CN111253790B - Preparation method of thin composite nano flake coating - Google Patents

Preparation method of thin composite nano flake coating Download PDF

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CN111253790B
CN111253790B CN202010074135.8A CN202010074135A CN111253790B CN 111253790 B CN111253790 B CN 111253790B CN 202010074135 A CN202010074135 A CN 202010074135A CN 111253790 B CN111253790 B CN 111253790B
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coating
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CN111253790A (en
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白日忠
陈景清
张蕴
杨献楠
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Jiangsu Chaotu New Material Technology Co ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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    • 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
    • C09D7/65—Additives macromolecular
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    • 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
    • C08K2003/0881—Titanium
    • 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
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • 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
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of 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; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of 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; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of 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; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/18—Homopolymers or copolymers or tetrafluoroethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
    • C08L81/02—Polythioethers; Polythioether-ethers

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Abstract

The invention relates to a preparation method of a thin composite nano flake coating. The preparation method comprises selecting resin base material, composite nanometer scale material and other auxiliary agents, mixing the above materials together, and mixing and dispersing with mixing and dispersing equipment to obtain composite nanometer scale coating. The surface of the composite nano scale has high-activity dangling bonds, and the high-activity dangling bonds are coordinated with organic matters to form chemical bonding and chemical adsorption, so that the binding force between the filler and resin in the coating is greatly improved, and the binding force between the coating resin molecules is also greatly improved.

Description

Preparation method of thin composite nano flake coating
Technical Field
The invention relates to a coating using a novel composite nano flake material as a filler, belongs to the field of coatings, and particularly relates to a preparation method of a thin composite nano flake coating.
Technical Field
The coating is widely applied to the protection in the fields of petrochemical industry, metallurgical industry, food industry, coal mining, marine industry, mechanical industry, electric power industry and the like, for example, in the marine industry, the coating is used on ships, can enhance the sea water resistance and prolong the service life of the ship body; in the steel industry, the protection of various pipelines, flues and desulfurization washing towers can reduce the economic loss caused by steel corrosion to the maximum extent; in the food industry, the requirements of equipment corrosion prevention and pollution prevention can be met simultaneously; in the petroleum industry, the coating can be used as a special anticorrosive and antiscale coating; in the household appliance industry, the coating can be used for solving the problems of corrosion resistance, adhesion resistance and the like.
With the increasing enhancement of environmental protection, the Chinese paint industry is developing towards low pollution and high performance as the world, and three types of high solid paint, water paint and solvent-free paint (powder paint and light curing paint) become the mainstream of the paint industry. Meanwhile, the paint with special performances such as high temperature resistance, heat conduction, insulation, static conduction, low surface energy, high decoration and the like, high performance and high quality is gradually accepted by people, which fully indicates that the paint industry is developing towards specialization and refinement. The thin coating can save a large amount of coating raw materials, can reduce coating defective materials and reduce coating cost, has great influence on the economy of the coating, and is the development direction of the coating in the future.
The scale-type coating such as dacromet coating, glass scale coating and the like plays a labyrinth role and eliminates the stress in the coating by utilizing the layered superposition effect of the scale, so that the coating has excellent permeation resistance and good adhesive force, and the corrosion resistance of the scale-type coating is good. However, the flake is thick and is difficult to be made into thin coating.
The existing nano coating has no scale lamination effect and poor anti-permeability; and the second is that the coating contains micron-sized other non-nano fillers, so the coating cannot be too thin.
In the prior invention patent ZL200510119141.6 preparation method of nano flake coating, the nano flake is directly dispersed in the base coating, and the following defects exist: firstly, because the original basic coating contains micron-sized powder, the coating is not thicker than the particle size of the micron powder due to the influence of the particle size of the micron powder (20-60 microns); although the nano scale is treated, the nano scale is not added with nano material dispersing agent, anti-settling agent and other auxiliary agents which are adaptive to the nano scale when the coating is prepared, so that the coating is well protected, and the coating with higher activity of the nano scale can generate agglomeration and settling phenomena when being stored, so that the protective performance of the coating is reduced, and the application of the coating with the nano scale is influenced; when the nano scale coating is prepared, nano material auxiliaries such as a flatting agent and a defoaming agent which are adaptive to the nano scales are not added, bubbles and shrinkage cavities are easy to appear during use, and when the coating is used, multiple coating is needed, so that the influence of the bubbles and the shrinkage cavities can be eliminated, and the coating cannot be made into a thin coating; fourthly, the nano scale is made of a single material and has single function. CN107384183A an ultrathin coating and a preparation method thereof, the ultrathin coating comprises the following main components in parts by weight: 20 to 29 percent of polyurethane acrylic resin, 25 to 28 percent of ammonium polyphosphate, 1.5 to 3.5 percent of initiator, 20 to 24 percent of titanium pigment, 0.8 to 1 percent of acrylic polymer, 0.5 to 1 percent of fluorine modified surfactant, 20.5 to 22.5 percent of chlorinated paraffin, 15 to 20 percent of solvent and 3 to 7 percent of hollow glass microsphere. It is mainly suitable for reducing the surface temperature loss of thermal equipment and reducing the energy consumption of the equipment in a humid environment. The thickness of the coating is influenced by the particle size (the wall thickness is 1-2 microns, the particle size is 10-250 microns) of the titanium dioxide and the hollow glass beads, so that the coating cannot be too thin.
