, wherein the average particle size of the few-layer molybdenum disulfide is 50 nm-0.5 mu m.
The second purpose of the invention is to enhance the impact resistance and oil resistance of the coating (the invention shows the oil resistance of the coating by testing the pencil hardness and adhesive force of the coating after 30 days of immersion of the coating), and the invention is specifically solved by adding a few layers of molybdenum disulfide, and the principle is as follows:
the few layers of molybdenum disulfide are inorganic functional fillers, which are insoluble in the resin, so the coating that is composed is a two-phase structure (resin and filler). Compared with the bulk molybdenum disulfide with the same mass and large particle size, the specific surface area dispersed in the resin is high, and the resin can be better combined with the resin. In the past researches, the enhancement of the resin by the filler with low content is directly related to the volume fraction, and when the filler content is increased, namely, the situation in the invention, the enhancement of the resin is related to the particle size of the filler, and the smaller the particle size is, the better the enhancement effect (the improvement of the impact resistance) is, and the effect of transmitting load and stress among the resins can be achieved. Large particle size fillers (bulk molybdenum disulfide) at high filler contents act as defects or stress concentration points. The few-layer molybdenum disulfide has very high in-plane strength, the Young modulus of the molybdenum disulfide can be more easily and uniformly dispersed with a resin matrix than that of the shoulder graphene, and the molybdenum disulfide can be used for reinforcing the resin matrix. Compared with few layers of molybdenum disulfide, the particle size of the bulk molybdenum disulfide is larger, and the bulk molybdenum disulfide is applied in a coating by virtue of interlayer slippage as a lubricant, but the bulk molybdenum disulfide is used as a filler and is easy to generate local defects. The liquid phase exfoliated less molybdenum disulfide is neither hydrophilic nor oleophilic, and when added as a filler into a coating, is more oleophobic (enhanced oil resistance) than the resin matrix.
In addition, the few-layer molybdenum disulfide has fewer defect sites in the surface than graphene, and the thermal property and lubrication performance under the environment of oil are more stable than those of graphene. Most importantly, besides being used as an extremely fine filler for reinforcing by dispersing stress in resin, a few layers of molybdenum disulfide serve as transition metal compounds to have metal bond action with a metal substrate covered by the coating, so that stronger bonding capability with the metal substrate is provided, and the coating adhesion capability is remarkably improved.
Furthermore, the addition of a suitable amount of a small layer of molybdenum disulfide to the coating will more readily result in the aforementioned reduction in coefficient of friction due to non-metric contact during the transfer film generation stage.
The invention controls the content of the few-layer molybdenum disulfide to be 3-8wt% because the few-layer molybdenum disulfide is also added as a solid phase substance, and the excessive addition amount can also cause the increase of the total content of the coating filler and the decrease of the strength; if too little, the mechanical enhancement performance and antifriction and wear-resistant performance of the composite material are not obviously improved; the average particle size of the few-layer molybdenum disulfide is controlled to be 50-500 nm, because the few-layer molybdenum disulfide with the overlarge particle size can generate autonomous shrinkage and curling due to large surface energy of the few-layer molybdenum disulfide, the occurrence of sliding is not facilitated, and the preparation cost is higher due to the overlarge particle size, and the few-layer molybdenum disulfide is prone to autonomous agglomeration and difficult to preserve for a long time.
The preparation process of the resin coating liquid suitable for oil lubrication and the few-layer molybdenum disulfide comprises the following steps: drying bulk molybdenum disulfide (the temperature is 80 ℃ and the time is 2-4 h), adding the bulk molybdenum disulfide into N-methyl pyrrolidone (the N-methyl pyrrolidone can be replaced by 80% isopropanol solution, but the N-methyl pyrrolidone is the solvent with the surface energy closest to that of the molybdenum disulfide, the stripping effect is highest) to obtain 50-80 mg/ml dispersion liquid, carrying out ultrasonic treatment at the power of 250-600W for 4-12 h at the temperature of 25-35 ℃ to obtain suspension containing few layers of molybdenum disulfide, carrying out post-treatment (centrifugal separation at the rotating speed of 10000rpm for 30min to obtain supernatant, adding 25% ethanol solution for repeated centrifugation and washing until the N-methyl pyrrolidone is completely replaced, and carrying out freeze-drying after centrifugal precipitation is dispersed in the 25% ethanol solution) to obtain the few layers of molybdenum disulfide.
A resin coating liquid suitable for oil lubrication as described above further comprises 0.1 to 1wt% of an additive.
One such resin coating fluid suitable for oil lubrication is described above, and the additive is dispersant Tech-6325 and/or leveling agent MHC60-6100.
The resin coating liquid is suitable for oil lubrication, the content of epoxy resin is 20-40 wt%, the content of organic solvent is 20-65 wt%, and the content of curing agent is 1-5 wt%.
One such resin coating fluid suitable for oil lubrication is described above, the epoxy resin being bisphenol A type epoxy resin YD-128 and/or bisphenol A type resin KSR-177; the curing agent is dicyandiamide; the organic solvent consists of acetone, 2-butanone, cyclohexanone and N, N-dimethylformamide, the volume ratio of the acetone, the 2-butanone and the cyclohexanone is 2:1:1, and the mass ratio of the N, N-dimethylformamide to the curing agent is 2-4:1.
