CN109957262B - Paint for material surface treatment, coating and preparation method thereof - Google Patents
Paint for material surface treatment, coating and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
- C09D7/63—Additives non-macromolecular organic
Abstract
The invention discloses a coating for material surface treatment, a coating and a preparation method thereof. The coating comprises an inorganic film-forming agent, a complexing agent, a filler, a pH regulator, a corrosion inhibitor and a dispersing agent, and the balance of the coating comprises deionized water. The coating is PH 1-4, and the coating is formed by coating the coating on the surface of a material and curing. The coating disclosed by the invention is single-component, stable in storage, convenient to prepare, environment-friendly, free of VOC (volatile organic Compounds) emission, high in hardness of a formed coating, excellent in wear resistance, and obviously superior to the prior art in anti-corrosion effect, is especially suitable for surface treatment of magnetic materials such as neodymium iron boron and fasteners, and has wide application prospect and popularization value.
Description
Technical Field
The invention relates to a coating and a coating for material surface treatment and a preparation method thereof, belonging to the technical field of material surface treatment.
Background
In the field of material surface treatment, forming an anticorrosive coating on the surface of a material by using an anticorrosive paint is one of important means for material anticorrosive surface treatment, and is a main method for improving the corrosion resistance of the material. At present, common surface treatment modes mainly comprise phosphating treatment, electroplating, electrophoretic coating, paint coating, organic coating, special coating, dacromet coating and the like, all the modes have respective advantages and have certain defects, and particularly, the phenomenon that the use requirements cannot be met in some special use occasions, such as the fields of rare earth permanent magnet material neodymium iron boron, threaded fasteners with high corrosion resistance and the like, still exists.
In the rare earth processing industry, magnetic materials are an important branch, and especially neodymium iron boron is most widely applied. The neodymium-iron-boron magnet has a special multi-phase structure, generally consists of a neodymium-rich phase, a boron-rich phase and a base phase of a thin-layer phase, different phases are mutually contacted, a plurality of micro batteries are formed due to the difference of electromotive force, and the porous characteristic of the magnet is added, so that the neodymium-iron-boron magnet is poor in corrosion resistance, is easy to rust and pulverize, and is particularly obvious in corrosion under the conditions of high temperature and high humidity. In order to improve the corrosion resistance of the neodymium iron boron and prolong the service life, the corrosion resistance is improved mainly by means of phosphorization, electroplating, electrophoresis and the like, and some research achievements represented by composite coatings have certain effect on the corrosion resistance of the neodymium iron boron.
Phosphating is a process in which chemical and electrochemical reactions form a phosphate chemical conversion coating. The phosphorization of neodymium iron boron comprises iron series phosphorization and zinc series phosphorization, generally used as surface pretreatment to provide a certain degree of protection for a magnet, and the problems of poor corrosion resistance, environmental pollution and the like exist only as a final anticorrosive technical means of neodymium iron boron. At present, the main technical means of surface treatment of neodymium iron boron is to perform composite treatment after a phosphating process, such as electroplating, electrophoresis treatment and the like. The electroplating cost is low but the pollution is serious, the environmental cost is high, and the quality stability and the corrosion resistance are also obviously insufficient; the electrophoresis treatment has the advantages of low VOC discharge, high material utilization rate, flat coating, good water resistance and chemical resistance, capability of realizing automatic fully-closed operation, wide applicability to parts with complex shapes, excellent corrosion resistance of an epoxy cathode electrophoresis layer, high one-time investment of electrophoresis complete equipment for neodymium iron boron surface treatment, higher management requirement of a swimming groove, more types of film forming defects, insufficient hardness and wear resistance of a cured film, insufficient long-time high temperature resistance, generation of a certain amount of waste liquid by swimming liquid replacement, higher cost of waste liquid treatment, and low applicability to small-batch single-piece operation.
Recently, composite coating researches aiming at neodymium iron boron surface treatment mainly focus on a scheme combining electrophoresis treatment and other pretreatment means and a scheme for improving the traditional Dacromet treatment process. Chinese patent CN105368100A, a coating liquid coating for magnetic material surface modification and a preparation method thereof, mainly adopts zinc and aluminum metal powder in a Dacromet process, combines titanium powder and ferrophosphorus powder, and silica sol as a film forming agent, and is supplemented with materials such as a complexing agent, a surfactant, a silane coupling agent, a wetting agent, a pH regulator, a diluent and the like, and then the proper curing treatment process is carried out, so that the problems of chromic acid pollution and film forming in the traditional Dacromet treatment are solved, and an excellent corrosion-resistant layer is obtained. The Chinese patent CN104894553B method for improving the performance of a surface modification layer and the application thereof, wherein an inorganic zinc-rich silica sol is coated on the surface of a material to be processed to form a priming layer, and a zinc-chromium coating solution is coated on the priming layer to form a zinc-chromium film, the zinc-chromium coating solution comprises zinc powder, aluminum powder, chromic anhydride, boric acid, a surfactant, a pH regulator, deionized water and the like, the bonding force and the wear resistance of the zinc-chromium film and a substrate are improved through the transition of the priming layer, the corrosion resistance is also improved to a great extent, the technical essence is the improvement of the traditional Dacromet process, priming treatment is needed, and the chromium-containing coating solution is used, so that the method has certain environmental hazard. Chinese patent CN105420669B is a vapor deposition method for permanent magnet anticorrosion treatment, which adopts physical vapor deposition technology to deposit a nano multilayer structure film on the surface of neodymium iron boron, then carries out electrophoresis treatment on the surface of the deposited film, adopts vapor deposition technology to pre-treat the surface of neodymium iron boron, replaces the method of phosphating, overcomes the magnetic property damage of neodymium iron boron caused by phosphating process, has good binding performance with magnet, obviously improves the corrosion resistance of neodymium iron boron, is the combination of vapor deposition technology and electrophoresis, but the vapor deposition technology is complex, has higher requirements on equipment and process, and is difficult to popularize and apply.
