CN110484064A - A kind of aluminum paste fluorocarbon coating and preparation method thereof - Google Patents
A kind of aluminum paste fluorocarbon coating and preparation method thereof Download PDFInfo
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- CN110484064A CN110484064A CN201910809300.7A CN201910809300A CN110484064A CN 110484064 A CN110484064 A CN 110484064A CN 201910809300 A CN201910809300 A CN 201910809300A CN 110484064 A CN110484064 A CN 110484064A
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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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/103—Anti-corrosive paints containing metal dust containing Al
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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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of aluminum paste fluorocarbon coatings, including following component based on parts by weight: 18-35 parts of water-based fluorocarbon resin, 13-24 parts of polyurethane resin, 0.5-1 parts of titanate esters modified graphene, 0.2-1 parts of silane coupling agent, 6-23 parts of water aluminum-silver slurry, 1-3 parts of opal shale micro mist, opal shale micro mist loads TiO22-5 parts, 5-9 parts of ethylene glycol, 0.1-1.5 parts of dispersing agent, 0.1-1.5 parts of levelling agent, 0.3-1.5 parts of defoaming agent, 0.1-0.6 parts of pH adjusting agent, 15-28 parts of deionized water.The present invention is mixed in proportion using water-based fluorocarbon resin and polyurethane resin as basis material, so that coating has good comprehensive performance, opal shale micro mist used and titanate esters modified graphene, silane coupling agent and polyethylene glycol collectively promote aligning for aluminum paste, and coating is made to have high metal luster.
Description
Technical field
The present invention relates to technical field of coatings, and in particular to a kind of aluminum paste fluorocarbon coating and preparation method thereof.
Background technique
Aluminum paste is a kind of pulpous state metallic pigments by certain process, and aluminium shape has flakes, fish scale-shaped and silver
First shape, its main feature is that aluminum flake surface is smooth, size distribution is concentrated, regular shape, has excellent luminous reflectanc and gold
Belong to gloss, be used in mixed way with transparent pigment, paint film has apparent effect, and the magnificent beauty of decorative effect is main to use
In car paint, plastic paint, metal industry coating, marine paint, heat-resisting paint, roof coating etc..
Fluorocarbon coating has many advantages, such as water resistance, solvent resistance, stain resistance, hardness height, weatherability, durability.But
Current fluorocarbon coating is based on solvent type, and containing higher VOC, solvent directly evaporate into air and can not recycle when construction,
It results in waste of resources, pollutes environment, and also have certain murder by poisoning to construction personnel.
Chinese patent literature CN107033710A discloses a kind of preparation method of breathable environment-protective fluorocarbon coating, by carbon nanometer
Pipe, which is placed in 1- hexyl -3- methyl imidazolium tetrafluoroborate, to be impregnated, and is dried, and heating, heat preservation obtains the first prefabricated material；By talcum
Powder, Titanium Nitrate, saturation ammonium hydroxide, water are uniformly mixed, and hydro-thermal reaction is dried to obtain the second prefabricated material；It is added into the first prefabricated material
Second prefabricated material, chlorosulfonated polyethylene, titanate coupling agent, heating, are dried to obtain first material；Xiang Shuizhong sequentially adds cocounut oil
Amido propyl betaine, polyvinyl alcohol stir evenly, and continuously add pH adjusting agent, defoaming agent, first material, gas phase titanium dioxide
Silicon, carbon fiber, water aluminum-silver slurry, coalescing agent, are uniformly mixing to obtain second material；Fluorine richness propylene is added into second material
Acid esters lotion, epoxy resin latex, preservative, mould inhibitor stirring, continuously add xanthan gum, polyether polyester modified organic silicon oxygen
Alkane, adhesion promoter are uniformly mixing to obtain breathable environment-protective fluorocarbon coating.Coating tensile strength with higher, shock resistance
Intensity is not easily broken, and thermostabilization is good, and ageing-resistant performance is excellent, and excellent anti-corrosion performance is not high but there are glossiness, and VOC is released
It is high-volume only able to satisfy standard, is less than 50g/L, the feature of environmental protection need the problem of being improved, and preparation step is cumbersome, raw materials used type
It is more, it is at high cost.
