CN111171681A - Graphene fluorine modified epoxy self-layering powder coating and preparation method thereof - Google Patents
Graphene fluorine modified epoxy self-layering powder coating and preparation method thereof Download PDFInfo
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- CN111171681A CN111171681A CN202010056159.0A CN202010056159A CN111171681A CN 111171681 A CN111171681 A CN 111171681A CN 202010056159 A CN202010056159 A CN 202010056159A CN 111171681 A CN111171681 A CN 111171681A
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- 239000000843 powder Substances 0.000 title claims abstract description 258
- 238000000576 coating method Methods 0.000 title claims abstract description 178
- 239000011248 coating agent Substances 0.000 title claims abstract description 173
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000004593 Epoxy Substances 0.000 title claims abstract description 92
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 92
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000011737 fluorine Substances 0.000 title claims abstract description 45
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 98
- 239000000463 material Substances 0.000 claims abstract description 36
- 238000001816 cooling Methods 0.000 claims abstract description 33
- 238000005260 corrosion Methods 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 31
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- 238000000227 grinding Methods 0.000 claims abstract description 29
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- 239000012752 auxiliary agent Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 4
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- 239000012943 hotmelt Substances 0.000 claims description 55
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 54
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 50
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 42
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 40
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- 244000028419 Styrax benzoin Species 0.000 claims description 2
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- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012965 benzophenone Substances 0.000 claims description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
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- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 description 1
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- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 1
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- 229910021511 zinc hydroxide Inorganic materials 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
- C09D163/04—Epoxynovolacs
-
- 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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- 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
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
-
- 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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
-
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a graphene fluorine modified epoxy self-layering powder coating and a preparation method thereof. Relates to the technical field of coating, and the powder coating is prepared from the following raw materials in parts by weight: base material, filler, graphene and auxiliary agent; it has weather resistance, excellent chemical resistance and super-strong corrosion resistance. The preparation method comprises the following steps: mixing the base material, the filler except the flaky zinc powder, the graphene and the auxiliary agent according to a set proportion, uniformly stirring, performing melt extrusion, pressing into a continuous flaky object, cooling, grinding, screening, then mixing with the flaky zinc powder according to a proportion, and binding to obtain a powder coating; the powder coating is prepared according to a specific process, so that the flaky zinc powder covers the surface of the coating, and a layer-by-layer lap-joint tile structure parallel to the coating is formed and arranged in an oriented manner, and the shielding property and the corrosion resistance are further improved.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a graphene fluorine modified epoxy self-layering powder coating and a preparation method thereof.
Background
The steel structure is a structure made of steel materials, mainly comprises beam steel, steel columns, steel trusses and other members made of section steel, steel plates and the like, and is widely applied to the fields of large-scale plants, venues, super-high buildings and the like. Along with the wider application of steel structures, the corrosion resistance of the steel structures is more and more important, the traditional steel structures have various corrosion resistance modes, mainly comprise hot dip galvanizing, hot spray galvanizing, powder plastic spraying, solvent-based organic zinc-rich coating and the like, but the hot dip galvanizing and the hot spray galvanizing are both famous for high pollution and high energy consumption, and the solvent-based coating is also strongly controlled by the nation. With the increasing demand for environmentally friendly production, low VOC (volatile organic compounds) or even zero VOC is a trend in future development.
In recent years, the trend of green production, energy conservation and emission reduction is changed from oil to water and from paint to powder, a product of 4E type coating, namely powder coating, which meets the requirements of high production efficiency (efficiency), excellent coating performance (excellence), ecological environment protection (ecology) and economy (ecology) is developed, and the powder coating is widely applied to the fields of household appliances, transportation, building materials, pipelines and the like.
In the field of powder, modified bisphenol A epoxy resin and polyester resin are used as main application systems, modified bisphenol A epoxy resin powder coating has excellent mechanical properties due to a bisphenol A framework and an ether chain with good flexibility, and meanwhile, because the framework does not have an ester group, the modified bisphenol A epoxy resin powder coating has better chemical resistance and salt mist resistance, so the modified bisphenol A epoxy resin powder coating is frequently used as an anticorrosive coating. However, the amount of filler added in the powder coating is limited, so that the excellent shielding property of the powder coating is often used as a main means for protecting a steel substrate, and even if zinc powder is added, a conduction path cannot be formed like a solvent-based zinc-rich coating, so that the powder coating plays a role in cathode protection. The fluorocarbon powder coating has good weather resistance due to the existence of C-F bonds, but has poor adhesive force and impact resistance compared with other powder coatings when used alone, and does not have heavy corrosion resistance. If two-layer powder coating of a fluorocarbon system and an epoxy system is used in a matched manner and is sprayed independently, repeated construction is needed, the process is complicated, and the cost is higher, so that a self-layered heavy-duty anticorrosive powder coating is urgently needed in order to further achieve the new industrial guidance of green production, energy conservation and emission reduction.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the graphene fluorine modified epoxy self-layering powder coating which can be self-layered in application, has super-weather resistance, excellent chemical resistance and super-strong corrosion resistance and is an excellent heavy-duty anticorrosive powder coating.