The invention also provides a method for preparing the resin coating liquid suitable for oil lubrication, which comprises the following steps:
(1) Adding a curing agent into N, N-dimethylformamide, and uniformly oscillating to obtain a clear solution;
(2) Uniformly mixing epoxy resin and a clarified solution to obtain a resin glue solution;
(3) Drying the block molybdenum disulfide and graphite (the temperature is 80 ℃ and the time is 2-4 h), mixing with resin glue solution, acetone, 2-butanone, cyclohexanone and additives, and performing ultrasonic dispersion for 30-60 min to obtain mixed glue solution;
(4) Filtering the mixed glue solution by using a 300-800-mesh gauze (the purpose of the filtering step is to obtain filler particles with finer particle size and narrower dispersion, or directly sieving the filler after the filler is dried to remove large-particle filler, and then adding the dispersion solution and the glue solution to obtain filtrate;
(5) Adding a few layers of molybdenum disulfide into the filtrate, and performing ultrasonic treatment for 30-60 min after shearing to obtain the resin coating liquid suitable for oil lubrication.
The invention also provides an application of the resin coating liquid suitable for oil lubrication, which is characterized in that after stirring and ultrasonic pre-dispersing for 20min, the resin coating liquid is sprayed on the surface of a metal substrate by an air spray gun and is solidified for 50-70 min at 165-175 ℃ to obtain a coating.
As a preferable technical scheme:
by the application, the thickness of the coating is 20-30 mu m, the impact resistance height is 40-45 cm, the friction coefficient of the coating is 0.03-0.045, and the wear rate of the coating is 0.260 multiplied by 10 -6 ～0.430×10 -6 mm 3 And (3) the adhesive force of the coating is 0 grade, the pencil hardness is 5H, the adhesive force of the coating is 0-1 grade after 30 days of oil immersion, and the pencil hardness is 3-4H.
The beneficial effects are that:
(1) The resin coating prepared by the invention has higher impact resistance height, adhesive force and pencil hardness on a metal substrate, and simultaneously has excellent low friction coefficient (the dry friction coefficient in the prior art can be as low as 0.2 at least, and the friction coefficient of the coating is further reduced by more than one order of magnitude compared with the prior art) and low wear rate, and the performances are kept unchanged after the coating is soaked in lubricating oil for thirty days;
(2) The preparation method is simple and efficient for preparing the few-layer molybdenum disulfide, and the key solvent can be recycled, so that the method is environment-friendly;
(3) The preparation method of the resin coating liquid has simple steps and rapid and efficient curing.
Drawings
FIG. 1 is a scanning image of the wear scar of the coating prepared in example 5 under a 350X scanning electron microscope;
FIG. 2 is a scan image and EDS spectrum of the wear scar of the coating made in example 5 under 4500 Xscanning electron microscope; in the figure, (a) is a scanning image of a grinding mark under a 4500X scanning electron microscope, and (b), (c) and (d) are EDS energy spectrums at white frames in (a); the EDS energy spectrum shows that the lower right corner of the white frame is enriched with Mo element, S element and Si element, and the combination image shows that the molybdenum disulfide sheet with the regular lower right corner of the white frame forms a film on the exposed surface, so that friction pairs are formed between resin and a metal steel ring, and the friction coefficient is reduced; the lower part of the white frame is coated with the resin, so that the stress is dispersed, the coating is enhanced, and the wear rate is reduced; part of the few layers of molybdenum disulfide are exposed on the surface in the friction process, so that the friction coefficient is further reduced;
FIG. 3 is an XRD image of bulk molybdenum disulfide before and after ultrasonic stripping; as can be seen by comparing the peak position with a standard PDF card, the crystal structure of the bulk molybdenum disulfide is 2H-type molybdenum disulfide, is the most stable molybdenum disulfide crystal structure with the smallest sliding potential barrier, and the intensity of each peak is obviously reduced after ultrasonic stripping, so that the orientation degree of the molybdenum disulfide in the crystal face direction is reduced, namely the molybdenum disulfide is stripped from top to bottom, the incomplete disappearance of the peak indicates that the molybdenum disulfide is not completely stripped to a single layer, and the success of the preparation of the few-layer molybdenum disulfide is proved.
Detailed Description
The invention is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Sources of related substances in the examples:
bisphenol A type epoxy resin YD-128: the manufacturer is Kunshan national chemical industry Co., ltd;
bisphenol A resin KSR-177: the manufacturer is Kunshan national chemical industry Co., ltd;
block molybdenum disulfide: the manufacturer is Shanghai colloid chemical industry Co., ltd, and the brand is MF-0;
graphite: the brand is SIAL, the product number is NISTRM8541;
dispersant Tech-6325: the manufacturer is Shanghai Tager polymer technology Co., ltd;
leveling agent MHC60-6100: the manufacturer is Shanghai Tager Polymer technology Co.
