CN114381182A - Graphene type low-viscosity thin-coating high-hardness super-wear-resistant solvent-free epoxy coating and preparation method thereof - Google Patents
Graphene type low-viscosity thin-coating high-hardness super-wear-resistant solvent-free epoxy coating and preparation method thereof Download PDFInfo
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000000576 coating method Methods 0.000 title claims abstract description 45
- 239000011248 coating agent Substances 0.000 title claims abstract description 43
- 229920006334 epoxy coating Polymers 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003822 epoxy resin Substances 0.000 claims abstract description 35
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 239000000945 filler Substances 0.000 claims abstract description 21
- 239000003085 diluting agent Substances 0.000 claims abstract description 12
- 239000003607 modifier Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 12
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 150000001412 amines Chemical class 0.000 claims description 33
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 22
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical class C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 17
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 16
- 150000004982 aromatic amines Chemical class 0.000 claims description 16
- 229920000570 polyether Polymers 0.000 claims description 16
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- 239000002518 antifoaming agent Substances 0.000 claims description 11
- -1 glycidyl ester Chemical class 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- JOLVYUIAMRUBRK-UHFFFAOYSA-N 11',12',14',15'-Tetradehydro(Z,Z-)-3-(8-Pentadecenyl)phenol Natural products OC1=CC=CC(CCCCCCCC=CCC=CCC=C)=C1 JOLVYUIAMRUBRK-UHFFFAOYSA-N 0.000 claims description 8
- YLKVIMNNMLKUGJ-UHFFFAOYSA-N 3-Delta8-pentadecenylphenol Natural products CCCCCCC=CCCCCCCCC1=CC=CC(O)=C1 YLKVIMNNMLKUGJ-UHFFFAOYSA-N 0.000 claims description 8
- JOLVYUIAMRUBRK-UTOQUPLUSA-N Cardanol Chemical compound OC1=CC=CC(CCCCCCC\C=C/C\C=C/CC=C)=C1 JOLVYUIAMRUBRK-UTOQUPLUSA-N 0.000 claims description 8
- FAYVLNWNMNHXGA-UHFFFAOYSA-N Cardanoldiene Natural products CCCC=CCC=CCCCCCCCC1=CC=CC(O)=C1 FAYVLNWNMNHXGA-UHFFFAOYSA-N 0.000 claims description 8
- 238000006683 Mannich reaction Methods 0.000 claims description 8
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- PTFIPECGHSYQNR-UHFFFAOYSA-N cardanol Natural products CCCCCCCCCCCCCCCC1=CC=CC(O)=C1 PTFIPECGHSYQNR-UHFFFAOYSA-N 0.000 claims description 8
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 8
- 229920002866 paraformaldehyde Polymers 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 150000003512 tertiary amines Chemical class 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical group O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 125000005586 carbonic acid group Chemical group 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 239000003973 paint Substances 0.000 abstract description 5
- 238000005507 spraying Methods 0.000 abstract description 5
- 239000004593 Epoxy Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000004842 bisphenol F epoxy resin Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 2
- OZCWUNHGNVXCCO-UHFFFAOYSA-N oxiran-2-ylmethyl hydrogen carbonate Chemical group OC(=O)OCC1CO1 OZCWUNHGNVXCCO-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 241000886569 Cyprogenia stegaria Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
- C08G59/621—Phenols
- C08G59/623—Aminophenols
-
- 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
- C09D5/08—Anti-corrosive 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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2150/00—Compositions for coatings
- C08G2150/90—Compositions for anticorrosive coatings
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A graphene type low-viscosity thin-coating high-hardness super-wear-resistant solvent-free epoxy coating and a preparation method thereof relate to the technical field of graphene type solvent-free epoxy coatings. The paint comprises a component A and a component B, wherein the component A comprises the following raw materials: 35-55% of modified epoxy resin, 4-12% of reactive diluent, 2-6% of non-reactive resin modifier, 0.1-2% of anti-settling thixotropic agent, 30-50% of graphene modified superhard wear-resistant filler and 0.1-5% of auxiliary agent, wherein the component B comprises a self-made low-viscosity curing agent. The invention has the beneficial effects that: the coating system has low viscosity, can be sprayed by conventional spraying equipment, has the thinnest film forming thickness of less than 50 mu m, solves the problem of thin coating of a solvent-free epoxy system, has excellent performance, can achieve excellent corrosion resistance effect below 100 mu m, and greatly reduces the material cost.