The second purpose of the invention is to provide a preparation method of the graphene fluorine modified epoxy self-layering powder coating, which is characterized in that the powder coating is prepared according to a specific process, so that flaky zinc powder covers the surface of a coating, and a layer-by-layer lap-joint tile structure parallel to the coating is formed and directionally arranged, thereby further improving the shielding property and the corrosion resistance of the coating.
In order to achieve the first object, the invention provides the following technical scheme: the graphene fluorine modified epoxy self-layering powder coating is prepared from the following raw materials in parts by weight: base material, filler, graphene and auxiliary agent;
the mass ratio of the base material to the filler is (0.5-3);
the mass of the graphene is 1-5% of the total mass of the base material and the filler;
the mass of the auxiliary agent is 1-10% of the total mass of the base material and the filler;
the base material comprises novolac epoxy powder resin, fluorocarbon powder resin, modified bisphenol A epoxy resin, polyurethane resin and aliphatic enclosed polyisocyanate;
the filler includes flaky zinc powder and spherical zinc powder.
By adopting the technical scheme, the powder coating prepared by the invention has the super-weather resistance of fluorocarbon resin and the excellent chemical resistance of modified bisphenol A epoxy resin, and has super-strong corrosion resistance based on the existence of graphene, filler and auxiliary agent. Due to the existence of the graphene, the filler and the auxiliary agent, on one hand, a conduction path can be formed, the electrochemical corrosion rate of the metal substrate is slowed down, and the coating has an excellent electrochemical protection effect; on the other hand, due to the small-size effect and the two-dimensional laminated structure of the graphene, the graphene can be filled into holes and defects of the coating, a compact physical isolation layer stacked layer upon layer is formed, the electrochemical protection effect and the physical isolation layer are matched with each other, the corrosion of external harmful substances to a protected material is blocked, the shielding property of the coating is greatly improved, and the efficient corrosion protection of the metal substrate is achieved.
In the invention, modified bisphenol A epoxy resin and novolac epoxy powder resin react to generate an epoxy system as a bottom layer; the fluorocarbon resin and the aliphatic closed polyisocyanate react to generate a fluorocarbon system as a surface layer; the polyurethane resin reacts with a small amount of aliphatic closed polyisocyanate to generate a polyurethane system, and reacts with a small amount of modified bisphenol A epoxy resin and novolac epoxy powder resin to form chemical bonds, wherein the chemical bonds are partially penetrated in the whole system, but most of the chemical bonds form an intermediate transition zone of an epoxy bottom layer and a fluorocarbon surface layer.
When in application, (1) firstly, spraying the finished powder coating on the surface of a base material by an electrostatic spray gun at the voltage of 60-80KV to form a powdery coating film, thus obtaining a sample piece; (2) then putting the sample piece into a 160 ℃ oven to bake for 5min-10min, and then putting the sample piece into a 200 ℃ oven to bake for 15min-25 min; (3) and finally cooling to prepare the sample plate.
Spraying the finished powder coating on the surface of a base material through an electrostatic spray gun, and then reacting at 160 ℃ for 5-10 min, wherein at the moment, the epoxy system has low phase reaction temperature (about 160 ℃) and short gel time, while the fluorocarbon system has high phase reaction temperature (about 200 ℃) and long gel time, so that the epoxy system has a crosslinking reaction, and the fluorocarbon resin has not yet undergone a crosslinking reaction; when the temperature is raised to 200 ℃ and baked for 15min-25min, the epoxy system finishes the crosslinking reaction, and the fluorocarbon system starts to carry out the crosslinking reaction; in the whole reaction process, the epoxy system is firstly cured to complete the change from a molten state to a solid state, the surface tension of the epoxy phase is instantly increased in the process, the migration to the surface of the base material is rapidly completed, and meanwhile, the epoxy phase has stronger wettability relative to the base material than fluorocarbon, is easy to form chemical bonds with the surface of the base material and stably exists on the surface of the base material to form the bottommost layer of the whole coating film; and the fluorocarbon phase has low interfacial tension and gradually migrates to the outer surface of the coating film, thereby forming a self-layered state.