The detection method of the correlation performance in the embodiment comprises the following steps:
soaking the coating in oil for 30 days, namely soaking the prepared coating in lubricating oil (the manufacturer is Beijing Xingpe fine chemical industry, the brand is RIPP 550) at 25 ℃ for 30 days;
coating adhesion: coating adhesion was tested with reference to standard GB 1720-79;
coating pencil hardness: the hardness of the coated pencil was tested with reference to standard GB/T6739-2022;
coating impact height: the impact height of the coating was tested with reference to standard GB/T1732-93;
coefficient of friction of the coating: curing the resin coating liquid prepared in the embodiment on a Q235 carbon steel plate with the length and width of 25 multiplied by 7 multiplied by 4mm to form a test block, testing at 25 ℃ by using an M-2000J type friction and wear tester with reference to standard GB/T12444-2006, adding a peristaltic pump and an oil box for circulating oil injection lubrication during the testing process, sampling once every 0.1 second, and recording friction coefficient data; removing data with errors greater than 6 standard deviations and taking the arithmetic average value of the residual data as the friction coefficient of the sample; the test ring is a GCr15 steel ring with a standard diameter of 36mm, which is matched with a testing machine, the test loads are respectively 50N, 100N, 150N and 200N, the test is carried out for 30min under each load, and the linear speed of the steel ring is 0.42m/s;
wear rate of the coating: curing the resin coating liquid prepared in the embodiment on a Q235 carbon steel plate with the length and width of 25 multiplied by 7 multiplied by 4mm to form a test block, and testing at 25 ℃ by using an M-2000J type friction and wear testing machine with reference to standard GB/T12444-2006 to obtain the wear volume and the wear range of the test block; wherein the test ring is a GCr15 steel ring with a standard diameter of 36mm, which is matched with a testing machine, the test time is 30min, and the linear speed of the steel ring is 0.42m/s; the wear rate of the coating was then calculated according to the following formula:
W s ＝V s /L·F；
in which W is s Wear rate (mm) 3 /(N·m))，V s Wear volume (mm) 3 ) L-milling (m), F-load (N);
three replicates were run to take the arithmetic mean.
Example 1
The preparation method of the resin coating liquid suitable for oil lubrication comprises the following specific steps:
(1) Preparing materials:
acetone;
2-butanone;
cyclohexanone;
n, N-dimethylformamide;
epoxy resin: a mixture of bisphenol A type epoxy resin YD-128 and bisphenol A type resin KSR-177 in a mass ratio of 1:3;
bulk solid lubricant: consists of bulk molybdenum disulfide and graphite in a mass ratio of 7:4; wherein, the average grain diameter of the bulk molybdenum disulfide is 20 mu m, and the average grain diameter of the graphite is 2 mu m;
curing agent: dicyandiamide;
additive: dispersant Tech-6325 and flatting agent MHC60-6100 mixture with a mass ratio of 2:1;
few-layer molybdenum disulfide: the preparation process comprises the following steps: drying bulk molybdenum disulfide for 2 hours at 80 ℃, adding the bulk molybdenum disulfide into N-methyl pyrrolidone to obtain a dispersion liquid with the concentration of 50mg/ml, carrying out ultrasonic treatment at the power of 250W for 12 hours at 30 ℃ to obtain a suspension containing less molybdenum disulfide, carrying out centrifugal separation at the rotating speed of 10000rpm for 30 minutes to obtain a supernatant, adding 25% ethanol solution, repeatedly centrifuging and washing until the N-methyl pyrrolidone is completely replaced, dispersing the centrifugal precipitate in the 25% ethanol solution, and carrying out freeze-drying to obtain the less molybdenum disulfide with the average particle size of 500 nm;
(2) Preparing a resin coating liquid:
(2.1) adding a curing agent into N, N-dimethylformamide, and uniformly oscillating to obtain a clear solution;
(2.2) uniformly mixing epoxy resin and the clarified solution to obtain resin glue solution;
(2.3) drying the bulk solid lubricant for 2 hours at the temperature of 80 ℃, mixing with resin glue solution, acetone, 2-butanone, cyclohexanone and additives, and performing ultrasonic dispersion for 30 minutes to obtain mixed glue solution;
(2.4) filtering the mixed glue solution through a 300-mesh gauze to obtain filtrate;
(2.5) adding a few layers of molybdenum disulfide into the filtrate, shearing for 10min at a shearing speed of 1000rpm, and continuing ultrasonic treatment for 30min to obtain the resin coating liquid suitable for oil lubrication.
In the finally prepared resin coating liquid suitable for oil lubrication, the volume ratio of acetone, 2-butanone and cyclohexanone is 2:1:1, the mass ratio of N, N-dimethylformamide to a curing agent is 3:1, the content of an organic solvent consisting of acetone, 2-butanone, cyclohexanone and N, N-dimethylformamide is 42.9wt%, the content of a bulk phase solid lubricant is 15wt%, the content of less molybdenum disulfide is 8wt%, the content of an additive is 0.1wt%, the content of epoxy resin is 32wt%, and the content of the curing agent is 2wt%.
The application of the resin coating liquid suitable for oil lubrication comprises the steps of carrying out ultrasonic treatment on the resin coating liquid prepared by the method for 20min, spraying the resin coating liquid on the surface of a carbon steel sheet by using an air spray gun at the pressure of 0.24bar, and curing the resin coating liquid at 165 ℃ for 70min to obtain a coating;
the thickness of the obtained coating is 24.39 μm, the impact height is 41cm, the friction coefficient is 0.043, and the abrasion rate is 0.427 multiplied by 10 -6 mm 3 and/(N.m), the adhesive force is 0 level, the pencil hardness is 5H, the adhesive force after soaking in oil for 30 days is 1 level, and the pencil hardness is 3H.
