CN116333557B - High-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating and preparation method thereof - Google Patents
High-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 108
- 239000011248 coating agent Substances 0.000 title claims abstract description 107
- 239000004593 Epoxy Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims description 71
- 239000011246 composite particle Substances 0.000 claims abstract description 38
- 238000005461 lubrication Methods 0.000 claims abstract description 19
- -1 polysiloxane Polymers 0.000 claims abstract description 15
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 14
- 238000001723 curing Methods 0.000 claims description 42
- 229910052751 metal Inorganic materials 0.000 claims description 34
- 239000002184 metal Substances 0.000 claims description 34
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- 238000010438 heat treatment Methods 0.000 claims description 26
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- 238000000034 method Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000005498 polishing Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000853 adhesive Substances 0.000 claims description 9
- 230000001070 adhesive effect Effects 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical group CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 8
- 125000003277 amino group Chemical group 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 7
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 239000003350 kerosene Substances 0.000 claims description 4
- 238000005201 scrubbing Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 15
- 239000003822 epoxy resin Substances 0.000 abstract description 14
- 229920000647 polyepoxide Polymers 0.000 abstract description 14
- 239000000314 lubricant Substances 0.000 abstract description 9
- 239000000446 fuel Substances 0.000 abstract description 5
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052982 molybdenum disulfide Inorganic materials 0.000 abstract description 5
- 229910052582 BN Inorganic materials 0.000 abstract description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 abstract description 3
- 229910018557 Si O Inorganic materials 0.000 abstract description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 6
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229920006334 epoxy coating Polymers 0.000 description 4
- 229920000587 hyperbranched polymer Polymers 0.000 description 4
- 102000020897 Formins Human genes 0.000 description 3
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- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
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- 238000013035 low temperature curing Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 150000003141 primary amines Chemical group 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 150000003512 tertiary amines Chemical group 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical group C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-UHFFFAOYSA-K 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 229920002647 polyamide Polymers 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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- 229920001187 thermosetting polymer Polymers 0.000 description 1
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Classifications
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- 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
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
-
- 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
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention relates to a high-temperature-resistant oil-resistant epoxy wear-resistant lubricating coating, and a preparation method and application thereof. The bonding solid lubricating coating is formed by hyperbranched polysiloxane (HSiNH) 2 ) Molybdenum disulfide/hexagonal boron nitride (MoS 2 and/h-BN) composite particles and epoxy resin. Wherein HSiNH 2 The active groups contained can react with epoxy functional groups, while the introduction of Si-O bonds can improve the flexibility, oil resistance and heat resistance of the coating by MoS 2 the/h-BN composite particles are solid lubricants. The high-temperature-resistant oil-resistant epoxy bonding solid lubricating coating has excellent physical and mechanical properties, high-temperature resistance, oil resistance, friction performance and the like, can solve the problems of friction, abrasion, lubrication, dynamic sealing and the like of the moving parts of the fuel system of the aerospace engine under extreme environments such as high temperature, high speed, high pressure and the like, has the characteristics of low cost, simple preparation process and industrialized production, and has great application potential in military and civil products.
Description
Technical Field
The invention belongs to the technical field of surface coatings, and relates to a high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating and a preparation method thereof.
Background
The wear-resistant lubricating coating plays a very important role in the fuel control system of the aerospace engine. However, with the rapid development of aerospace industry in China, the fuel system faces extreme environments such as high temperature, high pressure and high speed, so that higher requirements are put on the performance of the coating, and the coating is required to have low friction, high wear resistance, high temperature resistance and oil resistance, and particularly the applicability in the extreme environments. However, the existing wear-resistant lubricating coating used in China has the problems of complex process, easy embrittlement at low temperature, easy falling at high temperature, poor wear resistance, poor oil resistance, easy foaming, short service life and the like. Therefore, development of a wear-resistant lubricating coating with simple process and excellent comprehensive performance is urgent.