In the threaded fastener industry, the problem that the corrosion resistance of the fastener is insufficient is common in the industry, the fastener is corroded due to the connecting action and the fixing action of the fastener, the service life of the fastener is prolonged, the disassembly and the assembly are influenced, and the corrosion resistance treatment of the fastener is very important. At present, the main protection means mainly comprises methods such as electroplating, chemical plating, epoxy resin coating, oxidation treatment, Dacromet composite treatment, electrophoresis treatment and the like. The use of the electroplating, chemical plating and oxidation treatment methods is limited due to the generation of more waste liquid to influence the environment, the corrosion resistance is general, a certain amount of VOC (volatile organic compounds) emission is generated by epoxy resin coating, the dacromet treatment fastener loses the effect of a sacrificial anode under the condition of high temperature, effective electrochemical protection cannot be provided, the film layer is soft, and the wear resistance is also insufficient. Chinese patent CN107722765A discloses a water-based chromium-free zinc-aluminum coating and a preparation method thereof, the coating is composed of a film forming material, metal powder, a self-lubricating filler, a wetting agent, a dispersing agent, a corrosion inhibitor, a thickening agent, a defoaming agent and water, wherein a mixture of self-crosslinking acrylate emulsion and nano silica sol is used, the mixture is cured at normal temperature, the coating has a self-lubricating function, can not be worn and damaged in the assembling process, has excellent anti-corrosion performance and meets the environmental protection requirement, but the electrochemical protection effect is influenced due to the reversal of the electrode potential of zinc powder when the coating is used in a high-temperature environment. Chinese patent CN106700701A discloses a high temperature resistant environment-friendly Dacromet coating, a coating and a preparation method thereof, wherein a metal slurry, a chromium-free passivation solution and related auxiliary agents are used, the metal powder is composed of flaky zinc powder, flaky aluminum powder, flaky magnesium powder and flaky manganese powder, magnesium manganese powder is selected to replace part of zinc powder, and absolute ethyl alcohol is used to replace water, so that the problem that the traditional Dacromet coating fails due to high-temperature reversal of electrode potential of the zinc powder is effectively solved, the obtained coating has excellent high-temperature corrosion resistance and thermal shock resistance, and can play a good protection role on a fastener related to an ocean high-temperature component, thereby further prolonging the service life of the fastener, but certain hidden dangers are brought to safe production and environmental safety due to the use of the flaky magnesium powder and the absolute ethyl alcohol. Chinese patent CN103911508A discloses an anticorrosive antibacterial anodic electrophoretic coating for railway fasteners and a coating method thereof, wherein a color paste emulsion and deionized water are mixed and added into an electrophoresis tank to form the electrophoretic coating, and the electrophoretic coating is cured to form an anticorrosive antibacterial coating, so that the mechanical property and the corrosion resistance of the coating are excellent, the antibacterial property is excellent, but the hardness of the obtained coating is 2H, and the wear resistance of the coating needs to be improved.
From the above analysis, it is found that the conventional treatment methods and research results are not satisfactory to some extent in the field of material surface treatment. According to the invention, through a large number of tests and component screening, aiming at the characteristics of the neodymium iron boron porous structure material and the use position specificity of the threaded fastener, the unique component combination is combined, the obtained coating has the advantages of low comprehensive cost, single-component structure, high storage stability, no VOC (volatile organic compound) emission and no pollution in the field of surface treatment, and the obtained coating has high hardness, corrosion resistance and high temperature resistance.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a paint and a coating for material surface treatment and a preparation method thereof.
In order to achieve the purpose of the invention, the invention is realized by the following technical scheme.
The invention relates to a coating for material surface treatment, which comprises the following components in percentage by weight:
10-40% of an inorganic film-forming agent;
15-30% of a complexing agent;
8-25% of a filler;
3-10% of a pH regulator;
1-6% of a corrosion inhibitor;
2-10% of a dispersant;
the remainder contained deionized water.
The coating is adjusted in pH value through a pH regulator, so that the pH value of the coating is controlled to be 1-4.
The inorganic film forming agent is selected from one or two mixtures of acidic silica sol and acidic aluminum sol.
The complexing agent is one or a mixture of phytic acid, tannic acid, gallic acid and sulfosalicylic acid.
The filler is nano SiO2TiO 2 nanoparticles2Nano Al2O3Graphite, MoS2、WS2Two or more than two of boron nitride, mica powder, zinc phosphate, zinc dihydrogen phosphate, barium sulfate, calcium carbonate, calcium silicate, silicon whisker, silicon carbide, talcum powder and montmorillonite.