the graphene has the action mechanism that ① small-size effect and the two-dimensional lamellar structure of the graphene can increase the speed of an external corrosion road, the passing route of corrosive substances such as water, oxygen and the like is more tortuous, ② graphene has impermeability and can isolate various corrosive media, thirdly, ④ has excellent conductivity, provides a channel for electrons, forms a conduction path, can reduce the using amount of zinc powder and anti-rust pigment, achieves the efficient anti-corrosion effect, fourthly, ④ has excellent mechanical property, and the carbon atom sp in a single layer2Firm carbon-carbon bonds are formed after hybridization, the layers are mainly under the coupling action of Van der Waals force and pi electrons, the average breaking strength of the layers is about 55N/m, the layers are embedded in a coating system, and the flexibility and the impact property of the coating are greatly improved.
Furthermore, the mass ratio of the novolac epoxy powder resin, the fluorocarbon powder resin, the modified bisphenol A epoxy resin, the polyurethane resin and the aliphatic blocked polyisocyanate is (4-8): 2-6): 4-8): 1-3.
By adopting the technical scheme, the phenolic epoxy powder resin, the fluorocarbon powder resin, the modified bisphenol A epoxy resin, the polyurethane resin and the aliphatic enclosed polyisocyanate are matched according to a specific proportion, so that the heavy-duty anticorrosive self-layering powder coating with super-weather resistance can be prepared, and the basic performances of the powder coating are excellent.
In the invention, the filler comprises flaky zinc powder and spherical zinc powder; still further, the filler further comprises one or more of modified orthophosphate, polyphosphate, modified ferrophosphorus powder and modified mica powder.
By adopting the technical scheme, the filler is also called filler, namely extender pigment, and the filler is an inorganic compound with certain rigidity, strength and covering power. In the invention, the filler is also a part of the powder coating formula, and the filler mainly has the functions of improving the rigidity and the strength of the powder coating and also can save the formula cost to a certain extent. In the invention, the preferred mass ratio of the flaky zinc powder, the spherical zinc powder, the modified orthophosphate, the polyphosphate, the modified ferrophosphorus powder and the modified mica powder is (1-4): 2-8): 0-1): 0-2): (0-2).
The flaky zinc powder is prepared by ball milling spherical zinc powder, the flaky zinc powder and the spherical zinc powder are used as specific metal fillers to be applied to the coating, and the formed coating has a good protection effect on an iron matrix and is mainly embodied in the following three aspects: in the aspect of electrochemistry, the potential of zinc is more negative than that of iron, so that the zinc-iron composite material has good electrochemical protection effect on an iron matrix; second, sealing and sealing due to the corrosive reactants of zinc powder (mainly basic zinc carbonate, ZnCO)3、Zn(OH)2) Deposited among the zinc powder particles, fills gaps among the pigments and is not conductive, thereby having a sealing effect on the coating; and the flaky zinc powder is arranged in the coating layer in parallel to the surface of the coating film and is mutually overlapped and staggered, so that the distance of water and a corrosive medium penetrating through the coating layer is greatly increased, and the corrosion resistance of the coating layer is improved.
The modified ferrophosphorus powder is nontoxic, odorless and odorless, and is used as a filler in the powder coating, so that the powder coating has good electrical conductivity, thermal conductivity, special corrosion resistance, wear resistance, salt mist resistance and strong adhesive force. In the invention, the modified ferrophosphorus powder and the spherical zinc powder can play a role in superposition, not only can the corrosion be well prevented, but also a conductive path can be formed in a paint film, the cathodic protection efficiency of the paint can be improved, the conductivity of finish paint can be improved, the amount of other precious conductive pigments can be reduced, the price of the modified ferrophosphorus powder is lower than that of the zinc powder, and the cost can be reduced while the performance of the powder paint is improved.
According to the invention, the graphene is matched with the modified orthophosphate and/or polyphosphate, so that the using amount of zinc powder and anti-rust pigment can be reduced, the high-efficiency anti-corrosion effect is achieved, the anti-corrosion effect is enhanced, and the cost can be saved.
In the invention, the modified mica powder and the modified ferrophosphorus powder are used in the powder coating, so that the powder coating has good heat insulation, elasticity, toughness and high temperature resistance, and has good sliding property, strong covering property and adhesive force. Moreover, the price of the modified ferrophosphorus powder and the modified mica powder is relatively cheap, and a certain amount of the modified ferrophosphorus powder and the modified mica powder are used in the powder coating, so that the cost can be saved.