Disclosure of Invention
The invention aims to provide a preparation method of a thin composite nano scale coating, which overcomes the defects of the coating and can prepare an ultra-thin nano scale coating, wherein the composite nano scale forms a laminating effect and forms chemical adsorption or chemical bonding with resin, so that the coating can form a three-dimensional net-shaped integral structure and has the nano characteristics of multiple materials used for compounding, the nano scale has more functions, excellent adhesive force, good permeability resistance and high corrosion resistance, and the coating has more functions.
The technical scheme of the invention is as follows:
a preparation method of a thin composite nano flake coating comprises the following steps:
(1) selecting a resin base material; selecting a composite nano flake material which is not only an active filler of the coating, but also a modifier and a coupling agent of the coating; selecting an auxiliary agent, wherein the auxiliary agent is two or more or all of an anti-settling agent, a thickening agent, a defoaming agent, a leveling agent, a dispersing agent, a wetting agent, a surface modifier, a coupling agent and a solvent;
(2) the thin composite nano flake coating material comprises the following materials in percentage by weight:
a. the weight percentage of the resin base material and the composite nano scale material is as follows:
i, 10-90% of resin base material
II, 90-10% of composite nano flake material
b. The anti-settling agent accounts for 0.1-50% of the composite nano scale material by weight;
the thickener accounts for 0.1-40% of the composite nano scale material by weight percent;
the defoaming agent accounts for 0.1 to 30 percent of the composite nano scale material in percentage by weight
The weight percentage of the flatting agent in the composite nano scale material is 0.1-30%;
the dispersant accounts for 0.1-50% of the composite nano scale material by weight;
the wetting agent accounts for 0.1-40% of the composite nano scale material by weight percent;
the surface modifier accounts for 0.1-80% of the composite nano flake material by weight percent;
the coupling agent accounts for 0.1-50% of the composite nano scale material by weight;
the solvent accounts for 1-200% of the resin base material by weight;
(3) preparation:
mixing and dispersing the resin base material, the composite nano scale material and the selected auxiliary agent by using mixing and dispersing equipment according to the proportion.
The resin base material comprises one or more of epoxy resin base material, epoxy phenolic resin base material, polyphenylene sulfide resin base material, polyurethane resin base material, polyfluorinated resin base material, fluorocarbon resin base material, acrylic base material, chlorinated rubber base material, perchloroethylene base material and alkyd base material.
The composite nano scale material is prepared by the following method,
a. firstly, weighing base materials to be prepared into scales, wherein the base materials prepared from the scales are solid powder materials, the particle size of the powder is 1-100 mu m, the base materials are two or more, one of the base materials is a main base material, the other base materials are auxiliary base materials, and the weight ratio of the base materials to the auxiliary base materials is 1: 0.1 to 1;
b. selecting grinding balls, wherein the hardness of the grinding balls is greater than that of the base material, the diameters of the grinding balls are not less than three size specifications, and the stacking volume of the grinding balls accounts for 30-70% of the volume of the grinding cylinder;
c. selecting an auxiliary agent, selecting two or more or all kinds of a coupling agent, an anti-settling agent, a dispersing agent, a protective agent and a solvent according to the weight of the base powder material of the prepared scale, wherein the weight ratio of the coupling agent to the base material for preparing the scale is 1: 50-100 parts; the anti-settling agent accounts for 0.1-20% of the weight of the base material; the dispersant accounts for 0.1-20% of the weight of the base material; the protective agent accounts for 0.5-30% of the weight of the base material; the solvent accounts for 10-800% of the weight of the base material;
d. b, putting the base material prepared from the scales in the steps a, b and c, the selected auxiliary agent and the grinding balls into an intermittent grinding machine according to the formula proportion, and dispersing, mixing and primarily grinding to uniformly disperse and mix the base powder material prepared from the scales, the coupling agent, the anti-settling agent, the dispersing agent, the protective agent and the solvent;
e. preparing composite nano scales: and c, according to the ball formula in the step b, placing grinding balls in a grinding cylinder of a continuous planetary ball mill, adjusting grinding parameters of the continuous planetary ball mill, wherein the revolution speed is 100-1000 r/min, the rotation speed is 100-4000 r/min, and then conveying the uniform material prepared in the step d into the continuous planetary ball mill by using a metering pump to prepare a uniform composite nano scale material, wherein the thickness of the uniform composite nano scale material reaches 1-40 nm, and the size of the scale in the plane direction is 0.2-50 mu m.
The anti-settling agent is ultrafine powder or nano powder anti-settling agent or organic phosphate ester anti-settling agent, and is one or more of nano fumed silica, organic bentonite, N-methyl pyrrolidone solution of modified polyurea and organic phosphate ester F118; wherein the thickening agent comprises cellulose ethers, acrylic acid alkali swelling type, nonionic polyurethanes and hydrophobic modified alkali swelling type; the defoaming agent comprises: the coating defoaming agent comprises a water-based coating defoaming agent and a solvent-based coating defoaming agent, wherein the defoaming agent mainly comprises organic siloxane, polyether, silicon and ether graft, amine, imine and amide and is assisted by other defoaming agents; the leveling agent comprises: the water-based paint leveling agent and the solvent-based paint leveling agent comprise high-boiling organic solvents or mixtures thereof, wherein the high-boiling organic solvents are isophorone, diacetone alcohol and Solvesso 150; the dispersant comprises: one or more of anionic dispersant, cationic dispersant, nonionic dispersant, amphoteric wetting dispersant, electric neutral wetting dispersant, macromolecular hyperdispersant and free radical hyperdispersant; the wetting agents include: the low molecular weight surfactant and the high molecular compound with surface activity are one or more of polyoxyethylene alkyl phenyl ether and polyoxyethylene fatty acid ester; the surface modifier comprises: graphene, nano iron powder and polytetrafluoroethylene nano flakes; the coupling agent is one or more of silane coupling agent or titanate coupling agent; the solvent is one or more of alcohols, ketones, benzenes, esters, reactive diluents and deionized water.