Patent CN 1552782A discloses a high temperature resistant and wear resistant coating. The wear-resistant coating for medium-temperature curing and high-temperature use is prepared by taking epoxy resin as an adhesive, boron modified phenolic resin as a curing agent, molybdenum disulfide as a solid lubricant and antimony trioxide and cerium fluoride as high-temperature resistant additives. Although the problems of poor manufacturability, high curing temperature and the like existing in the application of the wear-resistant lubricating coating in a high temperature range are solved, the difficult problem of medium-temperature curing high-temperature use of the wear-resistant lubricating coating is solved, the components of the coating are complex, and the cost and the complexity of the process are obviously increased. Patent CN 113201266A discloses a high-performance epoxy bonding type solid self-lubricating coating and a preparation and application method thereof, wherein the coating is prepared from hyperbranched polysiloxane (HBPSi-PAA) capped by polyamide acid and molybdenum disulfide/graphene (MoS) 2 and/rGO) composite particles and epoxy resin. The coating has excellent antifriction and wear resistance, and also has excellent toughness, adhesive force, impact strength and other performances, but the preparation process of the coating is complex, and the curing temperature is high and can reach 250 ℃ at the highest, so that the application range of the coating is greatly limited.
The organic-inorganic hybrid resin has the characteristics of easy processability, good cohesiveness, excellent heat resistance and wear resistance of inorganic materials, and the like of the organic resinMeanwhile, the resin material meeting the actual demands can be prepared through structural design. Therefore, the organic-inorganic hybrid resin material is hopefully designed and prepared to solve the problems of poor processability, complex process, poor performance and the like of the existing wear-resistant lubricating coating. The hyperbranched polysiloxane has excellent segment flexibility, a branched topological structure containing holes, low surface energy, good oil-increasing performance and a large number of active groups, so that the hyperbranched polysiloxane not only has excellent effects of reinforcing, toughening, antifriction, antiwear and oil resistance on a thermosetting resin matrix, but also can be used as an interface modifier to improve the interface bonding strength between materials. Wherein the amino group-containing hyperbranched polysiloxane (HSiNH) prepared by a simple transesterification polycondensation method 2 ) The organic-inorganic hybrid hyperbranched polymer with Si-O-C as a main chain segment has the bond angle between Si-O-Si and C-O-C, so that the organic-inorganic hybrid hyperbranched polymer has the flexibility of a Si-O-Si structure and the rigidity of C-O-C, the organic-inorganic hybrid chain segment structure with 'hardness and softness' can better achieve the reinforcing and toughening modification effects, and active groups such as hydroxyl groups, primary amine and tertiary amine contained in the organic-inorganic hybrid hyperbranched polymer can effectively improve the compatibility of the organic-inorganic hybrid hyperbranched polymer and the solid lubricant with epoxy resin. At the same time, HSiNH 2 And the curing of the epoxy resin can be promoted, so that the aim of low-temperature curing and high-temperature use in the epoxy bonding solid lubricating coating is hopefully realized.
In addition, molybdenum disulfide is a layered solid lubricant with high compressive strength, good wear resistance and adhesiveness, and low friction coefficient (0.03-0.08), the friction coefficient of which does not change much in vacuum and air even at high temperature of 800 ℃, is particularly suitable for lubrication in the aerospace field, is an ideal solid lubricant, but has poor dispersibility, and is easy to cause particle aggregation to influence the performance. Hexagonal boron nitride (h-BN) has excellent thermal stability, can be kept stable at around 900 ℃ in an air environment, does not undergo obvious oxidation, and exhibits good lubricating performance. However, the friction coefficient of h-BN is high (about 0.3) at room temperature and its wettability with a metal surface is poor, so that it is difficult to bond with a metal substrate, thereby limiting its application in the friction field.
Therefore, the invention provides a MoS with excellent lubricity, high temperature resistance and high dispersibility by an ultrasonic assisted ball milling intercalation method 2 the/h-BN composite particles are used as solid lubricant and then pass through HSiNH 2 The modified epoxy resin is used for preparing an organic-inorganic hybrid epoxy resin material, and then the modified epoxy resin is used as a binder for preparing the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defect of applicability of the existing wear-resistant lubricating coating in extreme environments such as high temperature, high pressure, high speed and the like in the prior art, the invention provides a high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating and a preparation method thereof. The wear-resistant oil-resistant composite material has excellent high-temperature resistance and oil resistance while maintaining excellent antifriction and wear-resistant performances, and can provide an effective solution for the difficult lubrication problem of an aerospace engine fuel system in extreme environments.
Technical proposal
The high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating is characterized by comprising the following components in percentage by mass: 60 to 90 parts of epoxy E-51, 10 to 40 parts of epoxy AG-80, 1 to 35 parts of curing agent and 3 to 12 parts of hyperbranched polysiloxane HSiNH containing amino groups 2 And 30 to 50 parts of MoS 2 and/h-BN composite particles.