The pH regulator is a mixture of two or more of boric acid, phosphoric acid, citric acid, oxalic acid and phytic acid.
The corrosion inhibitor is one or a mixture of more than two of benzotriazole, methyl benzotriazole and mercapto benzothiazole salt.
The dispersant is one or a mixture of more than two of ethylene glycol, propylene glycol, glycerol and isopropanol.
The remainder comprises deionized water.
The rest part can also comprise aqueous resin, film-forming auxiliary agent, surfactant and defoaming agent.
The invention also provides a preparation method of the surface treatment coating, which comprises the following steps:
(1) preparing a filler dispersion liquid:
uniformly mixing an inorganic film-forming agent, deionized water, a dispersing agent and a filler to obtain a filler dispersion liquid;
(2) preparing a complexing agent solution:
uniformly mixing a complexing agent and deionized water, and stirring for 0.5-1 hour at 50-80 ℃ to obtain a complexing agent solution;
(3) preparing a coating:
and (3) uniformly mixing the materials obtained in the steps (1) and (2), adding a corrosion inhibitor and a pH regulator, regulating the pH value, and controlling the pH value to be 1-4 to obtain the coating.
The invention also provides a method for preparing a coating by using the coating, which comprises the following steps:
(1) pretreatment of materials:
degreasing, cleaning and drying the surface of a material to be treated;
(2) coating of the coating:
coating the paint on the surface of the pretreated material;
(3) curing the coating:
curing the workpiece coated with the coating to obtain a single-layer coating;
(4) preparing a double-layer coating:
repeating the step (2) and the step (3) to prepare a double-layer coating on the surface of the material;
(5) preparing a composite coating:
and (4) coating a sealing treatment agent on the surface of the coating prepared in the step (3) or the step (4), and curing to obtain the composite coating.
The curing treatment mode comprises normal-temperature natural drying curing or artificial curing.
The artificial curing conditions include: the temperature is 240-320 ℃, and the time is 5-60 minutes.
The sealing treatment agent is a mixture of a sodium methylsilicate aqueous solution and alkaline silica sol or water-soluble organic silicon resin.
The material for preparing the coating comprises a metal steel material or a rare earth permanent magnet material neodymium iron boron or a threaded fastener.
The coating system of the invention is an acid coating, a container of the coating must be made of acid-resistant materials, and the coating mode of the coating adopts an industry conventional mode and can be brush coating, spin coating, spray coating, roll coating and dip coating. The tools used in the coating process should also be made of acid resistant materials.
Compared with the prior art, the invention has the beneficial effects that:
1. the coating provided by the invention is of a water-based single-component structure, does not contain volatile organic solvents, has no peculiar smell, and is harmless to the environment;
2. the coating provided by the invention has the advantages of easily obtained raw materials, simple and convenient coating preparation, lower pretreatment requirement and low use cost;
3. the coating has the advantages that the comprehensive performance is obviously higher than that of the prior art, the pencil hardness is higher than 8H, the wear resistance and the corrosion resistance are excellent, the neutral salt spray resistance test reaches 1344H, the salt water immersion resistance reaches 1392H, no layer is formed, white rust and red rust are avoided, the temperature resistance is excellent, and the coating can be used for a long time at 340 ℃.
Detailed Description
Aiming at the defects of the prior art, the inventor provides the technical scheme of the coating and the coating for material surface treatment and the preparation method thereof through long-time repeated experimental research. The following further explanation and description of the technical solutions, it should be understood that the detailed description is only used to explain and illustrate the present invention, and not to limit the present invention.
The numerical ranges and endpoints disclosed in the present invention, should be understood that the numerical ranges resulting from various combinations between the endpoints of the respective numerical ranges are to be considered herein as specifically disclosed.
The components disclosed in the present invention should be understood as the same class of materials having the same or similar properties and effects, and not as specific limitations on the components, and equivalent substitutions or insubstantial additions or subtractions of the components should be considered as specifically disclosed herein.
The preparation method disclosed in the present invention should be understood as an effective method for achieving the object of the invention rather than the only method, and the recombination of the addition order of the components and the simple change of temperature and time should be considered as specifically disclosed herein, provided that the effect and performance of the final coating are not affected.
The specific disclosure of each component involved in the present invention is based on the disclosure of components actually used in the scope recognized by the inventors and numerous experiments, and is not intended to specifically limit the components.
The contents of the components expressed in the present invention are all weight percentages unless otherwise specified.
All raw materials in the examples of the present invention are commercially available industrial products and are commercially available, unless otherwise specified.
In one aspect, the present invention relates to a material surface treatment coating comprising:
10-40% of an inorganic film-forming agent;
15-30% of a complexing agent;
8-25% of a filler;
3-10% of a pH regulator;
1-6% of a corrosion inhibitor;
2-10% of a dispersant;
the remainder comprises deionized water.
The PH value of the coating is controlled to be 1-4.
The inorganic film forming agent is selected from one or a mixture of 10-40% of acidic silica sol and acidic aluminum sol, the acidic silica sol and the acidic aluminum sol both use water as a solvent, and the pH value, the particle size and the solid content of the inorganic film forming agent are conventional parameters of commercial industrial products. The preferable inorganic film forming agent is a mixture of acidic silica sol and acidic aluminum sol, the proportion of the acidic silica sol to the acidic aluminum sol is preferably 1: 1-3 of the solid content ratio, the formed film has better high-temperature resistance and certain toughness, the defect of a single component is overcome, the anti-cracking effect is better, and the hardness of the formed film is higher.