The weight percentage of the composite nano scale material is selected according to the protection requirement or the protection grade requirement, and the principle is that when the protection requirement is high, the weight percentage of the composite nano scale material is increased;
the mixing and dispersing equipment for preparing the thin composite nano flake coating comprises: a sand mill, a high-speed dispersion machine, a homogenizer, a colloid mill, a continuous planetary ball mill; the mixing and dispersing time is 5-120 min.
The invention has the advantages of
1. Chemical bonding and chemical adsorption: the surface of the composite nano scale has high-activity dangling bonds, and the high-activity dangling bonds are coordinated with organic matters to form chemical bonding and chemical adsorption, so that the binding force between the filler and resin in the coating is greatly improved, and the binding force between the coating resin molecules is also greatly improved.
2. Strong permeation resistance: firstly, chemical bonding and chemical adsorption are formed between the composite nano scale and resin molecules in the coating, a three-dimensional net-shaped integral structure is formed, and a permeation channel is blocked; secondly, the nonporous and integrally continuous characteristics of the composite nano scale can play a role of scale, the nano activity in the plane direction of the scale can be adsorbed with the coating surface, the scale is in uniformly distributed laminated distribution parallel to the coating surface, a good laminated labyrinth effect is played, and the permeation path is greatly prolonged; and thirdly, the coating surface of the composite nanometer scale has the functions of repelling permeable molecules and ions and playing a role in permeation resistance.
3. The use of the composite nano-scale can greatly reduce the thickness of the scale coating: the performance of the nano-scale coating is no lower than that of the glass-scale coating when the thickness of the nano-scale coating is 1 percent of that of the glass-scale coating. It can also be said that the nano scale coating can be made very thin, and has very high scale effect. Ultra-thin coatings of less than 5 microns can be prepared.
4. The adhesive force is high: because the nanometer scale forms chemical adsorption, the mutual superposition of the scales can eliminate internal stress, and the internal stress of the coating is very low, the nanometer scale coating has excellent adhesive force to metal, concrete, wood, glass and the like.
5. The corrosion resistance is good: firstly, the general coating is damaged by corroding media along the interface between molecules and fillers or the interface between resin molecules, and the nano scale coating forms a three-dimensional net-shaped integral structure by chemical bonding and chemical adsorption to block corrosion channels; secondly, the coating has strong anti-permeability capability, and the corrosion speed is effectively slowed down; and thirdly, the composite nano scale is made of corrosion-resistant materials such as titanium, polytetrafluoroethylene, polyphenylene sulfide, stainless steel and graphene, and has good corrosion resistance.
6. The composite nanometer scale is compounded with nanometer characteristic of several kinds of material, and has more functions, including scale stuffing, reinforcing agent and modifier, so that the continuous composite nanometer scale may be endowed with the special functions of antiscaling, conducting, heat conducting, magnetic conducting, wax preventing, drag reducing, wear resisting, low surface energy, etc.
7. The coating can achieve better protection and functionalization effects only by coating once or twice, and compared with the existing coating, the coating is thin, the coating times are few, the coating consumption is small, and the coating material and the coating construction cost are saved.
The popularization and the application of the invention to the paint protection industry have revolutionary changes.
1. The preparation method of the composite nano scale material solves the problems of high cost, low efficiency and low quality in fine powder processing, and the method adopts the following common superfine process steps: the composite nano scale material is prepared by a one-step method through the simplified combination of crushing, mixing, dispersing, surface treatment, modification, decomposition, nano powder synthesis and the like, and the composite nano scale material is a one-dimensional nano material with the thickness of 1-40 nm and the radial dimension of 0.2-50 mu m. The composite nano scale prepared by more than two powder materials has the nano characteristics of multiple materials used for compounding, and has more functions.
2. The surface energy and surface tension of the composite nano scale material are large, so that the property of the particles is changed. The surface atoms of the particles are different from the internal atoms in crystal field environment and binding energy, have a plurality of dangling bonds and have unsaturated properties, so that the particles are easy to be combined with other atoms and tend to be stable, and have high chemical activity.
3. The metal nano-scale has the particle size smaller than that of visible light of metal, has small light reflectivity and good light absorption performance, and can be used for solar energy conversion and invisible materials; the heat conducting capacity is very strong, can be used to the indirect heating equipment.
Drawings
Fig. 1 is an electron microscope photograph of nano-scale flakes without dispersed titanium and graphene composite.
Fig. 2 is an electron microscope photograph of a single titanium and graphene composite nano-scale.
Detailed Description
The invention relates to a protective coating using thin composite nano scale material as filler, the composite nano scale is uniformly dispersed in the protective coating, and is uniformly distributed in a laminated manner parallel to a coating surface, and the coating resin is combined with the composite nano scale in a crosslinking manner, so that the coating can form an integral structure taking the nano scale as a node, and the strength and the toughness of the coating are improved; by utilizing the laminating effect of the composite nanometer flakes, the effects of eliminating the internal stress of the coating, prolonging the permeation path of a medium, increasing the permeation resistance of the coating and improving the adhesive force and the corrosion resistance of the coating are achieved, the aims of endowing the coating with special functions and excellent performance are achieved, the thickness of the coating is greatly reduced, and the coating material and the construction cost are saved.
The present invention is further described with reference to the following specific examples, which are not intended to be limiting, but are intended to be exemplary only in light of the teachings of the present invention and are not intended to be limiting.