The composite wear-resistant lubricating coating is heated for 30 hours at 200 ℃ in an environment medium, the coating is free from foaming and cracking, the adhesive force is 1 level, the flexibility is 0.5mm, and the impact strength is 50cm; and heating the high-pressure reaction kettle for 30 hours at 180 ℃ by taking RP-3 aviation kerosene as a medium environment, wherein the coating is not foamed or discolored, and the adhesive force, the flexibility and the impact strength of the coating are still respectively maintained at 1 level, 0.5mm and 50cm.
The curing agent includes, but is not limited to, 4' -diaminodiphenyl sulfone, 4' -diaminodiphenyl methane, or 4,4' -diaminodiphenyl ether.
The hyperbranched polysiloxane HSiNH containing amino groups 2 The structural formula is as follows:
wherein:
the method for preparing the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating is characterized by comprising the following steps:
step 1: adding 60-80 parts of organic solvent into 3-12 parts of HSiNH according to mass fraction 2 And 30 to 50 parts of MoS 2 Stirring the mixture in the/h-BN composite particles for 30-60 min by ultrasonic, adding 1-35 parts of curing agent, adding 60-90 parts of epoxy E-51 and 10-40 parts of epoxy AG-80 after the curing agent is dissolved, and stirring for 5-10 min to obtain the epoxy composite coating;
step 2: uniformly spraying the prepared epoxy composite coating on the polished surface of the metal substrate for 3-5 times, curing at 80 ℃ for 5-10 min after each spraying, and then performing step heating curing, wherein the curing process comprises the following steps: and (3) curing for 2-3 h at 110-130 ℃, curing for 3-5 h at 130-150 ℃ and curing for 2-3 h at 160-180 ℃, and naturally cooling to room temperature after curing to obtain the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating.
The organic solvent is N, N-dimethylacetamide, N-dimethylformamide or N-methylpyrrolidone.
The metal substrate is polished, scrubbed and dried.
The hyperbranched polysiloxane HSiNH containing amino groups 2 Is prepared by the following steps: adding gamma-aminopropyl methyl diethoxy silane and triol (triethanolamine, glycerol) into a three-neck flask according to the mol ratio of 1:1-1:2, heating to 120-130 ℃ under nitrogen atmosphere, stirring for reaction for 2-4 h until distillate slowly flows out, then carrying out stepwise heating at the heating rate of 5-10 ℃ per hour until the distillate mass reaches 70-85% of theory, stopping the reaction, transferring the product into a vacuum drying oven, and vacuumizing (30-60) for min to obtain light yellow viscous liquid, namely HSiNH 2 。
The MoS 2 The preparation method of the/h-BN composite particles comprises the following steps: moS is carried out 2 Adding the h-BN into deionized water according to the mass ratio of 3:1-3:2, ultrasonically stirring for 1-2 h, performing suction filtration, washing with deionized water for 2-3 times, washing with absolute ethyl alcohol for 1-2 times, and performing vacuum drying for 3-6 h to obtain MoS 2 Hybrid particles loaded with h-BN. Then MoS is added according to the mass ratio of the ball materials of 1:1-3:1 2 The hybrid particles loaded with h-BN are placed in a ball milling tank and ball milled for 6 to 8 hours at the rotating speed of 300 to 600rpm/min to obtain MoS 2 and/h-BN composite particles.
Treatment of the metal substrate: firstly polishing a metal substrate by using 400-mesh sand paper, scrubbing most of abrasive dust on the surface of the metal substrate by using absolute ethyl alcohol, then placing the metal substrate in the absolute ethyl alcohol for ultrasonic treatment for 30-60 min, finally wiping the polished surface by using acetone, and drying in vacuum.