In the invention, the auxiliary agent comprises one or more of a flatting agent, a brightening agent, a conductive agent, a degassing agent, a corrosion inhibitor, a light stabilizer and an ultraviolet absorbent;
further, the leveling agent is selected from at least one of acrylate compounds, dimethyl polysiloxane and polyvinyl butyral;
further, the conductive agent is selected from at least one of conductive carbon black and conductive fibers;
further, the degassing agent is selected from at least one of benzoin and amide type micropowder wax;
further, the brightening agent is selected from at least one of butyl acrylate and methyl methacrylate;
further, the corrosion inhibitor is selected from at least one of 2-mercaptobenzothiazole and benzotriazole;
further, the light stabilizer is selected from at least one of a benzophenone-hindered amine composite light stabilizer and a triazine light stabilizer;
further, the ultraviolet absorbent is at least one selected from benzophenone ultraviolet absorbent, benzotriazole ultraviolet absorbent and benzotriazole ultraviolet absorbent.
By adopting the technical scheme, the coating additive is also called as paint auxiliary material and is an important auxiliary material for preparing the coating, so that the performance of the coating can be improved, and the formation of a coating film is promoted. The paint auxiliary agent is various, and in the invention, the paint auxiliary agent is selected from one or more of a leveling agent, a brightening agent, a conductive agent, a degassing agent, a corrosion inhibitor, a light stabilizer and an ultraviolet absorbent. The leveling agent is a common paint auxiliary agent, can promote the paint to form a flat, smooth and uniform coating film in the drying film-forming process, can effectively reduce the surface tension of the paint, improve the leveling property and uniformity of the paint, improve the permeability of the paint, reduce the possibility of generating spots and stains during brushing, increase the covering power and ensure that the film is formed uniformly and naturally.
The brightener is an auxiliary agent capable of enhancing the glossiness and the color of the powder coating. In the invention, a certain amount of brightener is added into the powder coating, so that the surface finish degree of the powder coating can be improved, the product and the environment are not polluted, the use is safe, and the decorative property of the powder coating is enhanced. Corrosion inhibitors, also known as corrosion inhibitors, are chemicals or compounds that can prevent or slow the corrosion of materials, even in small amounts, but with significant effectiveness.
The powder coating is charged by friction or corona discharge and then applied to the workpiece and adhered to the workpiece by electrostatic forces. In some applications, it is desirable that the coated surface have a low surface resistance to provide antistatic properties, even conductive properties. By adding the conductive agent, the prepared powder coating has conductive performance, the composite conductive and antistatic performance is lasting and stable, the performance is easy to adjust, the powder coating has high utilization efficiency, is easy to operate, does not contain volatile substances, and is environment-friendly.
In the construction process, the coating defects such as bubbles, shrinkage cavities, pinholes or particles appear on the surface of the coating, so that the decoration attractiveness of the surface of the coating is damaged, and the service life of a steel structure is shortened. In order to solve the problems, a degassing agent, also called a defoaming agent, is added into the coating, so that bubbles of the coating can be reduced, the coating is protected, and the decorative property of the coating is improved.
The ultraviolet absorbent is an auxiliary agent which can absorb the ultraviolet part in sunlight and a fluorescent light source and does not change. The addition of a certain amount of UV absorbers or light stabilizers to the coating improves the stability of the coating, shields or absorbs the energy of UV light, eliminates or slows down the possibility of photochemical reactions, prevents or delays the aging process, and thus extends the service life of the coating to some extent. Different light stabilizers and ultraviolet absorbers act at different stages in the anti-aging process, so in order to achieve better weather resistance, the benzophenone-hindered amine composite light stabilizer and the benzotriazole ultraviolet absorber are used in a matched manner, and the high-efficiency synergistic effect can be achieved.
In order to achieve the second object, the invention provides the following technical scheme:
a preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, mixing the base material, the filler except the flaky zinc powder, the graphene and the auxiliary agent according to a set proportion, and uniformly stirring to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 100-130 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1-2 mm, grinding into powder, and screening to obtain mixed powder;
s4, mixing the mixed powder and the flaky zinc powder in proportion, and binding for 50-70 min at a binding temperature of 60-80 ℃ and a binding current of 4-5.5A to obtain the powder coating.