A preparation method of a thin composite nano flake coating comprises the following steps:
(1) selecting resin base materials, wherein the resin base materials comprise one or more of epoxy resin base materials, epoxy phenolic resin base materials, polyphenylene sulfide resin base materials, polyurethane resin base materials, polyfluorinated resin base materials, fluorocarbon resin base materials, acrylic base materials, chlorinated rubber base materials, perchloroethylene base materials and alkyd base materials.
Selecting a composite nano flake material, wherein the thickness of the composite nano flake is 1-40 nm, and the size of the composite nano flake in the plane direction is 0.2-50 mu m; the one-dimensional composite nano scale material is uniform, active, multifunctional, highly dispersed, fully chemically bonded with a complexing agent, and coated by a protective agent, and is an active filler of a coating, a modifier and a coupling agent.
Selecting an auxiliary agent, and selecting two or more or all of an anti-settling agent, a thickening agent, a defoaming agent, a flatting agent, a dispersing agent, a wetting agent, a surface modifier, a coupling agent and a solvent prepared from the coating. The anti-settling agent is ultrafine powder or nano powder anti-settling agent or organic phosphate ester anti-settling agent, and is one or more of fumed silica, organic bentonite, N-methyl pyrrolidone solution of modified polyurea and organic phosphate ester F118; wherein the thickening agent comprises cellulose ethers, acrylic acid alkali swelling type, nonionic polyurethanes and hydrophobic modified alkali swelling type; the defoaming agent comprises: the coating defoaming agent comprises a water-based coating defoaming agent and a solvent-based coating defoaming agent, wherein the defoaming agent mainly comprises organic siloxane, polyether, silicon and ether graft, amine, imine and amide and is assisted by other defoaming agents; the leveling agent comprises: the aqueous paint leveling agent and the solvent paint leveling agent comprise high-boiling organic solvent or mixture thereof, isophorone, diacetone alcohol and Solvesso 150; the dispersant comprises: one or more of anionic dispersant, cationic dispersant, nonionic dispersant, amphoteric wetting dispersant, electric neutral wetting dispersant, macromolecular hyperdispersant and free radical hyperdispersant; the wetting agents include: low molecular weight surfactant and surface active polymer compound, one or more of polyoxyethylene alkyl phenyl ether and polyoxyethylene fatty acid ester; the surface modifier comprises: graphene, nano iron powder, nano flakes and composite nano flakes; the coupling agent is one or more of silane coupling agent or titanate coupling agent or nano scale or composite nano scale; the solvent is one or more of alcohols, ketones, benzenes, esters, reactive diluents and deionized water.
(2) The thin composite nano flake coating material comprises the following materials in percentage by weight:
a. the weight percentage of the resin base material and the composite nano scale material is as follows:
i, 10-90% of resin base material
II, 90-10% of composite nano flake material
The composite nano scale material is not only an active filler of the coating, but also a modifier and a coupling agent of the coating, the weight percentage of the composite nano scale material is selected according to the protection requirement or the protection grade requirement, and the principle is that when the protection requirement is high, the weight percentage of the composite nano scale material is increased;
b. the anti-settling agent accounts for 0.1-50% of the composite nano scale material by weight;
the thickener accounts for 0.1-40% of the composite nano scale material by weight percent;
the defoaming agent accounts for 0.1 to 30 percent of the composite nano scale material in percentage by weight
The weight percentage of the flatting agent in the composite nano scale material is 0.1-30%;
the dispersant accounts for 0.1-50% of the composite nano scale material by weight;
the wetting agent accounts for 0.1-40% of the composite nano scale material by weight percent;
the surface modifier accounts for 0.1-80% of the composite nano flake material by weight percent;
the coupling agent accounts for 0.1-50% of the composite nano scale material by weight;
the solvent accounts for 1-200% of the resin base material by weight;
(3) preparation:
mixing and dispersing the resin base material, the composite nano scale material and the selected auxiliary agent by using mixing and dispersing equipment according to the proportion. The mixing and dispersing equipment for preparing the thin composite nano flake coating comprises: a sand mill, a high-speed dispersion machine, a homogenizer and a continuous planetary ball mill; the mixing and dispersing time is 5-120 min.
The preparation method of the composite nano scale material comprises the following specific steps:
a. firstly, weighing base materials to be prepared into scales according to a formula, wherein the base materials prepared into the scales are solid powder materials, the particle size of the powder is 1-100 mu m, the base materials are two or more, one of the base materials is a main base material, the other base materials are auxiliary base materials, and the weight ratio of the base materials to the auxiliary base materials is 1: 0.1 to 1;
b. selecting grinding balls, wherein the hardness of the grinding balls is greater than that of the base material, the diameters of the grinding balls are not less than three size specifications, and the stacking volume of the grinding balls accounts for 30-70% of the volume of the grinding cylinder;
c. selecting an auxiliary agent, selecting two or more or all kinds of a coupling agent, an anti-settling agent, a dispersing agent, a protective agent and a solvent according to the weight of the base powder material of the prepared scale, wherein the weight ratio of the coupling agent to the base material for preparing the scale is 1: 50-100 parts; the anti-settling agent accounts for 0.1-20% of the weight of the base material; the dispersant accounts for 0.1-20% of the weight of the base material; the protective agent accounts for 0.5-30% of the weight of the base material; the solvent accounts for 10-800% of the weight of the base material;
d. b, putting the base material prepared from the scales in the steps a, b and c, the selected auxiliary agent and the grinding balls into an intermittent grinding machine according to the formula proportion, and dispersing, mixing and primarily grinding to uniformly disperse and mix several or all types of the base powder material prepared from the scales, the coupling agent, the anti-settling agent, the dispersing agent, the protective agent and the solvent;
e. and (d) when the composite nano scale is prepared, placing a grinding ball in a grinding cylinder of a continuous planetary ball mill, adjusting the grinding parameters of the continuous planetary ball mill, wherein the revolution speed is 100-1000 r/min, the rotation speed is 100-4000 r/min, and then, feeding the uniform material prepared in the step d into the continuous planetary ball mill by using a metering pump to prepare a uniform composite nano scale material, wherein the thickness of the uniform composite nano scale material reaches 1-40 nm, and the size of the scale in the plane direction is 0.2-50 mu m.