Description
Technical Field
The invention relates to the technical field of graphene type solvent-free epoxy coating, in particular to graphene type low-viscosity thin-coating high-hardness super-wear-resistant solvent-free epoxy coating and preparation thereof.
Background
The solvent-free coating is the development direction of heavy-duty anticorrosive coatings, and with the continuous improvement of requirements of heavy-duty anticorrosive fields on the coatings, the graphene high-hardness and super-wear-resistant coating is applied to the fields of pipeline protection and repair, large-load fine particle erosion fan shell, pump body, impeller protection and repair and the like with excellent anticorrosive performance; the epoxy coating is a two-component coating, has excellent corrosion resistance, provides excellent corrosion resistance and adhesive force by taking modified low-viscosity bisphenol F type epoxy resin and modified amine as main reaction film-forming substances, and simultaneously has a relatively strong amine ester polar group in a paint film, so that hydrogen bonds can be formed among amine ester bonds, and the wear resistance of the coating is improved; the graphene modified aluminum oxide, silicon carbide, cubic boron nitride and the like are used as fillers, so that the coating is more stable in a coating system, the chemical property of the coating is stable, the hardness is high, the wear resistance is excellent, the oil absorption is small, and the viscosity of the prepared coating is low.
The conventional solvent-free epoxy coating is generally sprayed to form a film with the thickness of more than 50 microns at a single time, the spraying thickness of at least more than 100 microns can play a good anticorrosion role, and the coating needs a special spraying device, so that the coating cost is high, the equipment volume is relatively large, and the mobility is poor.
Disclosure of Invention
The invention aims to provide the graphene type low-viscosity thin-coating high-hardness super-wear-resistant solvent-free epoxy coating and the preparation thereof, aiming at the defects and defects in the prior art, the coating system is low in viscosity, can be sprayed by conventional spraying equipment, can be thinned to a film thickness of less than 50 mu m at the thinnest time, solves the problem of thin coating of the solvent-free epoxy system, is excellent in performance, can achieve an excellent corrosion resistance effect when being less than 100 mu m, and greatly reduces the material cost.
In order to achieve the purpose, the invention adopts the following technical scheme: the graphene type low-viscosity high-hardness super-wear-resistant solvent-free epoxy coating with low viscosity and capable of being thinly coated comprises a component A and a component B.
In more detail, the component A comprises the following raw materials: 35-55% of modified epoxy resin, 4-12% of reactive diluent, 2-6% of non-reactive resin modifier, 0.1-2% of anti-settling thixotropic agent, 30-50% of graphene modified superhard wear-resistant filler and 0.1-5% of auxiliary agent.
In more detail, the component B comprises a self-made low-viscosity curing agent.
More specifically, the modified epoxy resin in the component A is prepared from a self-made polyurethane prepolymer and a modified bisphenol F type epoxy resin, wherein the polyurethane prepolymer is prepared from toluene-2, 4-diisocyanate (TDI) and polyethylene glycol with the molecular weight of 1500, the bisphenol F type epoxy resin is Dow D.E.R.354, the active diluent is glycidyl ester of tertiary carbonic acid, the inactive resin modifier is NX-2025 of Kadelian, the anti-settling thixotropic agent is Haimines SD-1, the graphene modified superhard wear-resistant filler is graphene modified silicon carbide, the auxiliary agent comprises a dispersing agent, a leveling agent, an antifoaming agent and a silane coupling agent, wherein the dispersing agent is BYK-9077, the leveling agent is BYK-333, the antifoaming agent is Defom6800 and the silane coupling agent is A-187.
In more detail, the component B is prepared by performing Mannich reaction on cardanol, paraformaldehyde and mixed amine; the mixed amine consists of polyether amine, aromatic amine, aliphatic amine and tertiary amine in certain proportion, and the curing agent has both the rigidity of the aromatic amine and the flexibility of the polyether amine.