By adopting the technical scheme, in the step S1, the base material, the filler except the flaky zinc powder, the graphene and the auxiliary agent are added into a high-speed mixer according to a set proportion, the mixture is stirred for 2-53 min, the raw materials are uniformly stirred, meanwhile, larger substances in the raw materials can be crushed, the agglomeration of the raw materials can be avoided, the dispersion effect is good, and the uniform mixture is obtained by stirring. In step S3, pressing the hot-melt mixture into continuous sheet-like objects, cooling to normal temperature, then crushing into small pieces with average length of 1 mm-2 mm, grinding, sieving, and selecting mixed powder with average grain size of 180 meshes or 200 meshes after sieving; and screening the size of the mixed powder so as to facilitate the binding of the subsequent steps and control the size of the final powder coating, thereby facilitating the spraying construction.
In the invention, the flaky zinc powder is added in the last step, namely step S4, by a binding process, at the moment, more than half of the flaky zinc powder covers the surface of the coating, and a layer-by-layer lap joint type tile structure parallel to the coating is formed and is directionally arranged, so that the shielding property can be further improved. In the anticorrosive process, the anti-rust pigment mainly acts on the middle and later stages and acts slowly, firstly depends on the resistance of the zinc powder to the outside, so that the flaky zinc powder which is tightly and orderly arranged on the surface layer just first rushes out, and the anticorrosive effect is further improved. The flaky zinc powder has double effects of shielding and corrosion prevention, and can strengthen the corrosion prevention performance of the coating. According to the invention, the powder coating is prepared according to a specific preparation process, so that the powder coating with excellent performance can be prepared.
In conclusion, the invention has the following beneficial effects: the powder coating has the advantages that the difference of the interfacial tension of the epoxy resin system and the fluorocarbon resin system to the base material is large, so that a self-layering state with the epoxy resin system as a bottom layer and the fluorocarbon system as a surface layer is formed, and the coating has the ultra-weather resistance of the fluorocarbon resin and the excellent chemical resistance of the modified bisphenol A epoxy resin; meanwhile, based on the existence of graphene, flaky zinc powder and spherical zinc powder, on one hand, a conduction path is formed, the electrochemical corrosion rate of a metal substrate is slowed down, and the coating has an excellent electrochemical protection effect; on the other hand, the small-size effect and the two-dimensional lamellar structure of the graphene enable the graphene to be filled into holes and defects of the coating, a compact physical isolation layer stacked layer upon layer is formed, meanwhile, the flaky zinc powder and the mica powder are overlapped layer upon layer to form a tight tile overlapping structure, external harmful substances are prevented from corroding the protected material, the shielding performance of the coating is greatly improved, and the high-efficiency anti-corrosion protection of the metal substrate is achieved. Therefore, the powder coating is a heavy-duty anticorrosive self-layering coating with super-weatherability.
Detailed Description
The present invention will be described in further detail with reference to examples.
Examples
In the examples of the present invention, some of the raw materials, the manufacturers and the types thereof are shown in Table 1
Table 1 partial materials table
Example 1
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 20kg of novolac epoxy powder resin, 10kg of fluorocarbon powder resin, 20kg of modified bisphenol A epoxy resin, 5kg of polyurethane resin, 5kg of aliphatic blocked polyisocyanate, 40kg of spherical zinc powder, 5.4kg of graphene, 4.5kg of dimethyl polysiloxane and 4.5kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 80kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 2
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 20kg of novolac epoxy powder resin, 10kg of fluorocarbon powder resin, 20kg of modified bisphenol A epoxy resin, 5kg of polyurethane resin, 5kg of aliphatic blocked polyisocyanate, 20kg of spherical zinc powder, 2.7kg of graphene, 2.25kg of dimethyl polysiloxane and 2.25kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 40kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 3
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 40kg of novolac epoxy powder resin, 30kg of fluorocarbon powder resin, 40kg of modified bisphenol A epoxy resin, 15kg of polyurethane resin, 15kg of aliphatic blocked polyisocyanate, 20kg of spherical zinc powder, 5.1kg of graphene, 5kg of dimethyl polysiloxane and 5kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 40kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 4
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 25kg of novolac epoxy powder resin, 15kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 20kg of spherical zinc powder, 3.6kg of graphene, 3kg of dimethylpolysiloxane and 3kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 40kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 5
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12kg of spherical zinc powder, 4.11kg of graphene, 3.43kg of dimethyl polysiloxane and 3.43kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 6
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 33.33kg of novolac epoxy powder resin, 16.67kg of fluorocarbon powder resin, 33.33kg of modified bisphenol A epoxy resin, 8.33kg of polyurethane resin, 8.33kg of aliphatic blocked polyisocyanate, 12kg of spherical zinc powder, 4.11kg of graphene, 3.43kg of dimethylpolysiloxane and 3.43kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 7