In the preparation method of the composite nano-scale material, the nano-scale base powder material can be one or more of metal powder, metal oxide powder, mineral powder, organic powder, graphite powder and multilayer graphene.
In the preparation method of the composite nano scale material, the grinding ball material can be bearing steel, stainless steel, agate, ceramic, titanium, alloy steel, diamond, cast stone or hard alloy, the grinding ball can be spherical or cylindrical or a mixed ball of the two, and the spherical diameter of the spherical grinding ball is 3-40 mm; the length-diameter ratio of the cylindrical grinding ball is 1-10: 1, the column diameter is 3-30 mm.
In the preparation method of the composite nano scale material, the coupling agent is one or more of silane coupling agent or titanate coupling agent; the anti-settling agent is one or more of superfine powder or a nano anti-settling agent; the dispersant is one or more of triethanolamine or surfactant; the protective agent is one or more of liquid polysulfide rubber, resin and a compound with more unsaturated double bonds of high molecular organic matter; the solvent is one or more of alcohols, ketones, benzenes, esters, reactive diluents and deionized water.
In the preparation method of the composite nano scale material, the continuous planetary ball mill is a wet continuous planetary ball mill.
Method for preparing coating of this application example 1
Thin titanium and graphene composite nano-scale epoxy phenolic coating (high-temperature curing type):
selecting a high-temperature curing type epoxy phenolic resin base material;
selecting titanium and graphene compounded nano flakes as a modifier and a coupling agent;
selecting fumed silica as an anti-settling agent;
the other auxiliary agents are respectively: xylene, butanol, acetone, a silane coupling agent, a nano dispersing agent and nano aluminum oxide;
the paint proportion (wt):
Figure BDA0002378045000000091
adding the components into a high-speed dispersion machine according to the weight percentage, rotating at 1000r/min, and mixing and dispersing in the high-speed dispersion machine for 30min to obtain the finished product of the thin titanium and graphene composite nano-scale epoxy phenolic coating.
The test effect is as follows:
coating thin titanium and graphene composite nano-scale epoxy phenolic coating once, wherein the dry film thickness is 15 mu m, and the coating is dried at 200 ℃ for 20min, and the performances are as follows:
detecting items Results
Boiling water at 100 deg.C for 120 hr Without change
10％NaOH 80℃ 120h Without change
3.5％NaCl 80℃ 120h Without change
10％H2SO4 80℃ 120h Without change
Method for preparing coating of this application example 2
Thin titanium and polytetrafluoroethylene composite nano-scale epoxy coating (normal temperature curing type):
1. selecting a normal-temperature cured epoxy resin base material;
2. selecting titanium and polytetrafluoroethylene composite nano flakes as a modifier and a coupling agent;
3. selecting organic bentonite F881 as an anti-settling agent;
4. other auxiliary agents are: xylene, butanol, titanate coupling agent and nano dispersant;
5. the paint proportion (wt):
Figure BDA0002378045000000101
adding the mixture into a high-speed dispersion machine according to the weight percentage, rotating at the speed of 1000r/min, and mixing and dispersing in the high-speed dispersion machine for 30min to obtain the finished thin titanium and polytetrafluoroethylene composite nano-scale epoxy coating.
The test effect is as follows:
the thin titanium and polytetrafluoroethylene composite nano-scale epoxy coating has a dry film thickness of 50 mu m and the following properties after being cured for 7 days at normal temperature:
detecting items Results
Boiling water at 100 deg.C for 30 days Without change
50% NaOH 30 days at 80 deg.C Without change
3.5% NaCl 30 days at 80 ℃ Without change
20％H2SO430 days at 80 DEG C Without change
Method for preparing coating of this application example 3
Thin titanium, polytetrafluoroethylene and graphene composite nano flake epoxy coating (high-temperature curing):
1. selecting a high-temperature curing epoxy resin base material;
2. selecting titanium, polytetrafluoroethylene and graphene composite nano flakes as a modifier and a coupling agent;
3. selecting organic bentonite SD-2 as an anti-settling agent;
4. other auxiliary agents are: xylene, butanol, a silane coupling agent, a titanate coupling agent and a nano dispersing agent;
5. the paint proportion (wt):
Figure BDA0002378045000000111
adding the components into a high-speed dispersion machine according to the weight percentage, rotating at 1000r/min, and mixing and dispersing in the high-speed dispersion machine for 30min to obtain the finished thin titanium, polytetrafluoroethylene and graphene composite nano-scale epoxy coating.