That there are VOC is excessively high for existing aluminum paste fluorocarbon coating, aluminum paste align it is poor cause reflecting feel not strong, adhesive force
The problems such as poor, corrosion resistance is not strong, is easy blistering.Therefore research and develop that low VOC, reflecting feel are strong, adhesive force is strong and good corrosion resistance
Water aluminum-silver slurry fluorocarbon coating be of great significance.
Summary of the invention
The present invention provide it is a kind of there is high gloss, enhanced water resistance and corrosion resistance, prepare it is simple, at low cost, can be in batches
Environment-friendly type aluminum paste fluorocarbon coating of production and preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions:
A kind of aluminum paste fluorocarbon coating, including following component based on parts by weight: 18-35 parts of water-based fluorocarbon resin, gathering
13-24 parts of urethane resin, 0.5-1 parts of titanate esters modified graphene, 0.2-1 parts of silane coupling agent, 6-23 parts of water aluminum-silver slurry, egg
1-3 parts of white stone shale micro mist, opal shale micro mist load TiO22-5 parts, 5-9 parts of ethylene glycol, 0.1-1.5 parts of dispersing agent, stream
Flat agent 0.1-1.5 parts, 0.3-1.5 parts of defoaming agent, 0.1-0.6 parts of pH adjusting agent, 15-28 parts of deionized water.
Further, the titanate esters modified graphene the preparation method comprises the following steps: graphite oxide is placed in reactor, ultrasound
Processing after graphite to be oxidized is completely dispersed, adjusts pH to 9-10,80 DEG C of constant temperature, hydrazine hydrate and titanate esters coupling is then added
Agent TM-200S reacts 8h, filters, wash while hot repeatedly, until filtrate is in neutrality to get titanate esters modified graphene.
Further, graphene oxide and titanate coupling agent TM-200S in the preparation method of titanate esters modified graphene
Mass ratio be 1:7.
Further, the water aluminum-silver slurry is double-coating aluminum paste, preparation method are as follows: by coated with silica aluminium
Silver paste disperses in ethanol, to sequentially add methyl methacrylate monomer, Butyl Acrylate Monomer, Hexafluorobutyl mathacrylate
Then monomer and acrylic monomers are added initiator azodiisobutyronitrile, stir evenly at room temperature, be warming up to 70 DEG C, constant temperature is anti-
5h is answered, the aluminum paste to get fluorinated acrylate and silica double-coating is filtered.
Further, the partial size of the opal shale micro mist is 10-20 μm.
Further, the opal shale micro mist loads TiO2The preparation method comprises the following steps: (1) opal shale micro mist in horse
3h is not calcined in furnace under the conditions of 300 DEG C, it is 15% phosphoric acid that calcined opal shale micro mist, which is then immersed in mass concentration,
In solution for 24 hours, it filters and washs to neutral spare；(2) titanyl sulfate is added in distilled water, heating stirring, until completely molten
It is filtered after solution, takes filtrate, opal shale micro mist made from step (1) is added in filtrate；(3) by mixed filtrate water
Bath is warming up to 75 DEG C, and precipitating reagent weak aqua ammonia is added dropwise, and after measuring pH=10, stops being added dropwise, continues water-bath 1h, filtering, gained
Filter residue is placed in baking oven dry 2h, and drying temperature is 120 DEG C, finally takes out and grinds to obtain the final product.
Further, the average molecular weight of the polyethylene glycol is 4000.
Further, the dispersing agent is sodium polycarboxylate dipersant；The levelling agent is hyperbranched type organosilicon levelling
Agent；The defoaming agent is Siloxane-Oxyalkylene Copolymers defoaming agent.