Advantageous effects
The invention provides a high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating and a preparation method thereof, wherein the bonding solid lubricating coating is prepared from hyperbranched polysiloxane (HSiNH) containing amino groups 2 ) Molybdenum disulfide/hexagonal boron nitride (MoS 2 and/h-BN) composite particles and epoxy resin. Wherein HSiNH 2 The active groups contained in the epoxy resin can react with epoxy functional groups, so that the interface bonding strength between the epoxy resin and the resin matrix is improved, good compatibility is realized, the epoxy resin can be endowed with good leveling property, and the flexibility, oil resistance and heat resistance of the coating can be improved by introducing Si-O bonds. At the same time by MoS 2 the/h-BN composite particles are solid lubricants, and are used in HSiNH 2 And MoS 2 Under the synergistic effect of the/h-BN, the coating not only can realize excellent antifriction and antiwear effects, but also can further improve the performances of heat resistance, oil resistance and the like of the coating. The high-temperature-resistant oil-resistant epoxy bonding solid lubricating coating has excellent physical and mechanical properties, high-temperature resistance, oil resistance, friction performance and the like, can solve the problems of friction, abrasion, lubrication, dynamic seal and the like of the moving parts of the fuel system of the aerospace engine under extreme environments such as high temperature, high speed, high pressure and the like, and has the advantages of low cost, simple preparation process and capability ofThe industrial production is characterized, so that the method has great application potential in military and civil products.
The epoxy composite coating is prepared from epoxy E-51, epoxy AG-80, curing agent and HSiNH 2 And MoS 2 and/h-BN composite particles. Wherein HSiNH 2 The composite material contains hydroxyl, primary amine, tertiary amine and other active groups, so that the compatibility of the composite material and the solid lubricant with epoxy resin can be effectively improved, and the introduced Si-O-C organic-inorganic hybrid chain segment structure with hardness and softness can effectively play a role in reinforcing and toughening. Meanwhile, the oil resistance and the friction performance of the epoxy composite coating can be effectively improved due to the good oil repellency and the low surface energy property of the epoxy composite coating. And, HSiNH 2 And the curing of the epoxy resin can be promoted, so that the aim of low-temperature curing and high-temperature use in the epoxy composite coating is hopefully realized. In addition, moS prepared by ultrasonic-assisted ball milling intercalation method 2 the/h-BN composite particles have the characteristics of excellent lubricity, high temperature resistance, high dispersibility and the like, and the anti-friction and wear resistance, the high temperature resistance, the service life and the like of the epoxy composite coating can be greatly improved by taking the composite particles as solid lubricants. Meanwhile, the epoxy composite coating has the characteristics of low cost, simple preparation process and the like, so that the epoxy composite coating can be applied to high-tech fields such as aviation, aerospace and the like and can also be applied to civil fields such as automobiles and the like.
Drawings
FIG. 1HSiNH 2 Is of (2)
FIG. 2MoS 2 h-BN and MoS 2 Dispersion diagram of 0h and 24h of/h-BN composite particles in epoxy paint by ultrasonic dispersion
FIG. 3 average coefficient of friction of high temperature resistant oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating
FIG. 4 is a diagram showing the physical and mechanical properties of the high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating after being treated by different medium environments and temperatures
Detailed Description
The invention will now be further described with reference to examples, figures:
the invention relates to a high-temperature resistant and oil resistant organic materialThe inorganic hybrid epoxy composite wear-resistant lubricating coating is characterized in that: heating in an environment medium at 200 ℃ for 30 hours, wherein the coating is not foamed or cracked, the adhesive force is 1 grade, the flexibility is 0.5mm, and the impact strength is 50cm; heating RP-3 aviation kerosene as a medium environment at 180 ℃ for 30 hours in a high-pressure reaction kettle, wherein the coating is not foamed or discolored, and the adhesive force, the flexibility and the impact strength of the coating are still respectively maintained at 1 level, 0.5mm and 50cm; the components are calculated according to mass fraction, 60-90 parts of epoxy E-51, 10-40 parts of epoxy AG-80, 1-35 parts of curing agent and 3-12 parts of hyperbranched polysiloxane (HSiNH) 2 ) 30-50 parts of MoS 2 and/h-BN composite particles. Wherein the curing agent is 4,4' -diaminodiphenyl sulfone, 4' -diaminodiphenyl methane or 4,4' -diaminodiphenyl ether; HSiNH 2 The structural schematic diagram is as follows:
wherein:
the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating is prepared by the following steps: firstly, polishing a metal substrate by using sand paper, cleaning the surface of the metal substrate by using absolute ethyl alcohol, and then wiping the polished surface by using acetone to ensure that the polished surface is free from pollution, oil stains and the like; then, uniformly spraying the epoxy composite coating on the polishing surface of the metal substrate; finally, the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating is obtained through gradient heating and solidification.