The test effect is as follows:
the thin titanium, polytetrafluoroethylene and graphene composite nano flake epoxy coating has the advantages that the thickness of a dry film is 40 mu m, the curing is carried out for 25min at 120 ℃, and the performance is as follows:
detecting items Results
Boiling water at 100 deg.C for 30 days Without change
50% NaOH 30 days at 80 deg.C Without change
3.5% NaCl 30 days at 80 ℃ Without change
20％H2SO430 days at 80 DEG C Without change
Fouling coefficient m2 ℃/KW 0.006
Method for preparing coating of this application example 4
Thin polytetrafluoroethylene and polyphenylene sulfide composite nano-scale high-temperature resistant water-based paint:
1. selecting organic silicon and epoxy composite emulsion as a resin base material;
2. selecting polytetrafluoroethylene and polyphenylene sulfide composite nano flakes as a modifier and a coupling agent;
3. selecting fumed silica as an anti-settling agent;
4. other auxiliary agents are: deionized water, a silane coupling agent, a 760W wetting dispersant, a BYK-018 antifoaming agent, a BYK-381 leveling agent, amino resin, a high-temperature film forming agent and a water-based nano dispersant;
5. the paint proportion (wt):
Figure BDA0002378045000000112
Figure BDA0002378045000000121
adding the components into a high-speed dispersion machine according to the weight percentage, rotating at the speed of 1200r/min, and mixing and dispersing the components in the high-speed dispersion machine for 30min to obtain the finished product of the thin polytetrafluoroethylene and polyphenylene sulfide composite nano-scale high-temperature resistant water-based coating.
The test effect is as follows:
the thin polytetrafluoroethylene and polyphenylene sulfide composite nano flake high-temperature resistant water-based paint has the advantages that the dry film thickness is 50 mu m, the curing is carried out for 24h at 25 ℃, and the film coating performance is as follows:
detecting items Results
Heat resistance of 300 ℃ for 3h Does not crack and pulverize
Neutral salt fog resistance, 500h By passing
Fouling coefficient m2 ℃/KW 0.006
The following describes specific experimental examples of composite nano-scale materials,
preparation example one of the composite nano scale material:
the preparation method comprises the steps of preparing polytetrafluoroethylene and graphene composite nano-scale, wherein an intermittent planetary ball mill is used for primary grinding, a continuous planetary ball mill is used for compounding, the main base material is 100-mesh polytetrafluoroethylene powder and auxiliary base material multi-layer graphene, the grinding balls are zirconia balls, and the coupling agent, the anti-settling agent, the dispersing agent, the protective agent and the solvent are respectively 3- (methacryloyloxy) propyl trimethoxy silane (KH-570), styryl phenol polyoxyethylene ether, dimethyl hydrochlorosilane, vinyl acetate and deionized water.
1. Weighing 100g of main base material polytetrafluoroethylene, 50g of auxiliary base material multilayer graphene, 3- (methacryloyloxy) propyl trimethoxy silane (KH-570), 4.5g of styrylphenol polyoxyethylene ether, 3g of vinyl acetate and 60g of deionized water.
2. The method is characterized in that five specifications of zirconia balls (13/16)' are selected for the auxiliary balls of the intermittent planetary ball mill; (19/32) "; (3/8) "; (5/16) "; (7/32) ". The weight of each zirconia ball calculated according to the volume of the ball milling working cylinder body is (13/16)' 320 g; (19/32) "150 g; (3/8) "100 g; (5/16) "15 g; (7/32) "15 g.
3. And (3) putting the mixture into an intermittent planetary ball mill according to the ball proportion and the material proportion, and carrying out primary grinding and mixing.
4. The method is characterized in that five specifications of zirconia balls (13/16)' are selected for ball matching of a continuous planetary ball mill; (19/32) "; (3/8) "; (5/16) "; (7/32) ". The weight of each zirconia ball calculated according to the volume of the ball milling working cylinder body is (13/16)' 320 g; (19/32) "150 g; (3/8) "100 g; (5/16) "15 g; (7/32) "15 g.
5. After the balls are loaded into a grinding cylinder of a continuous planetary ball mill according to the proportion, starting the continuous planetary ball mill, and adjusting the revolution speed to 350 r/min; the rotation speed is 1400 r/min. And (3) feeding the materials ground and mixed by the intermittent planetary ball mill into the continuous planetary ball mill by using a metering pump, adjusting the conveying flow, and monitoring and controlling the thickness of the polytetrafluoroethylene and graphene composite nano-scale to be 1-40 nm and the radial thickness of the one-dimensional nano-scale material to be 0.2-50 mu m.
The nano-scale material has the surface energy of nano-tetrafluoroethylene and the characteristics of graphene, is used for a water-based paint additive, and improves the permeation resistance, corrosion resistance, scaling resistance, thermal conductivity, light absorption, electric conductivity and the like of a coating.
Preparation example two:
in the preparation of the iron and cobalt composite nano scale, an intermittent planetary ball mill is used for primary grinding, a continuous planetary ball mill is used for compounding, the processed main base material is 200-mesh iron powder and the processed auxiliary base material is 300-mesh cobalt powder, grinding balls are steel balls, and a dispersing agent, a protective agent and a solvent are triethanolamine respectively; sodium hexametaphosphate; deionized water.
1. 100g of iron powder as a main base material; 100g of auxiliary base material cobalt powder; 10g of triethanolamine; 1g of sodium hexametaphosphate; 200g of water is added.
2. The method is characterized in that five specifications of zirconia balls (13/16)' are selected for the auxiliary balls of the intermittent planetary ball mill; (19/32) "; (3/8) "; (5/16) "; (7/32) ". The weight of each steel ball is (13/16)' 350g calculated according to the volume of the ball milling working cylinder body; (19/32) "160 g; (3/8) "110 g; (5/16) "20 g; (7/32) "20 g.
3. And (3) putting the mixture into an intermittent planetary ball mill according to the ball proportion and the material proportion, and carrying out primary grinding and mixing.