More specifically, the preparation steps of the graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating are as follows: preparing graphene modified superhard wear-resistant filler; preparing modified epoxy resin; preparing a curing agent; the self-made curing agent is prepared by performing Mannich reaction on cardanol, paraformaldehyde and mixed amine; the mixed amine consists of polyether amine, aromatic amine, aliphatic amine and tertiary amine according to a certain proportion, and the curing agent has the rigidity of the aromatic amine and the flexibility of the polyether amine; operation of the component A; the component A and the component B are mixed according to the mass ratio of 4:1 to obtain the graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating, and the coating with excellent performance is obtained after curing.
In more detail, the specific steps of preparing the graphene modified superhard wear-resistant filler are as follows: mixing graphite powder and potassium permanganate according to the proportion of 1: 1-1: 3, adding the mixture into 98% concentrated sulfuric acid, and adding an oxidant to obtain a graphite oxide concentrated sulfuric acid solution; filtering and washing are repeated for at least 3 times to obtain a graphene oxide solution; adjusting the pH value to 8-10 by using ammonia water, adding a surfactant, adding a strong reducing agent, heating to 95 ℃ for at least 4h, and reducing the graphene oxide solution into a graphene solution; adding the superhard wear-resistant filler into the graphene solution, uniformly stirring at a high speed, heating to 95 ℃ for at least 4 hours, and attaching the graphene to the surface of the powder; and (4) carrying out suction filtration, drying, crushing and sieving to obtain the graphene modified superhard wear-resistant filler for later use.
In more detail, the specific steps for preparing the modified epoxy resin are as follows: preparing a polyurethane prepolymer (-NCO content of 6-7%) by using toluene-2, 4-diisocyanate (TDI) and polyethylene glycol with a molecular weight of 1000-2000; modifying bisphenol F type epoxy resin with low viscosity and molecular weight of 160-200 by using polyurethane prepolymer, heating the polyurethane prepolymer to 50-80 ℃, adding the polyurethane prepolymer into vacuum dehydrated and dried epoxy resin with the temperature of 60-90 ℃ according to a certain proportion (5-10 percent), and stirring for 30 minutes by using a vacuum stirring device; obtaining the modified epoxy resin.
In more detail, the specific steps of the operation of the component A are as follows: adding a certain amount of modified epoxy resin, a certain amount of reactive diluent, a certain amount of non-reactive resin modifier and a certain amount of dispersant into a container, stirring for 10 minutes at a rotating speed of 1000r/min, and uniformly dispersing; adding the anti-settling thixotropic agent, the dispersing agent, the flatting agent, the defoaming agent and the silane coupling agent in sequence according to the amount, uniformly stirring, grinding to the fineness of 40 mu m, and filtering for later use.
The working principle of the invention is as follows: the modified epoxy resin is bisphenol F epoxy resin modified by a self-made polyurethane prepolymer, wherein the polyurethane prepolymer is prepared by toluene-2, 4-diisocyanate (TDI) and polyethylene glycol with the molecular weight of 1500, and the bisphenol F epoxy resin is Dow D.E.R.354; the reactive diluent adopts tertiary carbonic acid glycidyl ester; the non-reactive resin modifier is NX-2025 of Kadelian, and the anti-settling thixotropic agent is Bentone SD-1 of Haimines; the graphene modified superhard wear-resistant filler is graphene modified silicon carbide; the dispersing agent in the auxiliary agent is BYK-9077, the flatting agent is BYK-333, the defoaming agent is Defom6800, and the silane coupling agent is A-187; the component B is a self-made modified curing agent and is prepared by performing Mannich reaction on cardanol, paraformaldehyde and mixed amine; the mixed amine consists of polyether amine, aromatic amine, aliphatic amine and tertiary amine in certain proportion, and the curing agent has both the rigidity of the aromatic amine and the flexibility of the polyether amine.