Comparative example 1
A method for preparing a resin coating liquid, which is basically the same as in example 1, except that: in the step (1), the mass ratio of the molybdenum disulfide to the graphite in the bulk solid lubricant is 7:2.
The application of the resin coating liquid was basically the same as in example 1, except that: the resin coating liquid used was the resin coating liquid prepared in this comparative example;
the obtained coating has an impact height of 34cm, a friction coefficient NA (no average statistics in 30 min) and a wear rate of 2.612×10 -6 mm 3 and/(N.m), the adhesion was 0 grade, and the pencil hardness was 2H.
Comparative example 1 compared with example 1, comparative example 1 was reduced in pencil hardness and impact height of the coating because the coating becomes brittle due to excessive molybdenum disulfide content in the bulk solid lubricant, and the coating could not have sufficient abrasion resistance due to insufficient graphite content of soft texture, and the coating failed the test for 30min, namely, broken, to be worn through to the substrate in the test, and the abrasion rate was large.
Example 2
The preparation method of the resin coating liquid suitable for oil lubrication comprises the following specific steps:
(1) Preparing materials:
acetone;
2-butanone;
cyclohexanone;
n, N-dimethylformamide;
epoxy resin: a mixture of bisphenol A epoxy resin YD-128 and bisphenol A resin KSR-177 in a mass ratio of 1:2;
bulk solid lubricant: consists of bulk molybdenum disulfide and graphite in a mass ratio of 7:6; the average grain diameter of the bulk molybdenum disulfide is 8 mu m, and the average grain diameter of the graphite is 5 mu m;
curing agent: dicyandiamide;
additive: dispersant Tech-6325 and flatting agent MHC60-6100 mixture with a mass ratio of 1:2;
few-layer molybdenum disulfide: the preparation process comprises the following steps: drying bulk molybdenum disulfide for 2 hours at 80 ℃, adding the bulk molybdenum disulfide into N-methyl pyrrolidone to obtain a dispersion liquid with the concentration of 60mg/ml, carrying out ultrasonic treatment at the power of 350W for 10 hours at 30 ℃ to obtain a suspension containing less molybdenum disulfide, carrying out centrifugal separation at the rotating speed of 10000rpm for 30 minutes to obtain a supernatant, adding 25% ethanol solution, repeatedly centrifuging and washing until the N-methyl pyrrolidone is completely replaced, dispersing the centrifugal precipitate in the 25% ethanol solution, and carrying out freeze-drying to obtain the less molybdenum disulfide with the average particle size of 500 nm;
(2) Preparing a resin coating liquid:
(2.1) adding a curing agent into N, N-dimethylformamide, and uniformly oscillating to obtain a clear solution;
(2.2) uniformly mixing epoxy resin and the clarified solution to obtain resin glue solution;
(2.3) drying the bulk solid lubricant for 4 hours at the temperature of 80 ℃, mixing with resin glue solution, acetone, 2-butanone, cyclohexanone and additives, and performing ultrasonic dispersion for 30 minutes to obtain mixed glue solution;
(2.4) filtering the mixed glue solution through a 300-mesh gauze to obtain filtrate;
(2.5) adding a few layers of molybdenum disulfide into the filtrate, shearing for 10min at a shearing speed of 1000rpm, and continuing ultrasonic treatment for 60min to obtain the resin coating liquid suitable for oil lubrication.
In the finally prepared resin coating liquid suitable for oil lubrication, the volume ratio of acetone, 2-butanone and cyclohexanone is 2:1:1, the mass ratio of N, N-dimethylformamide to a curing agent is 2.5:1, the content of an organic solvent consisting of acetone, 2-butanone, cyclohexanone and N, N-dimethylformamide is 21wt%, the content of a bulk phase solid lubricant is 25wt%, the content of a few-layer molybdenum disulfide is 8wt%, the content of an additive is 1wt%, the content of epoxy resin is 40wt%, and the content of a curing agent is 5wt%.
The resin coating liquid is sprayed on the surface of a carbon steel sheet by an air spray gun at the pressure of 0.24bar after ultrasonic treatment for 20min, and is cured for 60min at 170 ℃ to obtain a coating;
the thickness of the obtained coating is 21.98 μm, the impact height is 43cm, the friction coefficient is 0.041, and the abrasion rate is 0.381×10 -6 mm 3 and/(N.m), the adhesive force is 0 level, the pencil hardness is 5H, the adhesive force after soaking in oil for 30 days is 0 level, and the pencil hardness is 4H.
Comparative example 2
A method for preparing a resin coating liquid, which is basically the same as in example 2, except that: in the step (1), the mass ratio of the molybdenum disulfide to the graphite in the bulk solid lubricant is 1:1.