4. Five specifications of steel balls (13/16) "are selected for matching the balls of the continuous planetary ball mill; (19/32) "; (3/8) "; (5/16) "; (7/32) ". The weight of each steel ball is (13/16)' 350g calculated according to the volume of the ball milling working cylinder body; (19/32) "160 g; (3/8) "110 g; (5/16) "20 g; (7/32) "20 g.
5. After the balls are assembled, starting the continuous planetary ball mill, and adjusting the revolution speed to 370 r/min; the spinning speed is 1480 r/min. And (3) feeding the materials ground and mixed by the intermittent planetary ball mill into the continuous planetary ball mill by using a metering pump, adjusting the conveying flow, and monitoring and controlling the one-dimensional nano-scale composite material with the thickness of 1-40 nm and the radial thickness of 0.2-50 mu m of the iron and cobalt composite nano-scale.
The powder can be used for magnetorheological fluid materials.
Preparation example three:
the preparation method comprises the steps of preparing titanium powder and graphene composite nano flakes, wherein an intermittent planetary ball mill is used for primary grinding, a continuous planetary ball mill is used for compounding, the processed main base materials are 320-mesh titanium powder and auxiliary base material multi-layer graphene, the grinding balls are stainless steel balls, and the coupling agent, the anti-settling agent, the dispersing agent, the protective agent and the solvent are respectively 3-glycidoxy propyl trimethoxy silane (KH-560), nano alumina, epoxy resin, polysulfide rubber and an epoxy active solvent.
1. 100g of main base material titanium, 40g of auxiliary base material multilayer graphene, 3g of 3-glycidoxypropyltrimethoxysilane (KH-560), 2.8g of nano-alumina, 8.4g of epoxy resin, 8.4g of polysulfide rubber and 42g of epoxy active solvent are weighed and mixed.
2. Five specifications of stainless steel balls (13/16)' are selected for matching the batch planetary ball mill and the continuous planetary ball mill; (19/32) "; (3/8) "; (5/16) "; (7/32) ".
The weight of each stainless steel ball is (13/16)' 350g calculated according to the volume of the ball milling working cylinder body; (19/32) "180 g; (3/8) "120 g; (5/16) "25 g; (7/32) "25 g.
3. Adding the mixture and balls into an intermittent planetary ball mill according to the mixture ratio, wherein the revolution speed is 350 r/min; the rotation speed was 1400r/min, and primary grinding and mixing were carried out for 2 hours.
4. After the balls of the continuous planetary ball mill are assembled, starting the continuous planetary ball mill, and adjusting the revolution speed to 400 r/min; the rotation speed is 1600 r/min. And (3) feeding the materials ground and mixed by the intermittent planetary ball mill into the continuous planetary ball mill by using a metering pump, adjusting the conveying flow, and monitoring and controlling the thickness of the titanium and graphene composite nano-scale to be 1-40 nm and the radial thickness of the one-dimensional nano-scale material to be 0.2-50 mu m. The first picture is an electron microscope photograph of nano-scale flakes compounded by titanium and graphene without dispersion; and the second picture is an electron microscope photograph of the single titanium and graphene compounded nano scale.
The nano-scale material has the characteristics and functions of a titanium nano-material and a graphene material, is used as a coating additive, and improves the permeation resistance, corrosion resistance, scaling resistance, thermal conductivity, light absorption, electrical conductivity and the like of a coating.
Preparation example four:
the preparation method comprises the steps of preparing nano-scale compounded by titanium powder, graphene and polytetrafluoroethylene, wherein an intermittent planetary ball mill is used for primary grinding, a continuous planetary ball mill is used for compounding, the processed main base material is 320-mesh titanium powder, the processed auxiliary base material is multilayer graphene, the processed auxiliary base material is 100-mesh polytetrafluoroethylene powder, the grinding balls are stainless steel balls, and the coupling agent, the anti-settling agent, the dispersing agent, the protective agent and the solvent are respectively 3-glycidoxy propyl trimethoxy silane (KH-560), nano-alumina, epoxy resin, polysulfide rubber and an epoxy active solvent.
1. Selecting 100g of main base material titanium, 30g of auxiliary base material graphene, 20g of auxiliary base material polytetrafluoroethylene, 3g of 3-glycidyl ether oxypropyltrimethoxysilane (KH-560), 3g of nano-alumina, 9g of epoxy resin and 9g of polysulfide rubber; and compounding 45g of epoxy active solvent.
2. Five specifications of stainless steel balls (13/16)' are selected for matching the batch planetary ball mill and the continuous planetary ball mill; (19/32) "; (3/8) "; (5/16) "; (7/32) ".
The weight of each stainless steel ball is (13/16)' 350g calculated according to the volume of the ball milling working cylinder body; (19/32) "180 g; (3/8) "120 g; (5/16) "25 g; (7/32) "25 g.
3. Adding the mixture and balls into an intermittent planetary ball mill according to the mixture ratio, wherein the revolution speed is 350 r/min; the rotation speed was 1400r/min, and primary grinding and mixing were carried out for 2 hours.
4. After the balls of the continuous planetary ball mill are assembled, starting the continuous planetary ball mill, and adjusting the revolution speed to 400 r/min; the rotation speed is 1600 r/min. And (3) feeding the materials ground and mixed by the intermittent planetary ball mill into the continuous planetary ball mill by using a metering pump, adjusting the conveying flow, and monitoring and controlling the thickness of the titanium and graphene composite nano-scale to be 1-30 nm and the radial thickness of the one-dimensional nano-scale material to be 0.2-50 mu m.