After the technical scheme is adopted, the invention has the beneficial effects that: the coating system has low viscosity, can be sprayed by conventional spraying equipment, has the thinnest film forming thickness of less than 50 mu m, solves the problem of thin coating of a solvent-free epoxy system, has excellent performance, can achieve excellent corrosion resistance effect below 100 mu m, and greatly reduces the material cost.
Detailed Description
The technical scheme adopted by the specific implementation mode is as follows:
the first embodiment is as follows:
the paint comprises a component A and a component B, wherein the component A comprises the following raw materials: 35-55% of modified epoxy resin, 4-12% of reactive diluent, 2-6% of non-reactive resin modifier, 0.1-2% of anti-settling thixotropic agent, 30-50% of graphene modified superhard wear-resistant filler and 0.1-5% of auxiliary agent, wherein the component B comprises a self-made low-viscosity curing agent.
The modified epoxy resin in the component A is prepared from a self-made polyurethane prepolymer and a modified bisphenol F type epoxy resin, wherein the polyurethane prepolymer is prepared from toluene-2, 4-diisocyanate (TDI) and polyethylene glycol with the molecular weight of 1500, the bisphenol F type epoxy resin is Dow D.E.R.354, the active diluent is glycidyl tertiary carbonate, the inactive resin modifier is Kadelian NX-2025, the anti-settling thixotropic agent is Hamming BENTONE SD-1, the graphene modified superhard wear-resistant filler is graphene modified silicon carbide, the auxiliary agent comprises a dispersing agent, a leveling agent, an antifoaming agent and a silane coupling agent, wherein the dispersing agent is BYK-9077, the leveling agent is BYK-333, the antifoaming agent is Defom6800, the silane coupling agent is A-187, and the component B is cardanol, Paraformaldehyde and mixed amine are prepared by Mannich reaction; the mixed amine consists of polyether amine, aromatic amine, aliphatic amine and tertiary amine in certain proportion, and the curing agent has both the rigidity of the aromatic amine and the flexibility of the polyether amine.
The preparation steps of the graphene type low-viscosity thin-coating high-hardness super-wear-resistant solvent-free epoxy coating are as follows: preparing the graphene modified superhard wear-resistant filler: mixing graphite powder and potassium permanganate according to the proportion of 1: 1-1: 3, adding the mixture into 98% concentrated sulfuric acid, and adding an oxidant to obtain a graphite oxide concentrated sulfuric acid solution; filtering and washing are repeated for at least 3 times to obtain a graphene oxide solution; adjusting the pH value to 8-10 by using ammonia water, adding a surfactant, adding a strong reducing agent, heating to 95 ℃ for at least 4h, and reducing the graphene oxide solution into a graphene solution; adding the superhard wear-resistant filler into the graphene solution, uniformly stirring at a high speed, heating to 95 ℃ for at least 4 hours, and attaching the graphene to the surface of the powder; carrying out suction filtration, drying, crushing and sieving to obtain the graphene modified superhard wear-resistant filler for later use; preparing modified epoxy resin: preparing a polyurethane prepolymer (-NCO content of 6-7%) by using toluene-2, 4-diisocyanate (TDI) and polyethylene glycol with a molecular weight of 1000-2000; modifying bisphenol F type epoxy resin with low viscosity and molecular weight of 160-200 by using polyurethane prepolymer, heating the polyurethane prepolymer to 50-80 ℃, adding the polyurethane prepolymer into vacuum dehydrated and dried epoxy resin with the temperature of 60-90 ℃ according to a certain proportion (5-10 percent), and stirring for 30 minutes by using a vacuum stirring device; obtaining modified epoxy resin; preparing a curing agent; the self-made curing agent is prepared by performing Mannich reaction on cardanol, paraformaldehyde and mixed amine; the mixed amine consists of polyether amine, aromatic amine, aliphatic amine and tertiary amine according to a certain proportion, and the curing agent has the rigidity of the aromatic amine and the flexibility of the polyether amine; the component A is operated as follows: adding a certain amount of modified epoxy resin, a certain amount of reactive diluent, a certain amount of non-reactive resin modifier and a certain amount of dispersant into a container, stirring for 10 minutes at a rotating speed of 1000r/min, and uniformly dispersing; sequentially adding the anti-settling thixotropic agent, the dispersing agent, the flatting agent, the defoaming agent and the silane coupling agent according to the amount, uniformly stirring, grinding the mixture to the fineness of 40 mu m, and filtering the mixture for later use; the component A and the component B are mixed according to the mass ratio of 4:1 to obtain the graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating, and the coating with excellent performance is obtained after curing.