The complexing agent is one or a mixture of several of phytic acid, tannic acid, gallic acid and sulfosalicylic acid, the content of the preferred tannic acid is 15-30%, the complexing agent can be complexed with metals such as iron, manganese, zinc, chromium, copper and the like at normal temperature to form a stable chelate, a compact inert layer is formed on the surface of the material, the occurrence of corrosion can be effectively controlled from the inner layer of the coating, the growth of corrosion products can be inhibited, and therefore the purpose of improving the corrosion resistance is achieved.
The filler is nano TiO2Nano SiO2Nano Al2O3Graphite, MoS2、WS2The composite material comprises two or more than two of boron nitride, mica powder, zinc phosphate, zinc dihydrogen phosphate, barium sulfate, calcium carbonate, calcium silicate, silicon whisker, silicon carbide, talcum powder and montmorillonite, wherein the content of the mixture is 8-25%, the fillers are all inactive substances, metal powder is not used, the composite material is stable in a weak acid environment, the particle size of the nano material is preferably 1-150 nm, the particle size of other materials is preferably 2000-8000 meshes, the composite material is preferably a mixture of nano titanium dioxide, mica powder, graphite powder and zinc phosphate, and the preferred mass ratio is 1: 5-15: 2-10: 2-10, most preferably 1: 5-10: 2-8: 2-6, the filler is added in a combination manner, through effective combination of various particle sizes, the sedimentation of the coating during storage is favorably slowed down, the obtained coating has high density, the hardness of the coating can be effectively improved, the obtained coating is an insulating coating, the electrochemical corrosion is effectively prevented, the filler with self-lubricating property is added, the water resistance of the coating is improved, the self-lubricating property of the coating is kept, particularly, the high-temperature wear resistance is better, and the temperature change resistance is better.
The pH regulator is a mixture of two or more of boric acid, phosphoric acid, oxalic acid, citric acid and phytic acid, the content of the pH regulator is 3-10%, the addition of the phosphoric acid is favorable for providing proper acidity, the pH regulator can cooperate with a complexing agent to form a phosphating layer on the surface of a material, and a double-layer inert protective layer is formed on the surface of the material, so that the corrosion is prevented, the corrosion resistance is obviously improved, the addition of the oxalic acid is favorable for precipitating rare earth in a weak acid environment, a stable compound is formed on the surface of the material, the chemical reaction of active metal is prevented, and meanwhile, the pH regulator has a strong coordination effect with alkaline earth metal, so that the corrosion is prevented, and the corrosion resistance is improved.
The corrosion inhibitor is one or a mixture of more of benzotriazole, methyl benzotriazole and mercapto benzothiazole salt, the content of the preferred benzotriazole is 1-6%, the corrosion inhibitor can form a chain polymer and an insoluble complex with various metal ions, and the corrosion inhibitor can effectively complex copper ions and zinc ions with accelerated corrosion capability, has the function of absorbing ultraviolet rays, and thus achieves the purpose of improving corrosion resistance and weather resistance.
The dispersing agent is one or a mixture of more of ethylene glycol, propylene glycol, glycerol and isopropanol, preferably propylene glycol, the content of the propylene glycol is 2-10%, the dispersing agent has the ability of dissolving a corrosion inhibitor, can effectively disperse a slow release agent, can play a role of an antifreezing agent, improves the low-temperature fluidity of the coating, has a certain hygroscopicity, can adjust the surface drying time of the coating, and enhances the adhesive force of the coating.
The rest part contains deionized water for dissolving complexing agent, wetting filler and adjusting the viscosity of the coating.
The rest part of the aqueous resin can also comprise aqueous resin, film-forming additive and defoaming agent, and the water-soluble resin is selected from resin which does not generate polymerization reaction or precipitation under acidic condition. Film-forming aids are known in the art. The defoaming agent is a water-based organic silicon defoaming agent.
On the other hand, the invention also provides a preparation method of the surface treatment coating, which comprises the steps of uniformly mixing the inorganic film-forming agent, the deionized water, the dispersant and the filler to obtain a filler dispersion liquid; uniformly mixing a complexing agent and deionized water, and stirring for 0.5-1 hour at 50-80 ℃ to obtain a complexing agent solution; and (3) uniformly mixing the filler dispersion liquid with the complexing agent solution, then adding a corrosion inhibitor and a pH regulator, and regulating the pH value to be controlled between 1 and 4 to obtain the coating.
The preparation method can also be used for adding all the components together, uniformly mixing, heating to 50-80 ℃, uniformly stirring, and obtaining the coating without insoluble substances and obvious caking substances.
On the other hand, the invention also provides a method for preparing a coating by using the coating, which comprises the steps of degreasing and degreasing the surface of a material to be treated, cleaning and drying, coating the coating on the surface of the material, curing to obtain a single-layer coating, repeatedly coating the single-layer coating, curing to obtain a double-layer coating, and coating a sealing treatment agent on the single-layer coating or the double-layer coating to cure to obtain a composite coating.
The curing treatment comprises natural drying curing or artificial curing at normal temperature.