The application of the resin coating liquid was basically the same as in example 2, except that: the resin coating liquid used was the resin coating liquid prepared in this comparative example;
the obtained coating has impact height of 36cm, friction coefficient NA (no average statistics in 30 min) and abrasion rate of 13.368 ×10 -6 mm 3 and/(N.m), the adhesion was grade 2, and the pencil hardness was 2H.
Compared with the comparative example 2, the performance indexes of the comparative example 2 are greatly reduced because the graphite content is higher and the molybdenum disulfide content is too small, so that the texture is softened, the adhesive wear probability is increased, and the wear resistance of the coating is sharply reduced; meanwhile, the graphite has poor antifriction and wear-resistant performance in the oil environment, and the coating loses severely after oil immersion, so that the coating fails.
Example 3
The preparation method of the resin coating liquid suitable for oil lubrication comprises the following specific steps:
(1) Preparing materials:
acetone;
2-butanone;
cyclohexanone;
n, N-dimethylformamide;
epoxy resin: bisphenol A type epoxy resin YD-128;
bulk solid lubricant: consists of bulk molybdenum disulfide and graphite in a mass ratio of 7:5; the average grain diameter of the bulk molybdenum disulfide is 1 mu m, and the average grain diameter of the graphite is 6 mu m;
curing agent: dicyandiamide;
additive: dispersant Tech-6325 and flatting agent MHC60-6100 mixture with a mass ratio of 3:1;
few-layer molybdenum disulfide: the preparation process comprises the following steps: drying bulk molybdenum disulfide for 2.5 hours at 80 ℃, adding the bulk molybdenum disulfide into N-methyl pyrrolidone to obtain a dispersion liquid with the concentration of 55mg/ml, carrying out ultrasonic treatment at the power of 550W for 6 hours at 35 ℃ to obtain a suspension containing less molybdenum disulfide, carrying out centrifugal separation at the rotating speed of 10000rpm for 30 minutes to obtain a supernatant, adding 25% ethanol solution, repeatedly centrifuging and washing until the N-methyl pyrrolidone is completely replaced, dispersing the centrifugal precipitate in the 25% ethanol solution, and carrying out freeze-drying to obtain the less molybdenum disulfide with the average particle size of 350 nm;
(2) Preparing a resin coating liquid:
(2.1) adding a curing agent into N, N-dimethylformamide, and uniformly oscillating to obtain a clear solution;
(2.2) uniformly mixing epoxy resin and the clarified solution to obtain resin glue solution;
(2.3) drying the bulk solid lubricant for 2.5 hours at the temperature of 80 ℃, mixing with resin glue solution, acetone, 2-butanone, cyclohexanone and additives, and performing ultrasonic dispersion for 45 minutes to obtain mixed glue solution;
(2.4) filtering the mixed glue solution through a screen with 800 meshes to obtain filtrate;
(2.5) adding a few layers of molybdenum disulfide into the filtrate, shearing for 10min at a shearing speed of 1000rpm, and continuing ultrasonic treatment for 60min to obtain the resin coating liquid suitable for oil lubrication.
In the finally prepared resin coating liquid suitable for oil lubrication, the volume ratio of acetone, 2-butanone and cyclohexanone is 2:1:1, the mass ratio of N, N-dimethylformamide to a curing agent is 2:1, the content of an organic solvent consisting of acetone, 2-butanone, cyclohexanone and N, N-dimethylformamide is 64.9wt%, the content of a bulk phase solid lubricant is 15wt%, the content of less molybdenum disulfide is 3wt%, the content of an additive is 0.1wt%, the content of epoxy resin is 16wt%, and the content of the curing agent is 1wt%.
The application of the resin coating liquid suitable for oil lubrication comprises the steps of carrying out ultrasonic treatment on the resin coating liquid prepared by the method for 20min, spraying the resin coating liquid on the surface of a carbon steel sheet by using an air spray gun at the pressure of 0.24bar, and curing the resin coating liquid at 175 ℃ for 50min to obtain a coating;
the obtained coating has a thickness of 29.88 μm, an impact height of 40cm, a friction coefficient of 0.038 and a wear rate of 0.366×10 -6 mm 3 and/(N.m), the adhesive force is 0 level, the pencil hardness is 5H, the adhesive force after soaking in oil for 30 days is 0 level, and the pencil hardness is 4H.