Example two:
the graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating is prepared from the following raw materials in percentage by weight: the component A comprises: 45% of modified epoxy resin, 6.5% of glycidyl versatate, 6.5% of NX-20253.5% of BENTONESD, 11% of BYK-90771% of graphene modified silicon carbide, 41% of BYK-3330.5% of Deform68000.5% of silane coupling agent A-1871%; the component B comprises: the home-made low viscosity cure was 100% and the procedure was the same as in example 1.
Example three:
the graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating is prepared from the following raw materials in percentage by weight: the component A comprises: 55% of modified epoxy resin, 8% of tert-carbonic acid glycidyl ester, 8% of NX-20254% of BENTONESD, 11% of BYK-90771%, 29% of graphene modified silicon carbide, 29% of BYK-3330.5% of Deform68000.5% of silane coupling agent A-1871%; the component B comprises: a low viscosity curing agent was prepared in a home-made 100% manner as in example 1.
The results of the paint performance tests of examples 1, 2 and 3 are shown in table 1 and the results of the coating tests are shown in table 2.
TABLE 1 paint Performance test results
TABLE 2 coating Performance test results
The working principle of the invention is as follows: the modified epoxy resin is bisphenol F epoxy resin modified by a self-made polyurethane prepolymer, wherein the polyurethane prepolymer is prepared by toluene-2, 4-diisocyanate (TDI) and polyethylene glycol with the molecular weight of 1500, and the bisphenol F epoxy resin is Dow D.E.R.354; the reactive diluent adopts tertiary carbonic acid glycidyl ester; the non-reactive resin modifier is NX-2025 of Kadelian, and the anti-settling thixotropic agent is Bentone SD-1 of Haimines; the graphene modified superhard wear-resistant filler is graphene modified silicon carbide; the dispersing agent in the auxiliary agent is BYK-9077, the flatting agent is BYK-333, the defoaming agent is Defom6800, and the silane coupling agent is A-187; the component B is a self-made modified curing agent and is prepared by performing Mannich reaction on cardanol, paraformaldehyde and mixed amine; the mixed amine consists of polyether amine, aromatic amine, aliphatic amine and tertiary amine in certain proportion, and the curing agent has both the rigidity of the aromatic amine and the flexibility of the polyether amine.
The above description is only for the purpose of illustrating the technical solutions of the present invention and not for the purpose of limiting the same, and other modifications or equivalent substitutions made by those skilled in the art to the technical solutions of the present invention should be covered within the scope of the claims of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The graphene type low-viscosity thin-coating high-hardness super-wear-resistant solvent-free epoxy coating is characterized by comprising the following components in parts by weight: it comprises a component A and a component B.
2. The graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating and the preparation method thereof according to claim 1 are characterized in that: the component A comprises the following raw materials: 35-55% of modified epoxy resin, 4-12% of reactive diluent, 2-6% of non-reactive resin modifier, 0.1-2% of anti-settling thixotropic agent, 30-50% of graphene modified superhard wear-resistant filler and 0.1-5% of auxiliary agent.
3. The graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating and the preparation method thereof according to claim 1 are characterized in that: the component B comprises a self-made low-viscosity curing agent.
4. The graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating and the preparation method thereof according to claim 1 are characterized in that: the modified epoxy resin in the component A is prepared from a self-made polyurethane prepolymer and a modified bisphenol F type epoxy resin, wherein the polyurethane prepolymer is prepared from toluene-2, 4-diisocyanate (TDI) and polyethylene glycol with the molecular weight of 1500, the bisphenol F type epoxy resin is Dow D.E.R.354, the active diluent is glycidyl ester of tertiary carbonic acid, the non-active resin modifier is NX-2025 of Kadelian, the anti-settling thixotropic agent is BENTONE SD-1 of Haimines, the graphene modified superhard wear-resistant filler is graphene modified silicon carbide, the auxiliary agent comprises a dispersing agent, a leveling agent, an antifoaming agent and a silane coupling agent, wherein the dispersing agent is BYK-9077, the leveling agent is BYK-333, the antifoaming agent is Defom6800 and the silane coupling agent is A-187.