The artificial curing conditions include: the temperature is 240-320 ℃, and the time is 5-60 minutes.
The sealing treatment agent is a mixture of a sodium methylsilicate aqueous solution and alkaline silica sol or water-soluble organic silicon resin.
The mixture of the sodium methylsilicate aqueous solution and the alkaline silica sol can be diluted by deionized water for use.
The water-soluble organic silicon resin is water-soluble and stable at a pH value of 1-4.
The preparation of the coating selectively uses a single-layer coating, a double-layer coating or a composite coating according to the use occasion and the corrosion resistance requirement. The coating mode can be selected from brush coating, spin coating, spray coating, roll coating and dip coating according to materials and working conditions.
The material used for preparing the coating comprises a steel material or a rare earth permanent magnet material neodymium iron boron or a threaded fastener.
The pretreatment comprises degreasing, cleaning and drying, and acid pickling and rust removal are not needed.
The coating is a single-component water-based coating, all the used components are non-toxic raw materials, the acidic silica sol and the acidic aluminum sol with a nano dispersion structure are used as main film forming agents, a complexing agent, a corrosion inhibitor and an inert filler are combined, a PH regulator is used, and the obtained coating is a weakly acidic coating and can be stably stored for a long time. The obtained coating is an insulating coating, has excellent wear resistance and corrosion resistance, can be used for protecting the surface of a common steel material, is more suitable for porous structure material neodymium iron boron and a threaded fastener with a connecting and fixing function, and is further explained in detail by combining with an embodiment.
The following examples, coatings according to the invention, produce the desired test materials:
sample A
Materials: a Q235 steel plate;
specification: 150mm × 75mm × 3 mm;
the pretreatment mode comprises the following steps: degreasing, removing oil, cleaning and drying;
quantity: 44;
sample B
Materials: sintered neodymium iron boron, N35;
specification: 35mm × 18mm × 2.5 mm;
the pretreatment mode comprises the following steps: chamfering and polishing, degreasing and deoiling, washing and drying;
quantity: 33;
sample C
Materials: no. 45 carbon steel hex bolts;
specification: m20 × 60;
the pretreatment mode comprises the following steps: degreasing, removing oil, performing shot blasting, cleaning, drying, flattening an end face grinding wheel, and polishing by using abrasive paper;
quantity: 33.
example 1:
(1) preparation of the coating
Taking 10 percent (mass percent, unless otherwise specified, all show the mass percent) of 30 percent acidic silica sol (the mass percent is the following unless otherwise specified, all show the mass percent), 30 percent deionized water, 2 percent ethylene glycol and nano TiO21% of nano SiO20.5 percent of mica powder, 5.5 percent of mica powder and 1 percent of graphite powder are evenly mixed to obtain filler dispersion liquid; taking 15% of phytic acid with the concentration of 50% (the phytic acid with the content of 50% is not particularly specified below) and 31% of deionized water, heating to 50 ℃, stirring, keeping the temperature for 0.5h, and uniformly stirring to obtain a complexing agent solution; mixing the filler dispersion liquid with a complexing agent solution, adding 1% of benzotriazole and 3% of boric acid into the mixed solution, and mixing to obtain a coating with a pH value of 4;
(2) preparation of the coating
The coating obtained in step (1) was applied to the surface of sample A, B, C by dip coating, and dried for 24 hours under natural conditions, to obtain single-layer coating samples a11, a12, a13, a14, B11, B12, B13, C11, C12, and C13.
Testing of coating Properties:
the test results are shown in Table 1.
Example 2:
(1) preparation of the coating
Taking 30% of 20% acidic aluminum sol (the content of 20% acidic aluminum sol is not specifically described below), 5% of deionized water, 10% of propylene glycol and MoS22 percent of zinc phosphate, 2 percent of silicon carbide, 2 percent of crystal whisker silicon and 5 percent of talcum powder are evenly mixed to obtain filler dispersion liquid; taking 15% of sulfosalicylic acid and 11% of deionized water, heating to 50 ℃, preserving heat, stirring for 1h, and uniformly stirring to obtain a complexing agent solution; mixing the filler dispersion liquid and a complexing agent solution, adding 6% of methylbenzotriazole, 5% of 85% phosphoric acid (hereinafter, unless otherwise specified, 85% phosphoric acid) and 5% of oxalic acid into the mixed solution, and uniformly mixing to obtain a coating with a pH value of 1;
(2) preparation of the coating
And (3) coating the paint obtained in the step (1) on the surface of a sample A, B, C by a brush coating mode, drying for 60 minutes at 240 ℃, then brushing the paint obtained in the step (1) on the surface of the obtained coating, and drying for 5 minutes at 320 ℃ to obtain double-layer coating samples A21, A22, A23, A24, B21, B22, B23, C21, C22 and C23.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Example 3:
(1) preparation of the coating
Taking 5% of acidic silica sol, 15% of acidic alumina sol, 10% of deionized water, 6% of glycerol and nano Al2O38%、WS23 percent of zinc dihydrogen phosphate and 8 percent of silicon carbide are evenly mixed to obtain filler dispersion liquid; heating 15% of tannic acid and 13% of deionized water to 65 ℃, preserving heat, stirring for 30 minutes, and uniformly stirring to obtain a complexing agent solution; mixing the filler dispersion liquid with a complexing agent solution, adding 3.5% of mercapto benzothiazole salt and 7.5% of citric acid into the mixed liquid, and uniformly mixing to obtain a coating with a pH value of 3;