Specific examples:
the first step: preparation of amino-containing hyperbranched polysiloxanes (HSiNH) 2 ). Firstly, adding gamma-aminopropyl methyl diethoxy silane and triol (triethanolamine and glycerol) into a three-neck flask according to the mol ratio of 1:1-1:2, heating to (120-130) DEG C under nitrogen atmosphere, stirring and reacting for (2-4) h until distillate slowly flows out, and then carrying out stepwise heating at the heating rate of (5-10) DEG C per hour untilStopping the reaction when the distillate mass reaches 70-85% of the theoretical mass, transferring the product into a vacuum drying oven, and vacuumizing (30-60) for min to obtain light yellow viscous liquid, namely HSiNH 2 。
And a second step of: preparation of MoS 2 and/h-BN composite particles. First, moS is to 2 Adding the h-BN into deionized water according to the mass ratio of 3:1-3:2, ultrasonically stirring (1-2) for 1-2 h, suction filtering, washing with deionized water for 2-3 times, washing with absolute ethyl alcohol for 1-2 times, and vacuum drying (3-6) for h to obtain MoS 2 Hybrid particles loaded with h-BN. Then MoS is added according to the mass ratio of the ball materials of 1:1-3:1 2 The hybridized particles loaded with h-BN are placed in a ball milling tank and ball milled for 6-8 h at the rotating speed of (300-600) rpm/min to obtain MoS 2 and/h-BN composite particles.
And a third step of: preparing the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating.
(1) Firstly polishing a metal substrate by using 400-mesh sand paper, scrubbing most of abrasive dust on the surface of the metal substrate by using absolute ethyl alcohol, then placing the metal substrate in the absolute ethyl alcohol for ultrasonic treatment (30-60) for a minute, finally wiping the polished surface by using acetone, and drying in vacuum for later use;
(2) Adding 60-80 parts of organic solvent into 3-12 parts of HSiNH according to mass fraction 2 And 30 to 50 parts of MoS 2 And (3) ultrasonically stirring (30-60) the/h-BN composite particles for a period of time, then adding 1-35 parts of curing agent, adding 60-90 parts of epoxy E-51 and 10-40 parts of epoxy AG-80 after the curing agent is dissolved, and stirring (5-10) for a period of time to obtain the epoxy composite coating. Wherein the organic solvent is N, N-dimethylacetamide, N-dimethylformamide or N-methylpyrrolidone;
(3) Uniformly spraying the prepared epoxy composite coating on the polished surface of the metal substrate for 3-5 times, curing (5-10) at 80 ℃ for min after each spraying, and then performing step heating curing, wherein the curing process comprises the following steps: solidifying (2-3) h at (110-130) DEG C, (3-5) h at (130-150) DEG C, solidifying (2-3) h at (160-180) DEG C, and naturally cooling to room temperature after solidification to obtain the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating.
Example 1
(1)HSiNH 2 Is prepared from
Weighing gamma-aminopropyl methyl diethoxy silane and triethanolamine according to a molar ratio of 1:2, heating to 120 ℃ under nitrogen atmosphere, stirring for reaction for 3 hours until distillate slowly flows out, heating stepwise at a heating rate of 10 ℃ per hour until the distillate quality reaches 80% of theory, stopping reaction, transferring the product into a vacuum drying oven, and vacuumizing for 30 minutes to obtain pale yellow viscous liquid HSiNH 2 ；
(2)MoS 2 Preparation of/h-BN composite particles
First, moS is to 2 Adding h-BN into deionized water according to the mass ratio of 3:2, stirring for 1h by ultrasonic, filtering, washing with deionized water for 2 times, washing with absolute ethyl alcohol for 1 time, and vacuum drying for 6h to obtain MoS 2 Hybrid particles loaded with h-BN. Then MoS is carried out according to the mass ratio of the ball materials of 2:1 2 Placing the hybrid particles loaded with the h-BN into a ball milling tank, and ball milling for 6 hours at a rotating speed of 500rpm/min to obtain MoS 2 the/h-BN composite particles;
(3) Polishing treatment of metal substrates
Firstly polishing a metal substrate by using 400-mesh sand paper, scrubbing most of abrasive dust on the surface of the metal substrate by using absolute ethyl alcohol, then placing the metal substrate in the absolute ethyl alcohol for ultrasonic treatment for 60min, finally wiping the polished surface by using acetone, and drying in vacuum for later use;
(4) Preparation of epoxy composite coating
According to mass fraction, 35 parts of MoS is taken 2 Stirring the/h-BN composite particles in 60 parts of DMAc for 30min by ultrasonic waves, then adding 80 parts of epoxy E-51 and 20 parts of epoxy AG-80, and stirring for 5min to obtain an epoxy composite coating;
(5) Preparation of high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating
Uniformly spraying the prepared epoxy composite coating on the polished surface of the metal substrate for 3 times, curing at 80 ℃ for 5min after each spraying, and then carrying out step heating curing, wherein the curing process comprises the following steps: and (3) curing for 2 hours at 130 ℃,4 hours at 150 ℃ and 3 hours at 180 ℃, and naturally cooling to room temperature after curing to obtain the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating.