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 28.57kg of novolac epoxy powder resin, 21.42kg of fluorocarbon powder resin, 28.57kg of modified bisphenol A epoxy resin, 10.71kg of polyurethane resin, 10.71kg of aliphatic blocked polyisocyanate, 12kg of spherical zinc powder, 4.11kg of graphene, 3.43kg of dimethylpolysiloxane and 3.43kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 8
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 27.8kg of novolac epoxy powder resin, 27.8kg of fluorocarbon powder resin, 27.8kg of modified bisphenol A epoxy resin, 5.48kg of polyurethane resin, 11.2kg of aliphatic blocked polyisocyanate, 12kg of spherical zinc powder, 4.11kg of graphene, 3.43kg of dimethylpolysiloxane and 3.43kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 9
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 20kg of novolac epoxy powder resin, 40kg of fluorocarbon powder resin, 20kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12kg of spherical zinc powder, 4.11kg of graphene, 3.43kg of dimethyl polysiloxane and 3.43kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 10
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 20kg of spherical zinc powder, 5kg of modified orthophosphate, 10kg of polyphosphate, 10kg of modified ferrophosphorus powder and 10kg of modified mica powder, 5.85kg of graphene, 4.88kg of dimethyl polysiloxane and 4.88kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 40kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 11
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 5g of spherical zinc powder, 1kg of modified orthophosphate, 5kg of polyphosphate, 5kg of modified ferrophosphorus powder and 5kg of modified mica powder, 5.85kg of graphene, 4.88kg of dimethyl polysiloxane and 4.88kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 12
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 5kg of modified mica powder, 4.83kg of graphene, 4.03kg of dimethylpolysiloxane and 4.03kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 13
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphoric acid, 4.2kg of graphene, 3.5kg of dimethylpolysiloxane and 3.5kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 14
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 7kg of polyphosphate, 4.32kg of graphene, 3.6kg of dimethylpolysiloxane and 3.6kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 15
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 4.41kg of graphene, 3.68kg of dimethylpolysiloxane and 4.03kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 16
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 4.63kg of graphene, 3.85kg of dimethyl polysiloxane and 3.85kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 17
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 7kg of modified mica powder, 1.54kg of graphene, 3.85kg of dimethyl polysiloxane and 3.85kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 18
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 7kg of modified mica powder, 7.7kg of graphene, 3.85kg of dimethyl polysiloxane and 3.85kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 19
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 7kg of modified mica powder, 4.62kg of graphene, 0.77kg of dimethyl polysiloxane and 0.77kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 20
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 7kg of modified mica powder, 4.62kg of graphene, 7.7kg of dimethyl polysiloxane and 7.7kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 21
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 7kg of modified mica powder, 4.62kg of graphene, 2.8kg of dimethyl polysiloxane, 2.9kg of 2-mercaptobenzothiazole and 2kg of benzophenone-hindered amine composite light stabilizer into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 22
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 7kg of modified mica powder, 4.62kg of graphene, 2.8kg of dimethyl polysiloxane, 2.9kg of 2-mercaptobenzothiazole and 2kg of benzotriazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 23
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of phenolic epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of polyphosphate, 7kg of modified ferrophosphorus powder, 7kg of modified mica powder, 4.62kg of graphene, 2.8kg of dimethyl polysiloxane, 2.9kg of 2-mercaptobenzothiazole, 1kg of benzophenone-hindered amine compound stabilizer and 1kg of benzotriazole into a high-speed mixer, and stirring for 3min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 115 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1.5mm, grinding into powder, and sieving with a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 60min at a binding temperature of 70 ℃ and a binding current of 5A to obtain the powder coating.
Example 24
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of modified mica powder, 4.2kg of graphene, 3.5kg of dimethyl polysiloxane and 3.5kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 2min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 100 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1mm, grinding into powder, and sieving through a 180-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 50min at a binding temperature of 60 ℃ and a binding current of 4A to obtain the powder coating.
Example 25
A preparation process of graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
s1, adding 30kg of novolac epoxy powder resin, 20kg of fluorocarbon powder resin, 30kg of modified bisphenol A epoxy resin, 10kg of polyurethane resin, 10kg of aliphatic blocked polyisocyanate, 12g of spherical zinc powder, 3kg of modified orthophosphate, 7kg of modified mica powder, 4.2kg of graphene, 3.5kg of dimethyl polysiloxane and 3.5kg of 2-mercaptobenzothiazole into a high-speed mixer, and stirring for 5min to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 130 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 2mm, grinding into powder, and sieving with a 200-mesh sieve to obtain mixed powder;
s4, mixing the mixed powder with 25kg of flaky zinc powder, and binding for 70min at a binding temperature of 80 ℃ and a binding current of 5.5A to obtain the powder coating.