Example 4
The preparation method of the resin coating liquid suitable for oil lubrication comprises the following specific steps:
(1) Preparing materials:
acetone;
2-butanone;
cyclohexanone;
n, N-dimethylformamide;
epoxy resin: bisphenol a resin KSR-177;
bulk solid lubricant: consists of bulk molybdenum disulfide and graphite in a mass ratio of 14:9; the average grain diameter of the bulk molybdenum disulfide is 5 mu m, and the average grain diameter of the graphite is 10 mu m;
curing agent: dicyandiamide;
additive: dispersant Tech-6325;
few-layer molybdenum disulfide: the preparation process comprises the following steps: drying bulk molybdenum disulfide for 3 hours at 80 ℃, adding the bulk molybdenum disulfide into N-methyl pyrrolidone to obtain a dispersion liquid with the concentration of 65mg/ml, carrying out ultrasonic treatment at 25 ℃ under the power of 250W for 12 hours to obtain a suspension containing less molybdenum disulfide, carrying out centrifugal separation at the rotating speed of 10000rpm for 30 minutes to obtain a supernatant, adding 25% ethanol solution, repeatedly centrifuging and washing until the N-methyl pyrrolidone is completely replaced, dispersing the centrifugal precipitate in the 25% ethanol solution, and carrying out freeze-drying to obtain the less molybdenum disulfide with the average particle size of 500 nm;
(2) Preparing a resin coating liquid:
(2.1) adding a curing agent into N, N-dimethylformamide, and uniformly oscillating to obtain a clear solution;
(2.2) uniformly mixing epoxy resin and the clarified solution to obtain resin glue solution;
(2.3) drying the bulk solid lubricant for 3 hours at the temperature of 80 ℃, mixing with resin glue solution, acetone, 2-butanone, cyclohexanone and additives, and performing ultrasonic dispersion for 60 minutes to obtain mixed glue solution;
(2.4) filtering the mixed glue solution through a 500-mesh gauze to obtain filtrate;
(2.5) adding a few layers of molybdenum disulfide into the filtrate, shearing for 10min at a shearing speed of 1000rpm, and continuing ultrasonic treatment for 60min to obtain the resin coating liquid suitable for oil lubrication.
In the finally prepared resin coating liquid suitable for oil lubrication, the volume ratio of acetone, 2-butanone and cyclohexanone is 2:1:1, the mass ratio of N, N-dimethylformamide to a curing agent is 4:1, the content of an organic solvent consisting of acetone, 2-butanone, cyclohexanone and N, N-dimethylformamide is 55wt%, the content of a bulk phase solid lubricant is 15wt%, the content of a few-layer molybdenum disulfide is 3wt%, the content of an additive is 0.5wt%, the content of epoxy resin is 25wt%, and the content of the curing agent is 1.5wt%.
The application of the resin coating liquid suitable for oil lubrication comprises the steps of carrying out ultrasonic treatment on the resin coating liquid prepared by the method for 20min, spraying the resin coating liquid on the surface of a carbon steel sheet by using an air spray gun at the pressure of 0.24bar, and curing the resin coating liquid at 165 ℃ for 70min to obtain a coating;
the thickness of the obtained coating is 20.15 μm, the impact height is 43cm, and the friction is generatedCoefficient of 0.039, wear rate of 0.324×10 -6 mm 3 and/(N.m), the adhesive force is 0 level, the pencil hardness is 5H, the adhesive force after soaking in oil for 30 days is 0 level, and the pencil hardness is 4H.
Example 5
The preparation method of the resin coating liquid suitable for oil lubrication comprises the following specific steps:
(1) Preparing materials:
acetone;
2-butanone;
cyclohexanone;
n, N-dimethylformamide;
epoxy resin: a mixture of bisphenol A type epoxy resin YD-128 and bisphenol A type resin KSR-177 in a mass ratio of 1:1;
bulk solid lubricant: consists of bulk molybdenum disulfide and graphite in a mass ratio of 14:11; the average grain diameter of the bulk molybdenum disulfide is 4 mu m, and the average grain diameter of the graphite is 8 mu m;
curing agent: dicyandiamide;
additive: leveling agent MHC60-6100;
few-layer molybdenum disulfide: the preparation process comprises the following steps: drying bulk molybdenum disulfide for 3.5 hours at 80 ℃, adding the bulk molybdenum disulfide into N-methyl pyrrolidone to obtain a dispersion liquid with the concentration of 70mg/ml, carrying out ultrasonic treatment at 25 ℃ under 600W power for 12 hours to obtain a suspension containing less molybdenum disulfide, carrying out centrifugal separation at 10000rpm for 30 minutes to obtain a supernatant, adding 25% ethanol solution, repeatedly centrifuging and washing until the N-methyl pyrrolidone is completely replaced, dispersing the centrifugal precipitate in the 25% ethanol solution, and carrying out freeze-drying to obtain the less molybdenum disulfide with the average particle size of 50 nm;
(2) Preparing a resin coating liquid:
(2.1) adding a curing agent into N, N-dimethylformamide, and uniformly oscillating to obtain a clear solution;
(2.2) uniformly mixing epoxy resin and the clarified solution to obtain resin glue solution;
(2.3) drying the bulk solid lubricant for 3.5 hours at the temperature of 80 ℃, mixing with resin glue solution, acetone, 2-butanone, cyclohexanone and additives, and performing ultrasonic dispersion for 60 minutes to obtain mixed glue solution;
(2.4) filtering the mixed glue solution through a 500-mesh gauze to obtain filtrate;
(2.5) adding a few layers of molybdenum disulfide into the filtrate, shearing for 10min at a shearing speed of 1000rpm, and continuing ultrasonic treatment for 30min to obtain the resin coating liquid suitable for oil lubrication.
In the finally prepared resin coating liquid suitable for oil lubrication, the volume ratio of acetone, 2-butanone and cyclohexanone is 2:1:1, the mass ratio of N, N-dimethylformamide to a curing agent is 4:1, the content of an organic solvent consisting of acetone, 2-butanone, cyclohexanone and N, N-dimethylformamide is 45wt%, the content of a bulk phase solid lubricant is 15wt%, the content of a few-layer molybdenum disulfide is 4wt%, the content of an additive is 1wt%, the content of epoxy resin is 32wt%, and the content of the curing agent is 3wt%.