Example 2
(1)HSiNH 2 Is prepared from
Weighing gamma-aminopropyl methyl diethoxy silane and triethanolamine according to a molar ratio of 1:2, heating to 120 ℃ under nitrogen atmosphere, stirring for reaction for 3 hours until distillate slowly flows out, then carrying out stepwise heating at a heating rate of 10 ℃ per hour until the mass of the distillate reaches 60% of theory, stopping the reaction, transferring the product into a vacuum drying oven, and vacuumizing for 30 minutes to obtain pale yellow viscous liquid HSiNH 2 ；
(2)MoS 2 Preparation of the/h-BN composite particles the same as in example 1
(3) Polishing treatment of Metal substrate the same as in example 1
(4) Preparation of epoxy composite coating the same as in example 1
(5) Preparation of high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating is the same as in example 1 and example 3
(1)HSiNH 2 Preparation of (C) the same as in example 1
(2)MoS 2 Preparation of/h-BN composite particles
First, moS is to 2 Adding h-BN into deionized water according to the mass ratio of 3:1, stirring for 1h by ultrasonic, filtering, washing with deionized water for 2 times, washing with absolute ethyl alcohol for 1 time, and vacuum drying for 6h to obtain MoS 2 Hybrid particles loaded with h-BN. Then MoS is carried out according to the mass ratio of the ball materials of 2:1 2 Placing the hybrid particles loaded with the h-BN into a ball milling tank, and ball milling for 6 hours at a rotating speed of 500rpm/min to obtain MoS 2 the/h-BN composite particles;
(3) Polishing treatment of Metal substrate the same as in example 1
(4) Preparation of epoxy composite coating the same as in example 1
(5) Preparation of high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating is the same as in example 1 and example 4
(1)HSiNH 2 Preparation of (C) the same as in example 1
(2)MoS 2 Preparation of the/h-BN composite particles the same as in example 1
(3) Polishing treatment of Metal substrate the same as in example 1
(4) Preparation of epoxy composite coating
40 parts of MoS are taken according to mass fraction 2 Stirring the/h-BN composite particles in 60 parts of DMAc for 30min by ultrasonic waves, then adding 80 parts of epoxy E-51 and 20 parts of epoxy AG-80, and stirring for 5min to obtain an epoxy composite coating;
(5) Preparation of high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating is the same as in example 1 and example 5
(1)HSiNH 2 Preparation of (C) the same as in example 1
(2)MoS 2 Preparation of the/h-BN composite particles the same as in example 1
(3) Polishing treatment of Metal substrate the same as in example 1
(4) Preparation of epoxy composite coating
45 parts of MoS are taken according to mass fraction 2 Stirring the/h-BN composite particles in 60 parts of DMAc for 30min by ultrasonic waves, then adding 80 parts of epoxy E-51 and 20 parts of epoxy AG-80, and stirring for 5min to obtain an epoxy composite coating;
(5) Preparation of high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating is the same as in example 1 and example 6
(1)HSiNH 2 Preparation of (C) the same as in example 1
(2)MoS 2 Preparation of the/h-BN composite particles the same as in example 1
(3) Polishing treatment of Metal substrate the same as in example 1
(4) Preparation of epoxy composite coating
50 parts of MoS are taken according to mass fraction 2 Stirring the/h-BN composite particles in 60 parts of DMAc for 30min by ultrasonic waves, then adding 80 parts of epoxy E-51 and 20 parts of epoxy AG-80, and stirring for 5min to obtain an epoxy composite coating;
(5) Preparation of high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating is the same as in example 1 and example 7
(1)HSiNH 2 Preparation of (C) the same as in example 2
(2)MoS 2 Preparation of the/h-BN composite particles the same as in example 1
(3) Polishing treatment of Metal substrate the same as in example 1
(4) Preparation of epoxy composite coating the same as in example 5
(5) Preparation of high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating is the same as in example 1 and example 8
(1)HSiNH 2 Preparation of (C) the same as in example 1
(2)MoS 2 Preparation of the/h-BN composite particles the same as in example 3
(3) Polishing treatment of Metal substrate the same as in example 1
(4) Preparation of epoxy composite coating the same as in example 5
(5) Preparation of high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating is the same as in example 1 and example 9
(1)HSiNH 2 Preparation of (C) the same as in example 2
(2)MoS 2 Preparation of the/h-BN composite particles the same as in example 3
(3) Polishing treatment of Metal substrate the same as in example 1
(4) Preparation of epoxy composite coating the same as in example 5
(5) Preparation of high temperature resistant oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating is the same as in example 1
The performance test of the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating prepared in the embodiment is shown in the attached drawing of the specification.