A kind of preparation method of aluminum paste fluorocarbon coating, comprising the following steps:
Step 1: portions of de-ionized water addition is fed intake in kettle, it is micro- to sequentially add water aluminum-silver slurry, opal shale
Powder, titanate esters modified graphene, silane coupling agent, after mixing evenly, ultrasonic treatment obtains aluminum paste pre-dispersed liquid；
Step 2: remaining number deionized water is added into blend tank, water-based fluorocarbon resin, polyurethane tree is then added
Rouge, ethylene glycol, opal shale micro mist load TiO2, after mixing evenly, aluminum paste pre-dispersed liquid obtained by step 1 is added and is adjusted
In distribution tank, continue to stir, add dispersing agent, levelling agent, defoaming agent and pH adjusting agent, continues to stir, obtain seasoning liquid；
Step 3: seasoning liquid after mixing evenly is crossed 200 meshes to get aluminum paste fluorocarbon coating.
Further, the power being ultrasonically treated in step 1 is 200W, and the time is 40~60min.
The present invention uses water-based fluorocarbon resin, polyurethane resin for coating matrix material, water-based fluorocarbon resin crosslinking used
Density is high, has good weatherability, and aqueous polyester resin has good oil resistivity, toughness, wearability, and metatitanic acid is ester modified
Graphene can be coupled with resin, since graphene has high mechanical strength, high temperature resistant, corrosion resistant good characteristic, with tree
The combination of aliphatic radical body can be improved coating comprehensive performance, while the PEG-4000 being added in preparation process can be with opal shale
The carrier as solid dispersion is cooperateed with, achievees the purpose that solid is promoted to disperse, after coating decoration, the two can adjust solvent and wave
Rate is sent out, aligns aluminum paste, to improve coating metal gloss；In addition, passing through silane coupling agent and basis material knot
The porous nanometer structure of the opal nano powder of conjunction also can effectively prevent coating cracking, be bubbled.
It uses coated with silica aluminum paste for raw material in the preparation method of water aluminum-silver slurry of the present invention, makes itself and four kinds of lists
Body hybrid reaction, wherein methyl methacrylate assigns clad hardness；Hexafluorobutyl mathacrylate makes clad two
Silica aluminum paste surface has good adhesive force, while improving the ageing resistance of clad；Butyl acrylate makes to coat
Layer has flexibility；Acrylic acid assigns the good mechanical stability of clad, advanced optimizes, ratio is methyl methacrylate
Aqueous aluminium when monomer, Butyl Acrylate Monomer, Hexafluorobutyl mathacrylate monomer and acrylic monomers 2:4:3:6 in mass ratio
The hydrophobicity of silver paste, resistance to acid and alkali, the ageing-resistant and best performance of resistance to soluble-salt.
The present invention carries out high-temperature calcination to opal shale micro mist first and phosphoric acid handles the activation of two steps, increases its specific surface
Product, simple TiO2Without visible light catalysis activity, and the opal after being activated is supported on by hydrolysis methods
After on shale micro mist, good anatase titanium dioxide is obtained, while remaining p and s element pair in opal shale
Titanium dioxide crystal is doped, so that opal shale micro mist loads TiO2Visible light catalytic efficiency up to 90%.
The present invention water aluminum-silver slurry is carried out in deionized water first it is pre-dispersed, by be added opal shale micro mist,
Titanate esters modified graphene, silane coupling agent, under ultrasonication, silane coupling agent and titanate esters modified graphene can be with albumen
Stone shale micropowder bonded, forms continuous network structure, and water aluminum-silver slurry is promoted to be uniformly dispersed, and is conducive to determining for aluminium powder in coating
To arrangement, silane coupling agent contains cross-linkable solidifying group-OCH due to it3, can after step 2 is mixed with resin component
Solidification is crosslinked, the mechanical strength and hardness of coating are improved；Titanate esters modified graphene can be with opal shale and aqueous
The surface group of aluminum paste is coupled, and improves the dispersing uniformity and mobility of aluminum paste pre-dispersed liquid, moreover it is possible to coating be avoided to generate
Piebald.