(2) preparation of the coating
Coating the paint obtained in the step (1) on the surface of a sample A, B, C by a spraying method, drying for 30 minutes at 280 ℃, spraying a sealant solution prepared by mixing 50% of sodium methyl silicate with the content of 30% (all the sodium methyl silicates with the content of 30% are not particularly specified below) and 50% of alkaline silica sol with water according to the ratio of 1:10 on the surface of the obtained coating, and drying for 96 hours under natural conditions to obtain samples A31, A32, A33, A34, B31, B32, B33, C31, C32 and C33 of the composite coating.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Example 4:
(1) preparation of the coating
Taking 5% of acidic silica sol, 7.5% of acidic alumina sol, 10% of deionized water, 3% of ethylene glycol, 2% of glycerol and nano TiO21 percent of mica powder, 6 percent of graphite powder and 4 percent of zinc phosphate are evenly mixed to obtain a filler dispersion liquid; heating gallic acid 15% and deionized water 20% to 80 deg.C, maintaining the temperature and stirring for 60 min, and mixing well to obtain complexing agent solution; mixing the filler dispersion liquid with a complexing agent solution, adding benzotriazole 6%, boric acid 2%, phosphoric acid 4%, oxalic acid 1%, water-soluble organic silicon resin with the solid content of 25% and the pH value of 5 6%, dodecyl ester 1% and organic silicon defoamer 0.5% into the mixed solution, and uniformly mixing to obtain a coating with the pH value of 2.5;
(2) preparation of the coating
Coating the paint obtained in the step (1) on the surface of a sample A, B, C by using a spin coating process, after naturally drying and curing for 72h, spin coating the paint (1) on the surface of the cured coating, drying and curing for 15 min at 300 ℃, then coating water-soluble organic silicon resin with the pH value of 4 and the solid content of 30% on the surface of the dried and cured coating, and drying for 30 min at 320 ℃ to cure the paint into the samples A41, A42, A43, A44, B41, B42, B43, C41, C42 and C43 of the composite coating.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Example 5:
(1) preparation of the coating
Taking 10 percent of acid silica sol, 10 percent of deionized water, 3 percent of propylene glycol and nano TiO21 percent of mica powder, 2 percent of graphite powder and 4 percent of zinc phosphate are evenly mixed to obtain the filler dispersionLiquid; heating 30% of tannic acid and 20% of deionized water to 62 ℃, preserving heat and stirring for 30 minutes to obtain a complexing agent solution; mixing the filler dispersion liquid with a complexing agent solution, adding 5% of benzotriazole, 1% of boric acid, 5% of phosphoric acid and 4% of oxalic acid into the mixed solution, and uniformly mixing to obtain a coating with a pH value of 1.2;
(2) preparation of the coating
And (3) brushing the paint obtained in the step (1) on the surface of a test sample A, B, C, drying for 5 minutes at 320 ℃, brushing the paint obtained in the step (1) on the surface of the cured coating, and drying for 60 minutes at 240 ℃ to obtain test samples A51, A52, A53, A54, B51, B52, B53, C51, C52 and C53 with double-layer coatings.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Example 6:
(1) preparation of the coating
Taking 10 percent of acidic silica sol, 15 percent of acidic alumina sol, 6 percent of propylene glycol and nano TiO21% of nano SiO20.5 percent of mica powder, 10 percent of graphite powder and 2 percent of zinc phosphate, adding 22.5 percent of tannic acid and 19 percent of deionized water after uniformly mixing, adding 3.5 percent of benzotriazole, 4 percent of boric acid, 3 percent of phosphoric acid and 0.5 percent of oxalic acid, mixing and heating to 62 ℃, preserving heat and stirring for 60 minutes to obtain a coating with the pH value of 3.2 after uniformly mixing;
(2) preparation of the coating
The paint obtained in step (1) was brushed on the surface of a sample A, B, C, and dried for 72 hours under natural conditions to obtain samples A61, A62, A63, A64, B61, B62, B63, C61, C62 and C63 of single-layer coating.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Example 7:
(1) preparation of the coating
Taking 6% of acidic silica sol, 18% of acidic alumina sol, 6% of deionized water, 3% of propylene glycol and nano TiO21% of mica powder, 8% of graphite powder and 5% of zinc dihydrogen phosphate, and uniformly mixing to obtain a filler dispersion liquid; mixing and heating 24% of tannic acid and 13% of deionized water to 65 ℃, preserving heat and stirring for 30 minutes to obtain a complexing agent solution; mixingAdding 3% of benzotriazole, 1% of boric acid, 5% of phosphoric acid and 2% of oxalic acid into the filler dispersion liquid and the complexing agent solution, and uniformly mixing to obtain a coating with a pH value of 2.5;
(2) preparation of the coating
After the paint obtained in the step (1) is brushed on the surface of a sample A, B, C, the sample is dried for 10 minutes at 300 ℃ to obtain samples A71, A72, A73, A74, B71, B72, B73, C71, C72 and C73 of the artificial cured single-layer coating.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Example 8:
(1) preparation of the coating