FIG. 1 shows gamma-aminopropyl methyldiethoxysilane (JH-M902), triethanolamine (TEA) and HSiNH 2 And a comparative infrared spectrum of distillate and ethanol. From FIG. 1a, it can be seen that HSiNH 2 At 3360-3300 cm -1 Is at the position of-NH 2 And a stretching vibration peak of-OH, 1112cm -1 Is a stretching vibration peak of C-O bond in Si-O-C bond, 1055cm -1 Is the stretching vibration peak of Si-O bond in Si-O-C bond, 796cm -1 Is the stretching vibration peak of Si-C bond, and preliminarily shows HSiNH 2 Is successfully synthesized. To further confirm HSiNH 2 Successful synthesis, comparing the infrared spectra of distillate and ethanol (as shown in fig. 1 b), found that the spectra of both remained substantially identical, consistent with the theoretical reaction. To sum up, the analysis shows successSynthesis of HSiNH 2 。
FIG. 2 is MoS 2 h-BN and MoS 2 Dispersion pattern of the/h-BN composite particles in the epoxy coating for 0h (2 a) and 24h (2 b) by ultrasonic dispersion. Wherein the organic solvent is DMAc. It can be seen that all three particles are uniformly dispersed in the epoxy coating after ultrasonic dispersion. After standing for 24 hours, moS was clearly observed 2 Layering with the epoxy coating, while h-BN is only slightly settled, most particles still can maintain good dispersibility in the epoxy coating. At the same time, see MoS 2 the/h-BN composite particles do not settle after standing for 24 hours, and maintain excellent dispersion performance, which lays a good foundation for preparing the high-performance high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating.
FIG. 3 is a graph of the average coefficient of friction (FIG. 3 a) and wear life (FIG. 3 b) of a high temperature resistant oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating measured at 290rpm/min under dry friction conditions. It can be seen that the lowest average coefficient of friction of the coating is 0.04 and the longest lifetime is up to 736s, which shows excellent wear resistance and lubrication properties.
FIG. 4 shows the adhesion, impact strength and flexibility of the high temperature resistant and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubricating coating after heating at 200 ℃ for 30 hours in an environment medium and heating at 180 ℃ for 30 hours in a high pressure reaction kettle by taking RP-3 aviation kerosene as a medium, which can reach 1 grade, 50cm and 0.5mm respectively, and shows that the coating has excellent physical and mechanical properties and also has better high temperature resistance and oil resistance.
The high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating and the preparation method thereof provided by the invention have the advantages of excellent flexibility, impact strength and adhesive force, good high-temperature resistance and oil resistance, and the preparation method is simple in process, low in cost and capable of realizing industrial production, so that the epoxy composite lubricating coating has great application potential in the military and civil fields.
The foregoing is a further detailed description of the present invention in connection with specific examples thereof, which, although not disclosed, are not intended to limit the invention to the particular forms disclosed, but are to be construed as being within the spirit and scope of the invention.