Application example
The application of the graphene fluorine modified epoxy self-layering powder coating comprises the following steps:
(1) spraying the powder coating on the surface of a base material by an electrostatic spray gun under the voltage of 70KV to form a powder coating film, thus obtaining a sample piece;
(2) putting the sample piece into a drying oven with the temperature of 160 ℃ for baking for 8min, and then putting the sample piece into a drying oven with the temperature of 200 ℃ for baking for 20 min;
(3) and cooling to obtain the sample plate.
Comparative example
Comparative example 1
Comparative example 1 differs from example 12 in that comparative example 1 does not contain the novolac epoxy powder resin and the modified bisphenol a epoxy resin (i.e., no epoxy system), and otherwise remains the same as example 12.
Comparative example 2
Comparative example 2 differs from example 12 in that comparative example 2 does not include the fluorocarbon powder resin and the aliphatic blocked polyisocyanate (i.e., no fluorocarbon system), and otherwise remains the same as example 12.
Comparative example 3
Comparative example 3 differs from example 12 in that comparative example 3 does not have the polyurethane resin added (i.e., no intermediate tie system) and otherwise remains the same as example 12.
Comparative example 4
Comparative example 4 differs from example 12 in that comparative example 4 does not contain flake zinc powder and spherical zinc powder, and the other is identical to example 12.
Comparative example 5
Comparative example 5 differs from example 12 in that: in comparative example 5, no graphene was added, and the rest was in accordance with example 12.
Comparative example 6
Comparative example 6 differs from example 12 in that: in comparative example 6, at step S1, a flaky zinc powder was charged in a high-speed mixer, and the rest was kept in accordance with example 12.
Performance test
Respectively spraying the powder coatings prepared in the examples 1-24 and the comparative examples 1-6 on the same substrate surface in an electrostatic spraying manner to obtain corresponding sample pieces; then putting the various pieces into an oven with the temperature of 160 ℃ for baking for 8min, and then putting the various pieces into an oven with the temperature of 200 ℃ for baking for 20 min; cooling and cooling to obtain the corresponding various boards.
1. The self-delamination of the coating is demonstrated by means of an artificially accelerated ageing test (UVB-313), in particular the weathering resistance of the respective panels is tested according to the fluorescent ultraviolet method of Standard GB/T14522 method for accelerated weathering test of plastics, paints, rubber materials for mechanical Industrial applications, and then judged according to the requirements of Standard HG/T2006 method for resistance to Artificial weathering in thermosetting powder paints.
The pure epoxy system has poor weather resistance, and if the system floats on the surface or the epoxy system and the fluorocarbon system are mixed and dispersed in the whole coating, the UVB-313 test time is short and is difficult to reach 3500h of the pure fluorocarbon system; when all resin base materials are mixed and reacted and the weather resistance still reaches 3000h, the fluorocarbon system basically floats on the surface, and the self-layering effect is achieved.
When the fluorescent ultraviolet method is used for detection, the detection conditions are as follows: the illumination time is 4h, and the illumination temperature is 60 ℃; the condensation time is 4h, and the condensation temperature is 50 ℃. Specific weather resistance data for each sample tested are shown in table 2.
2. The samples prepared according to the examples and comparative examples of the invention were tested and evaluated for their heavy corrosion protection according to the salt spray resistance test of standard HG/T2006 thermosetting powder. The longer the salt spray resistance time, the longer the corrosion life, which shows that the powder coatings prepared in the examples and comparative examples have better heavy corrosion resistance, and the specific test data are shown in Table 2.
3. The adhesion, impact properties, bending properties, etc. of the samples prepared in the examples and comparative examples were measured according to the standards GB/T5210, GB/T1732, GB/T6742, etc., respectively, and the results are shown in Table 2.
TABLE 2 Performance test Table
As can be seen from Table 2, the powder coating prepared by the formulation and the preparation method of the invention can be self-layered when applied, has super weather resistance, excellent chemical resistance and super corrosion resistance, and belongs to heavy-duty anticorrosive powder coatings. Specifically, in the total formula, except for the base material, the larger the proportion of the novolac epoxy powder resin and the modified bisphenol A epoxy resin in the base material is, the better the mechanical properties are; the larger the proportion of the fluorocarbon powder resin and the aliphatic closed polyisocyanate in the base material is, the better the weather resistance is.