The resin coating liquid is sprayed on the surface of a carbon steel sheet by an air spray gun at the pressure of 0.24bar after ultrasonic treatment for 20min, and is cured for 60min at 170 ℃ to obtain a coating;
the thickness of the obtained coating is 26.32 μm, the impact height is 45cm, the friction coefficient is 0.035, and the abrasion rate is 0.268 multiplied by 10 -6 mm 3 and/(N.m), the adhesive force is 0 level, the pencil hardness is 5H, the adhesive force after soaking in oil for 30 days is 0 level, and the pencil hardness is 4H.
Example 6
The preparation method of the resin coating liquid suitable for oil lubrication comprises the following specific steps:
(1) Preparing materials:
acetone;
2-butanone;
cyclohexanone;
n, N-dimethylformamide;
epoxy resin: a mixture of bisphenol A epoxy resin YD-128 and bisphenol A resin KSR-177 in a mass ratio of 2:1;
bulk solid lubricant: consists of bulk molybdenum disulfide and graphite in a mass ratio of 14:11; the average grain diameter of the bulk molybdenum disulfide is 6 mu m, and the average grain diameter of the graphite is 4 mu m;
curing agent: dicyandiamide;
additive: a dispersant Tech-6325 and flatting agent MHC60-6100 mixture with a mass ratio of 1:1;
few-layer molybdenum disulfide: the preparation process comprises the following steps: drying bulk molybdenum disulfide for 4 hours at 80 ℃, adding the bulk molybdenum disulfide into N-methyl pyrrolidone to obtain a dispersion liquid with the concentration of 80mg/ml, carrying out ultrasonic treatment at 25 ℃ under 400W power for 8 hours to obtain a suspension containing less molybdenum disulfide, carrying out centrifugal separation at 10000rpm for 30 minutes to obtain a supernatant, adding 25% ethanol solution, repeatedly centrifuging and washing until the N-methyl pyrrolidone is completely replaced, dispersing the centrifugal precipitate in the 25% ethanol solution, and carrying out freeze-drying to obtain the less molybdenum disulfide with the average particle size of 150 nm;
(2) Preparing a resin coating liquid:
(2.1) adding a curing agent into N, N-dimethylformamide, and uniformly oscillating to obtain a clear solution;
(2.2) uniformly mixing epoxy resin and the clarified solution to obtain resin glue solution;
(2.3) drying the bulk solid lubricant for 4 hours at the temperature of 80 ℃, mixing the solid lubricant with resin glue solution, acetone, 2-butanone, cyclohexanone and additives, and performing ultrasonic dispersion for 45 minutes to obtain mixed glue solution;
(2.4) filtering the mixed glue solution through a 500-mesh gauze to obtain filtrate;
(2.5) adding a few layers of molybdenum disulfide into the filtrate, shearing for 10min at a shearing speed of 1000rpm, and continuing ultrasonic treatment for 30min to obtain the resin coating liquid suitable for oil lubrication.
In the finally prepared resin coating liquid suitable for oil lubrication, the volume ratio of acetone, 2-butanone and cyclohexanone is 2:1:1, the mass ratio of N, N-dimethylformamide to a curing agent is 3:1, the content of an organic solvent consisting of acetone, 2-butanone, cyclohexanone and N, N-dimethylformamide is 40wt%, the content of a bulk phase solid lubricant is 20wt%, the content of a few-layer molybdenum disulfide is 5wt%, the content of an additive is 1wt%, the content of epoxy resin is 32wt%, and the content of the curing agent is 2wt%.
The application of the resin coating liquid suitable for oil lubrication comprises the steps of carrying out ultrasonic treatment on the resin coating liquid prepared by the method for 20min, spraying the resin coating liquid on the surface of a carbon steel sheet by using an air spray gun at the pressure of 0.24bar, and curing the resin coating liquid at 175 ℃ for 50min to obtain a coating;
the thickness of the obtained coating is 24.53 μm, the impact height is 41cm, the friction coefficient is 0.041, and the abrasion rate is 0.339 multiplied by 10 -6 mm 3 and/(N.m), the adhesive force is 0 level, the pencil hardness is 5H, the adhesive force after soaking in oil for 30 days is 0 level, and the pencil hardness is 4H.
Claims (11)
1. A resin coating liquid suitable for oil lubrication is characterized by comprising epoxy resin, bulk solid lubricant, organic solvent and curing agent;
the content of the bulk solid lubricant is 15-25 wt%;
the bulk phase solid lubricant consists of bulk molybdenum disulfide and graphite in a mass ratio of 7:4-6; the average grain diameter of the bulk molybdenum disulfide is 0.1-20 mu m, and the average grain diameter of the graphite is 0.1-10 mu m.
2. The resin coating liquid for oil lubrication according to claim 1, wherein the average particle size of the bulk molybdenum disulfide is 0.1 to 5 μm and the average particle size of the graphite is 0.1 to 5 μm.
3. The resin coating liquid for oil lubrication according to claim 1, further comprising 3 to 8wt% of a small layer of molybdenum disulfide, the small layer of molybdenum disulfide having an average particle diameter of 50nm to 0.5 μm.