5. The graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating and the preparation method thereof according to claim 1 are characterized in that: the component B is prepared by performing Mannich reaction on cardanol, paraformaldehyde and mixed amine; the mixed amine consists of polyether amine, aromatic amine, aliphatic amine and tertiary amine in certain proportion, and the curing agent has both the rigidity of the aromatic amine and the flexibility of the polyether amine.
6. The graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating and the preparation method thereof according to claim 1 are characterized in that: the preparation steps of the graphene type low-viscosity thin-coating high-hardness super-wear-resistant solvent-free epoxy coating are as follows:
1) preparing graphene modified superhard wear-resistant filler;
2) preparing modified epoxy resin;
3) preparing a curing agent; the self-made curing agent is prepared by performing Mannich reaction on cardanol, paraformaldehyde and mixed amine; the mixed amine consists of polyether amine, aromatic amine, aliphatic amine and tertiary amine according to a certain proportion, and the curing agent has the rigidity of the aromatic amine and the flexibility of the polyether amine;
4) operation of the component A;
5) the component A and the component B are mixed according to the mass ratio of 4:1 to obtain the graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating, and the coating with excellent performance is obtained after curing.
7. The graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating and the preparation method thereof according to claim 6 are characterized in that: the specific steps for preparing the graphene modified superhard wear-resistant filler are as follows:
a) mixing graphite powder and potassium permanganate according to the proportion of 1: 1-1: 3, adding the mixture into 98% concentrated sulfuric acid, and adding an oxidant to obtain a graphite oxide concentrated sulfuric acid solution;
b) filtering and washing are repeated for at least 3 times to obtain a graphene oxide solution;
c) adjusting the pH value to 8-10 by using ammonia water, adding a surfactant, adding a strong reducing agent, heating to 95 ℃ for at least 4h, and reducing the graphene oxide solution into a graphene solution;
d) adding the superhard wear-resistant filler into the graphene solution, uniformly stirring at a high speed, heating to 95 ℃ for at least 4 hours, and attaching the graphene to the surface of the powder;
e) and (4) carrying out suction filtration, drying, crushing and sieving to obtain the graphene modified superhard wear-resistant filler for later use.
8. The graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating and the preparation method thereof according to claim 6 are characterized in that: the preparation method of the modified epoxy resin comprises the following specific steps:
a) preparing a polyurethane prepolymer (-NCO content of 6-7%) by using toluene-2, 4-diisocyanate (TDI) and polyethylene glycol with a molecular weight of 1000-2000;
b) modifying bisphenol F type epoxy resin with low viscosity and molecular weight of 160-200 by using polyurethane prepolymer, heating the polyurethane prepolymer to 50-80 ℃, adding the polyurethane prepolymer into vacuum dehydrated and dried epoxy resin with the temperature of 60-90 ℃ according to a certain proportion (5-10 percent), and stirring for 30 minutes by using a vacuum stirring device;
c) obtaining the modified epoxy resin.
9. The graphene type low-viscosity thin-coating high-hardness ultra-wear-resistant solvent-free epoxy coating and the preparation method thereof according to claim 6 are characterized in that: the specific steps of the component A operation are as follows:
a) adding a certain amount of modified epoxy resin, a certain amount of reactive diluent, a certain amount of non-reactive resin modifier and a certain amount of dispersant into a container, stirring for 10 minutes at a rotating speed of 1000r/min, and uniformly dispersing;
b) adding the anti-settling thixotropic agent, the dispersing agent, the flatting agent, the defoaming agent and the silane coupling agent in sequence according to the amount, uniformly stirring, grinding to the fineness of 40 mu m, and filtering for later use.
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