When the ratio of the base material to the filler is (1-2): 1, the performances are better; in the range, the proportion of the filler is increased, which is beneficial to improving the salt spray performance, but is not beneficial to improving various mechanical properties.
The polyurethane resin is used as an intermediate connection link of the self-laminating system, has the functions of supporting and removing and binding, and has obvious influence on various performances. The lack of the resin can reduce the cohesion of the coating, deteriorate the mechanical property, influence the curing and crosslinking structure of the coating, and deteriorate the salt spray resistance and the aging resistance.
Flaky zinc powder and spherical zinc powder are one of the most core parts in the whole coating anticorrosion system and have important influence on various performances of the coating; the addition amount of the graphene obviously influences the salt spray performance of the coating film; the addition of the assistant corrosion inhibitor is beneficial to the improvement of the salt spray performance of the coating; the ultraviolet absorbent and the light stabilizer are compounded for use, have a synergistic effect and are beneficial to improving the ultraviolet resistance.
In the production process of the powder coating, the adding mode of the flaky zinc powder is very important, and the flaky zinc powder is bound by a binding machine generally, so that the flaky zinc powder can be better parallel to the whole coating and has obvious influence on ultraviolet resistance and salt spray resistance.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (12)
1. The utility model provides a graphite alkene fluorine modified epoxy is from layering powder coating which characterized in that: the coating is prepared from the following raw materials in parts by weight: base material, filler, graphene and auxiliary agent;
the mass ratio of the base material to the filler is (0.5-3);
the mass of the graphene is 1-5% of the total mass of the base material and the filler;
the mass of the auxiliary agent is 1-10% of the total mass of the base material and the filler;
the base material comprises novolac epoxy powder resin, fluorocarbon powder resin, modified bisphenol A epoxy resin, polyurethane resin and aliphatic enclosed polyisocyanate;
the filler includes flaky zinc powder and spherical zinc powder.
2. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 1, wherein: the mass ratio of the phenolic epoxy powder resin to the fluorocarbon powder resin to the modified bisphenol A epoxy resin to the polyurethane resin to the aliphatic blocked polyisocyanate is (4-8) to (2-6) to (4-8) to (1-3).
3. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 1, wherein: the filler further comprises one or more of modified orthophosphate, polyphosphate, modified ferrophosphorus powder and modified mica powder.
4. The graphene fluorine-modified epoxy self-layering powder coating as claimed in any one of claims 1 to 3, characterized in that: the auxiliary agent comprises one or more of a leveling agent, a brightening agent, a conductive agent, a degassing agent, a corrosion inhibitor, a light stabilizer and an ultraviolet absorbent.
5. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 4, wherein: the leveling agent is at least one selected from acrylate compounds, dimethyl polysiloxane and polyvinyl butyral.
6. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 4, wherein: the conductive agent is selected from at least one of conductive carbon black and conductive fibers.
7. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 4, wherein: the degassing agent is selected from at least one of benzoin and amide type micropowder wax.
8. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 4, wherein: the brightening agent is selected from at least one of butyl acrylate and methyl methacrylate.
9. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 4, wherein: the corrosion inhibitor is selected from at least one of 2-mercaptobenzothiazole and benzotriazole.
10. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 4, wherein: the light stabilizer is at least one selected from a benzophenone-hindered amine composite light stabilizer and a triazine light stabilizer.
11. The graphene fluorine modified epoxy self-layering powder coating as claimed in claim 4, wherein: the ultraviolet absorbent is at least one of benzophenone ultraviolet absorbent, benzotriazole ultraviolet absorbent and benzotriazole ultraviolet absorbent.
12. The preparation process of the graphene fluorine modified epoxy self-layering powder coating according to any one of claims 1 to 11, characterized by comprising the following steps: the preparation process comprises the following steps:
s1, mixing the base material, the filler except the flaky zinc powder, the graphene and the auxiliary agent according to a set proportion, and uniformly stirring to obtain a uniform mixture;
s2, melting and extruding the uniform mixture at the temperature of 100-130 ℃ to obtain a hot-melt mixture;
s3, pressing the hot-melt mixture into continuous flaky objects, cooling to normal temperature, crushing into flaky objects with the average length of 1-2 mm, grinding into powder, and screening to obtain mixed powder;
s4, mixing the mixed powder and the flaky zinc powder in proportion, and binding for 50-70 min at a binding temperature of 60-80 ℃ and a binding current of 4-5.5A to obtain the powder coating.
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