Claims (9)
1. The high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating is characterized by comprising the following components in percentage by mass: 60 to 90 parts of epoxy E-51, 10 to 40 parts of epoxy AG-80, 1 to 35 parts of curing agent and 3 to 12 parts of hyperbranched polysiloxane HSiNH containing amino groups 2 And 30 to 50 parts of MoS 2 the/h-BN composite particles; the hyperbranched polysiloxane HSiNH containing amino groups 2 The structural formula is as follows:
wherein the method comprises the steps of
2. The high temperature and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating according to claim 1, wherein the lubrication coating is characterized in that: the composite wear-resistant lubricating coating is heated for 30 hours at 200 ℃ in an environment medium, the coating is not foamed or cracked, the adhesive force is 1 level, the flexibility is 0.5mm, and the impact strength is 50cm; and heating the high-pressure reaction kettle for 30 hours at 180 ℃ by taking RP-3 aviation kerosene as a medium environment, wherein the coating is not foamed or discolored, and the adhesive force, the flexibility and the impact strength of the coating are still respectively maintained at 1 level, 0.5mm and 50cm.
3. The high temperature and oil resistant organic-inorganic hybrid epoxy composite wear resistant lubrication coating according to claim 1, wherein the lubrication coating is characterized in that: the curing agent includes, but is not limited to, 4' -diaminodiphenyl sulfone, 4' -diaminodiphenyl methane, or 4,4' -diaminodiphenyl ether.
4. A method for preparing the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating according to any one of claims 1 to 3, which is characterized by comprising the following steps:
step 1: adding 60-80 parts of organic solvent into 3-12 parts of HSiNH according to mass fraction 2 And 30 to 50 parts of MoS 2 Stirring the mixture in the/h-BN composite particles for 30-60 min by ultrasonic, adding 1-35 parts of curing agent, adding 60-90 parts of epoxy E-51 and 10-40 parts of epoxy AG-80 after the curing agent is dissolved, and stirring for 5-10 min to obtain the epoxy composite coating;
step 2: uniformly spraying the prepared epoxy composite coating on the polished surface of the metal substrate for 3-5 times, curing at 80 ℃ for 5-10 min after each spraying, and then performing step heating curing, wherein the curing process comprises the following steps: and (3) curing for 2-3 h at 110-130 ℃, curing for 3-5 h at 130-150 ℃ and curing for 2-3 h at 160-180 ℃, and naturally cooling to room temperature after curing to obtain the high-temperature-resistant oil-resistant organic-inorganic hybrid epoxy composite wear-resistant lubricating coating.
5. The method according to claim 4, wherein: the organic solvent is N, N-dimethylacetamide, N-dimethylformamide or N-methylpyrrolidone.
6. The method according to claim 4, wherein: the metal substrate is polished, scrubbed and dried.
7. The method according to claim 4, wherein: the hyperbranched polysiloxane HSiNH containing amino groups 2 Is prepared by the following steps: adding gamma-aminopropyl methyl diethoxy silane and triol into a three-neck flask according to the molar ratio of 1:1-1:2, heating to 120-130 ℃ under nitrogen atmosphere, stirring for reaction for 2-4 h until distillate slowly flows out, then carrying out stepwise heating at the heating rate of 5-10 ℃ per hour until the distillate mass reaches 70-85% of theory, stopping the reaction, transferring the product into a vacuum drying oven, vacuumizing for 30-60 min to obtain light yellow viscous liquid, namely HSiNH 2 。
8. The method according to claim 4, wherein: the MoS 2 Preparation of/h-BN composite particlesThe preparation method comprises the following steps: moS is carried out 2 Adding the h-BN into deionized water according to the mass ratio of 3:1-3:2, ultrasonically stirring for 1-2 h, performing suction filtration, washing with deionized water for 2-3 times, washing with absolute ethyl alcohol for 1-2 times, and performing vacuum drying for 3-6 h to obtain MoS 2 h-BN loaded hybrid particles; then MoS is added according to the mass ratio of the ball materials of 1:1-3:1 2 The hybrid particles loaded with h-BN are placed in a ball milling tank and ball milled for 6 to 8 hours at the rotating speed of 300 to 600rpm/min to obtain MoS 2 and/h-BN composite particles.
9. The method according to claim 4, wherein: treatment of the metal substrate: firstly polishing a metal substrate by using 400-mesh sand paper, scrubbing most of abrasive dust on the surface of the metal substrate by using absolute ethyl alcohol, then placing the metal substrate in the absolute ethyl alcohol for ultrasonic treatment for 30-60 min, finally wiping the polished surface by using acetone, and drying in vacuum.
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