The nano-scale material has the characteristics and functions of a titanium nano-material, a graphene material and nano-thickness polytetrafluoroethylene, is used as a coating additive, and improves the permeation resistance, corrosion resistance, low surface energy, scaling resistance, thermal conductivity, light absorption, electrical conductivity and the like of a coating.

Claims (6)

1. A preparation method of a thin composite nano flake coating is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) selecting a resin base material; selecting a composite nano scale material; selecting an auxiliary agent, wherein the auxiliary agent is two or more or all of an anti-settling agent, a thickening agent, a defoaming agent, a leveling agent, a dispersing agent, a wetting agent, a surface modifier, a coupling agent and a solvent;
(2) the proportion of the thin composite nano flake coating material is as follows:
a. the weight percentage of the resin base material and the composite nano scale material is as follows:
i, 10-90% of resin base material
II, 90-10% of composite nano flake material
b. The anti-settling agent accounts for 0.1-50% of the composite nano scale material by weight;
the thickener accounts for 0.1-40% of the composite nano scale material by weight percent;
the defoaming agent accounts for 0.1 to 30 percent of the composite nano scale material in percentage by weight
The weight percentage of the flatting agent in the composite nano scale material is 0.1-30%;
the dispersant accounts for 0.1-50% of the composite nano scale material by weight;
the wetting agent accounts for 0.1-40% of the composite nano scale material by weight percent;
the surface modifier accounts for 0.1-80% of the composite nano flake material by weight percent;
the coupling agent accounts for 0.1-50% of the composite nano scale material by weight;
the solvent accounts for 1-200% of the resin base material by weight;
(3) preparation:
mixing and dispersing the resin base material, the composite nano flake material and the selected auxiliary agent by using mixing and dispersing equipment according to the proportion;
the composite nano flake material is prepared by the following method,
a. at first, weigh the base material that will prepare into the scale, the base material of its scale preparation is solid powder material, and the particle size of powder is at 1 ~ 100 mu m, and base material is two kinds or more, and one of them is main base material, and other are supplementary base material, and base material and supplementary base material's weight ratio is 1: 0.1 to 1;
b. selecting grinding balls, wherein the hardness of the grinding balls is greater than that of the base material, the diameters of the grinding balls are not less than three size specifications, and the stacking volume of the grinding balls accounts for 30-70% of the volume of the grinding cylinder;
c. selecting an auxiliary agent, selecting two or more or all kinds of coupling agent, anti-settling agent, dispersing agent, protective agent and solvent according to the total weight of the main base material and the auxiliary base material of the prepared scale, wherein the weight ratio of the coupling agent to the total base material for preparing the scale is 1: 50-100 parts; the anti-settling agent accounts for 0.1-20% of the total weight of the base material; the dispersant accounts for 0.1-20% of the total weight of the base material; the protective agent accounts for 0.5-30% of the total weight of the base material; the solvent accounts for 10-800% of the total weight of the base material;
d. b, preparing a base material from the scales in the steps a, b and c, selecting an auxiliary agent and grinding balls, putting the base material, the selected auxiliary agent and the grinding balls into an intermittent planetary ball mill according to a formula proportion, and dispersing, mixing and primarily grinding the base material, the coupling agent, the anti-settling agent, the dispersing agent, the protective agent and the solvent to be uniformly dispersed and mixed;
e. preparing composite nano scales: b, according to the ball distribution in the step b, placing grinding balls in a grinding cylinder of a continuous planetary ball mill, adjusting grinding parameters of the continuous planetary ball mill, wherein the revolution speed is 100-1000 r/min, the rotation speed is 100-4000 r/min, and then sending the uniform material prepared in the step d into the continuous planetary ball mill by using a metering pump to prepare a uniform composite nano scale material, wherein the thickness of the uniform composite nano scale material reaches 1-40 nm, and the size of the sheet in the plane direction is 0.2-50 mu m;
the nano-scale base material and the auxiliary base material can be two or more of metal powder, metal oxide powder, mineral powder, organic powder, graphite powder and multilayer graphene.
2. The method for preparing the thin composite nano flake coating according to claim 1, wherein the method comprises the following steps: the resin base material comprises an epoxy resin base material and an epoxy phenolic resin base material.
3. The method for preparing the thin composite nano flake coating according to claim 1, wherein the method comprises the following steps: the grinding ball material can be bearing steel, stainless steel, agate, ceramic, titanium, alloy steel, diamond, cast stone or hard alloy, the shape of the grinding ball can be spherical or cylindrical or a mixture of the spherical and cylindrical grinding balls, and the spherical diameter of the spherical grinding ball is 3-40 mm; the length-diameter ratio of the cylindrical grinding ball is 1-10: 1, the column diameter is 3-30 mm.
4. The method for preparing the thin composite nano flake coating according to claim 1, wherein the method comprises the following steps: the continuous planetary ball mill is a wet continuous planetary ball mill.
5. The method for preparing the thin composite nano flake coating according to claim 1, wherein the method comprises the following steps: the composite nano flake material is an active filler of the coating, a modifier and a coupling agent of the coating, the weight percentage of the composite nano flake material is selected according to the protection requirement or the protection grade requirement, and the principle is that when the protection requirement is high and the protection grade is high, the weight percentage of the composite nano flake material is increased.
6. The method for preparing the thin composite nano flake coating according to claim 1, wherein the method comprises the following steps: the mixing and dispersing equipment for preparing the thin composite nano flake coating comprises: a sand mill, a high-speed dispersion machine, a homogenizer and a continuous planetary ball mill; the mixing and dispersing time is 5-120 min.
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