Taking 6% of acidic silica sol, 18% of acidic alumina sol, 6% of deionized water, 3% of propylene glycol and nano TiO21% of mica powder, 8% of graphite powder and 5% of zinc dihydrogen phosphate, and uniformly mixing to obtain a filler dispersion liquid; mixing and heating 24% of tannic acid and 13% of deionized water to 65 ℃, preserving heat and stirring for 30 minutes to obtain a complexing agent solution; after mixing the filler dispersion liquid and the complexing agent solution, adding 3% of benzotriazole, 1% of boric acid, 5% of phosphoric acid and 2% of oxalic acid, and uniformly mixing to obtain a coating with a pH value of 2.5;
(2) preparation of the coating
And (3) after the paint obtained in the step (1) is coated on the surface of a sample A, B, C by brushing, drying for 15 minutes at 290 ℃ to obtain an artificial cured single-layer coating, brushing the paint obtained in the step (1) on the single-layer coating, and drying for 30 minutes at 290 ℃ to obtain artificial cured double-layer coating samples A81, A82, A83, A84, B81, B82, B83, C81, C82 and C83.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Example 9:
(1) preparation of the coating
Taking 6% of acidic silica sol, 18% of acidic alumina sol, 6% of deionized water, 3% of propylene glycol and nano TiO21% of mica powder, 8% of graphite powder and 5% of zinc dihydrogen phosphate, and uniformly mixing to obtain a filler dispersion liquid; mixing and heating 24% of tannic acid and 13% of deionized water to 65 ℃, preserving heat and stirring for 30 minutes to obtain a complexing agent solution; mixed fillerAdding 3% of benzotriazole, 1% of boric acid, 5% of phosphoric acid and 2% of oxalic acid into the dispersion liquid and the complexing agent solution, and uniformly mixing to obtain a coating with a pH value of 2.5;
(2) preparation of the coating
And (2) after the coating obtained in the step (1) is coated on the surface of a test sample A, B, C by brush, drying for 15 minutes at 290 ℃ to obtain an artificial cured single-layer coating, coating the coating obtained in the step (1) on the single-layer coating again, drying for 30 minutes at 290 ℃ to obtain an artificial cured double-layer coating, coating the surface of the artificial cured double-layer coating with water-soluble silicone resin with the pH value of 4 and the solid content of 40%, and drying for 20 minutes at 320 ℃ to obtain artificial cured composite coating samples A91, A92, A93, A94, B91, B92, B93, C91, C92 and C93.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Comparative example 1:
(1) preparation of the coating
Taking 6% of acidic silica sol, 18% of acidic alumina sol, 10% of deionized water, 3% of propylene glycol and nano TiO21%, 8% of mica powder, 5% of graphite powder and 5% of zinc dihydrogen phosphate, and uniformly mixing to obtain a filler dispersion liquid; mixing and heating 24% of tannic acid and 17% of deionized water to 65 ℃, preserving heat and stirring for 30 minutes to obtain a complexing agent solution; after mixing the filler dispersion liquid and the complexing agent solution, adding 3% of benzotriazole, and uniformly mixing to obtain a coating with a pH value of 5;
(2) preparation of the coating
After the paint obtained in (1) was applied by brush to the surface of a test sample A, B, C, the paint was dried at 300 ℃ for 10 minutes to obtain samples a101, a102, a103, a104, B101, B102, B103, C101, C102, and C103 of the artificially cured single-layer coating.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
Comparative example 2:
(1) dacromet paint
The commercially available Dacromet coating is purchased from Changzhou Junhe science and technology Co., Ltd, model JH9390 Dacromet coating and a zinc-aluminum system;
(2) coating solution and coating preparation
The samples A111, A112, A113, A114, B111, B112, B113, C111, C112, C113 of the comparative Dacromet sample were prepared, applied, cured, 2-coat 2 baked according to the instructions.
And (3) testing the performance of the coating:
the test results are shown in Table 1.
The resulting samples were subjected to performance tests, the test standards and methods being as follows.
(1) Salt spray resistance test:
the test is carried out according to the GB/T10125-2012 test standard. A. And (3) carrying out edge sealing treatment on the sample B, observing the sample B once at intervals of 24h, and calculating the time by taking red rust points as the test end, and calculating the time by taking more than 2 red rust points at the tip of the thread as the test end.
(2) And (3) testing the salt water resistance:
A. and B, performing edge sealing treatment on the sample B, soaking the sample in a 5% NaCl aqueous solution, covering and sealing at normal temperature, observing the sample at intervals of 24h, and calculating the time by taking red rust points as the test finishing time, wherein the time by taking more than 2 red rust points at the tip of the thread as the test finishing time is used for the sample C.
(3) And (3) testing the moist heat resistance:
A. and B, performing edge sealing treatment on the sample C, setting the temperature of the wet and hot box to be 40 +/-2 ℃, setting the relative humidity to be 95% +/-3%, vertically suspending the sample in the wet and hot box, observing the sample at intervals of 24h, and calculating the time when the red rust appears as the test end, wherein the time when the sample C takes more than 2 red rust points appearing at the tip of the thread as the test end.
(4) And (3) testing pencil hardness:
the test is carried out according to GB/T6379-1966 test standards. Pencil hardness the pencil hardness of the a test piece was taken as representative data.