Opal shale micro mist of the present invention loads TiO2Catalyst is in situ by the activated protein stone micro mist of large specific surface area
Load TiO2, the phenomenon that not only effectively preventing directly adding titanium dioxide nano-particle inactivation easy to reunite in coating, but also make
Obtain TiO2With it is very high can by photocatalytic activity, under silane coupling agent effect catalyst can with aluminum paste in coating
Even distribution, good compatibility is firmly combined it with coating matrix between opal shale micro mist and matrix resin, catalyst
Particle not easily runs off in coating use process；Due to opal shale have good absorption property, can adsorbed gas have
Machine pollutant provides higher reactant concentration for light-catalyzed reaction, further improves rate of photocatalytic oxidation, substantially reduce
The VOC of coating.
Compared with the prior art, the invention has the following beneficial effects:
(1) aluminum paste fluorocarbon coating provided by the invention, water aluminum-silver slurry used pass through double-coating, and reflecting feel is strong, lead to
Cross addition opal shale micro mist, titanate esters modified graphene, silane coupling agent can without using acetylbutyrylcellulose
Promote aluminum paste aligning in the coating, so that gloss can achieve 90 or more, reduces coating cost, and aluminum paste has
There are good water resistance, wearability and corrosion resistance, gloss, which is used for a long time, not to be reduced；
(2) aluminum paste fluorocarbon coating provided by the invention, is mixed in proportion by water-based fluorocarbon resin and polyurethane resin
As basis material, the good characteristic that both can be integrated, so that coating has good impact strength, tensile strength, resistance to
Mill property and weatherability, titanate esters modified graphene used can also be coupled with resin matrix and be combined, and further increase the intensity of coating
And corrosion resistance, opal shale micro mist used is light compared with other inorganic fillers, so that coating easily disperses, do not settle,
The solid dispersibility for improving coating jointly with PEG-4000, promotes aligning for aluminum paste；
(3) aluminum paste fluorocarbon coating provided by the invention, added opal shale micro mist load TiO2It can not only
Absorb ultraviolet light, moreover it is possible to which reflection and scatters ultraviolet substantially increase the ultraviolet-resistant aging performance of coating, also have very high
Can be by photocatalytic activity, the organic pollutant that can adsorb opal shale decomposes rapidly mineralising, while opal shale is micro-
Powder can also discharge anion, purify air.
(4) aluminum paste fluorocarbon coating provided by the invention, preparation method is simple, at low cost, to metal, plastic cement, concrete
Substrate has good adhesive force, has a wide range of application.
Specific embodiment
Further to illustrate technological means and its effect adopted by the present invention, carried out below in conjunction with specific embodiment detailed
Thin description.
Embodiment 1
A kind of aluminum paste fluorocarbon coating, including following component based on parts by weight: 18 parts of water-based fluorocarbon resin, polyurethane
13 parts of resin, 0.5 part of titanate esters modified graphene, 0.2 part of silane coupling agent, 6 parts of water aluminum-silver slurry, opal shale micro mist 1
Part, opal shale micro mist loads TiO22 parts, 5 parts of ethylene glycol, 0.1 part of dispersing agent, 0.1 part of levelling agent, 0.3 part of defoaming agent,
0.1 part of pH adjusting agent, 15 parts of deionized water.
Further, the titanate esters modified graphene the preparation method comprises the following steps: graphite oxide is placed in reactor, ultrasound
Processing after graphite to be oxidized is completely dispersed, adjusts pH to 9-10,80 DEG C of constant temperature, hydrazine hydrate and titanate esters coupling is then added
Agent TM-200S reacts 8h, filters, wash while hot repeatedly, until filtrate is in neutrality to get titanate esters modified graphene.
Further, graphene oxide and titanate coupling agent TM-200S in the preparation method of titanate esters modified graphene
Mass ratio be 1:7.