4. A resin coating liquid suitable for oil lubrication according to claim 3, wherein the preparation process of the few-layer molybdenum disulfide is: and (3) drying the block molybdenum disulfide, adding the block molybdenum disulfide into N-methyl pyrrolidone to obtain a dispersion liquid with the concentration of 50-80 mg/ml, carrying out ultrasonic treatment at the power of 250-600W for 4-12 hours at the temperature of 25-35 ℃ to obtain a suspension containing few layers of molybdenum disulfide, and carrying out post-treatment to obtain the few layers of molybdenum disulfide.
5. A resin coating liquid suitable for oil lubrication according to claim 3, further comprising 0.1 to 1wt% of an additive.
6. The resin coating liquid for oil lubrication according to claim 5, wherein the additive is a dispersant Tech-6325 and/or a leveling agent MHC60-6100.
7. The resin coating liquid for oil lubrication according to claim 5, wherein the content of the epoxy resin is 20 to 40wt%, the content of the organic solvent is 20 to 65wt%, and the content of the curing agent is 1 to 5wt%.
8. A resin coating liquid suitable for oil lubrication according to claim 7, wherein the epoxy resin is bisphenol a type epoxy resin YD-128 and/or bisphenol a type resin KSR-177; the curing agent is dicyandiamide; the organic solvent consists of acetone, 2-butanone, cyclohexanone and N, N-dimethylformamide, wherein the volume ratio of the acetone, the 2-butanone and the cyclohexanone is 2:1:1, and the mass ratio of the N, N-dimethylformamide to the curing agent is 2-4:1.
9. A method for preparing a resin coating liquid suitable for oil lubrication according to any one of claims 1 to 8, comprising the steps of:
(1) Adding a curing agent into N, N-dimethylformamide, and uniformly oscillating to obtain a clear solution;
(2) Uniformly mixing epoxy resin and a clarified solution to obtain a resin glue solution;
(3) Drying the block molybdenum disulfide and graphite, mixing with resin glue solution, acetone, 2-butanone, cyclohexanone and additives, and performing ultrasonic dispersion for 30-60 min to obtain mixed glue solution;
(4) Filtering the mixed glue solution to obtain filtrate;
(5) Adding a few layers of molybdenum disulfide into the filtrate, and performing ultrasonic treatment for 30-60 min after shearing to obtain the resin coating liquid suitable for oil lubrication.
10. Use of a resin coating liquid for oil lubrication according to any of claims 1-8, wherein the resin coating liquid is sprayed onto the surface of a metal substrate and cured to obtain the coating.
11. The use according to claim 10, wherein the coating has a thickness of 20 to 30 μm, an impact height of 40 to 45cm, a coefficient of friction of 0.03 to 0.045 and a wear rate of 0.260 x 10 -6 ～0.430×10 -6 mm 3 And (3) the adhesive force of the coating is 0 grade, the pencil hardness is 5H, the adhesive force of the coating is 0-1 grade after 30 days of oil immersion, and the pencil hardness is 3-4H.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310567256.XA CN116535933A (en) | 2023-05-19 | 2023-05-19 | Resin coating liquid suitable for oil lubrication and preparation method and application thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4329238A (en) * | 1979-07-30 | 1982-05-11 | Mitrofanova Alla K | Antifriction paste and solid antifriction coating prepared from same |
| US20030186060A1 (en) * | 2002-04-02 | 2003-10-02 | Ford Motor Company | Low wear and low friction coatings for articles made of low softening point materials |
| CN1470625A (en) * | 2003-06-17 | 2004-01-28 | 燕山大学 | Expanded grahpite/molybdenum disulfide composite solid lubricating material and its preparing process |
| CN102002302A (en) * | 2010-11-17 | 2011-04-06 | 安庆中船柴油机有限公司 | Liquid coating and preparation method thereof |
| CN104495936A (en) * | 2014-12-12 | 2015-04-08 | 电子科技大学 | Preparation method of stratified molybdenum disulfide nano material |
-
2023
- 2023-05-19 CN CN202310567256.XA patent/CN116535933A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4329238A (en) * | 1979-07-30 | 1982-05-11 | Mitrofanova Alla K | Antifriction paste and solid antifriction coating prepared from same |
| US20030186060A1 (en) * | 2002-04-02 | 2003-10-02 | Ford Motor Company | Low wear and low friction coatings for articles made of low softening point materials |
| CN1470625A (en) * | 2003-06-17 | 2004-01-28 | 燕山大学 | Expanded grahpite/molybdenum disulfide composite solid lubricating material and its preparing process |
| CN102002302A (en) * | 2010-11-17 | 2011-04-06 | 安庆中船柴油机有限公司 | Liquid coating and preparation method thereof |
| CN104495936A (en) * | 2014-12-12 | 2015-04-08 | 电子科技大学 | Preparation method of stratified molybdenum disulfide nano material |
Non-Patent Citations (1)
| Title |
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| 卢鹏等: "超声液相剥离制备二维MoS2作为润滑脂添加剂的摩擦学研究", 材料工程, vol. 51, no. 2, 28 February 2023 (2023-02-28), pages 160 - 168 * |
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