(5) Coating thickness test:
and (5) testing by using a thickness gauge. Sample thickness a sample thickness is taken as representative data.
(6) Adhesion test
According to the GB/T9286-1998 test standard. After the hardness and the coating thickness of the pencil are tested, the adhesive force is tested after the temperature of the sample is kept at 340 ℃ for 1h, and the data of the sample A is taken as representative data.
Table 1:
as can be seen from the comparison of the test results in Table 1, the coating obtained by using the single-component water-based paint of the invention has the advantages of excellent adhesion, good corrosion resistance, high hardness, thinner thickness and excellent comprehensive use performance. The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit of the present invention should be construed as equivalents and are included in the scope of the present invention.
Claims (6)
1. A method of preparing a coating, comprising the steps of:
pretreatment of material
Degreasing, cleaning and drying the surface of a material to be treated;
application of the coating
Coating a coating for material surface treatment on the surface of the pretreated material;
the coating comprises the following components in percentage by weight:
10-40% of an inorganic film-forming agent;
15-30% of a complexing agent;
8-25% of a filler;
3-10% of a pH regulator;
1-6% of a corrosion inhibitor;
2-10% of a dispersant;
the rest part comprises deionized water;
the pH value of the coating is 1-4;
the inorganic film forming agent is selected from one or a mixture of two of acidic silica sol and acidic aluminum sol; the complexing agent is one or a mixture of several of phytic acid, tannic acid, gallic acid and sulfosalicylic acid; the above-mentionedThe filler is nano TiO2Nano SiO2Nano Al2O3Graphite powder and MoS2、WS2Boron nitride, mica powder, zinc dihydrogen phosphate, zinc phosphate, barium sulfate, calcium carbonate, calcium silicate, talcum powder, montmorillonite, silicon carbide and whisker silicon, wherein metal powder is not used; the dispersing agent is one or a mixture of more of ethylene glycol, propylene glycol, glycerol and isopropanol;
curing of the coating
Curing the material coated with the coating to obtain a single-layer coating;
preparation of double-layer coating
Repeating the steps and the step three, and preparing a double-layer coating on the surface of the material;
preparation of the composite coating
Coating a sealing treatment agent on the surface of the coating prepared in the third step or the fourth step, and curing to obtain a composite coating; the sealing treatment agent is a mixture of a methyl sodium silicate aqueous solution and alkaline silica sol or water-soluble organic silicon resin.
2. The method of claim 1, wherein: the pH regulator is a mixture of two or more of boric acid, phosphoric acid, oxalic acid, citric acid and phytic acid.
3. The method of claim 1, wherein: the corrosion inhibitor is one or a mixture of benzotriazole, tolyltriazole and mercapto benzothiazole salt.
4. The method of claim 1, wherein: the preparation method of the coating for material surface treatment comprises the following steps:
preparation of a filler dispersion liquid
Uniformly mixing an inorganic film-forming agent, deionized water, a dispersing agent and a filler to obtain a filler dispersion liquid;
preparation of complexing agent solution
Uniformly mixing a complexing agent and deionized water, and stirring for 0.5-1 hour at 50-80 ℃ to obtain a complexing agent solution;
preparation of the coating
The coating is prepared by adding a corrosion inhibitor and a pH regulator to regulate the pH value after uniformly mixing, and controlling the pH value to be 1-4.
5. The method of claim 1, wherein: the curing treatment comprises natural drying curing or artificial curing at normal temperature; the artificial curing conditions include: the temperature is 240-320 ℃, and the time is 5-60 minutes.
6. The method of claim 1, wherein the material comprises a metallic steel material or a rare earth permanent magnet material neodymium iron boron or a threaded fastener.
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| CN110922832B (en) * | 2019-12-19 | 2021-11-26 | 和县卜集振兴标准件厂 | Anti-slip thread rust-proof treatment process for bolt surface |
| CN111117323A (en) * | 2020-01-19 | 2020-05-08 | 泰兴库本机电有限公司 | Water-based paint and coating for surface treatment of metal material and preparation method thereof |
| CN112680001B (en) * | 2020-12-28 | 2022-04-15 | 全球能源互联网研究院有限公司 | Insulating masking liquid, insulating coating, preparation method and application thereof |
| CN113744947A (en) * | 2021-08-02 | 2021-12-03 | 安徽省瀚海新材料股份有限公司 | Sintered neodymium iron boron grain boundary diffusion anti-sticking coating and application thereof |
| CN113773709A (en) * | 2021-09-03 | 2021-12-10 | 北京科技大学 | Self-warning and self-repairing dual-functional coating based on natural polyphenol filler and preparation |
| CN114426784A (en) * | 2022-01-12 | 2022-05-03 | 上海应用技术大学 | Nano inorganic coating for exterior wall and preparation method thereof |
| CN114737189A (en) * | 2022-03-18 | 2022-07-12 | 东南大学 | Method for producing a surface pretreatment layer |
| CN115798905B (en) * | 2022-09-27 | 2023-09-01 | 宁波佳丰磁材科技有限公司 | High-strength and high-toughness neodymium-iron-boron magnet and preparation method thereof |
| CN116285521B (en) * | 2022-12-19 | 2024-01-09 | 合肥博朗德纳米技术有限公司 | Rust conversion rust fixing agent for metal corrosion rust coating and preparation method thereof |
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