Further, the water aluminum-silver slurry is double-coating aluminum paste, preparation method are as follows: by coated with silica aluminium
Silver paste disperses in ethanol, to sequentially add methyl methacrylate monomer, Butyl Acrylate Monomer, Hexafluorobutyl mathacrylate
Then monomer and acrylic monomers are added initiator azodiisobutyronitrile, stir evenly at room temperature, be warming up to 70 DEG C, constant temperature is anti-
5h is answered, the aluminum paste to get fluorinated acrylate and silica double-coating is filtered.
Further, the partial size of the opal shale micro mist is 10-20 μm.
Further, the opal shale micro mist loads TiO2The preparation method comprises the following steps: (1) opal shale micro mist in horse
3h is not calcined in furnace under the conditions of 300 DEG C, it is 15% phosphoric acid that calcined opal shale micro mist, which is then immersed in mass concentration,
In solution for 24 hours, it filters and washs to neutral spare；(2) titanyl sulfate is added in distilled water, heating stirring, until completely molten
It is filtered after solution, takes filtrate, opal shale micro mist made from step (1) is added in filtrate；(3) by mixed filtrate water
Bath is warming up to 75 DEG C, and precipitating reagent weak aqua ammonia is added dropwise, and after measuring pH=10, stops being added dropwise, continues water-bath 1h, filtering, gained
Filter residue is placed in baking oven dry 2h, and drying temperature is 120 DEG C, finally takes out and grinds to obtain the final product.
Further, the dispersing agent is sodium polycarboxylate dipersant；The levelling agent is hyperbranched type organosilicon levelling
Agent；The defoaming agent is Siloxane-Oxyalkylene Copolymers defoaming agent.
A kind of preparation method of aluminum paste fluorocarbon coating, comprising the following steps:
Step 1: the addition of 5 parts of deionized waters is fed intake in kettle, sequentially add water aluminum-silver slurry, opal shale micro mist,
Titanate esters modified graphene, silane coupling agent, after mixing evenly, ultrasonic treatment obtains aluminum paste pre-dispersed liquid；
Step 2: remaining 10 parts of deionized waters are added into blend tank, water-based fluorocarbon resin, polyurethane tree is then added
Rouge, ethylene glycol, opal shale micro mist load TiO2, after mixing evenly, aluminum paste pre-dispersed liquid obtained by step 1 is added and is adjusted
In distribution tank, continue to stir, add dispersing agent, levelling agent, defoaming agent and pH adjusting agent, continues to stir, obtain seasoning liquid；
Step 3: seasoning liquid after mixing evenly is crossed 200 meshes to get aluminum paste fluorocarbon coating.
Further, the power being ultrasonically treated in step 1 is 200W, time 40min.
Embodiment 2
A kind of aluminum paste fluorocarbon coating, including following component based on parts by weight: 22 parts of water-based fluorocarbon resin, polyurethane
15 parts of resin, 0.6 part of titanate esters modified graphene, 0.3 part of silane coupling agent, 8 parts of water aluminum-silver slurry, opal shale micro mist
1.5 parts, opal shale micro mist loads TiO23 parts, 6 parts of ethylene glycol, 0.5 part of dispersing agent, 0.5 part of levelling agent, defoaming agent 0.6
Part, 0.2 part of pH adjusting agent, 17 parts of deionized water.
Further, the titanate esters modified graphene the preparation method comprises the following steps: graphite oxide is placed in reactor, ultrasound
Processing after graphite to be oxidized is completely dispersed, adjusts pH to 9-10,80 DEG C of constant temperature, hydrazine hydrate and titanate esters coupling is then added
Agent TM-200S reacts 8h, filters, wash while hot repeatedly, until filtrate is in neutrality to get titanate esters modified graphene.
Further, graphene oxide and titanate coupling agent TM-200S in the preparation method of titanate esters modified graphene
Mass ratio be 1:7.
Further, the water aluminum-silver slurry is double-coating aluminum paste, preparation method are as follows: by coated with silica aluminium
Silver paste disperses in ethanol, to sequentially add methyl methacrylate monomer, Butyl Acrylate Monomer, Hexafluorobutyl mathacrylate
Then monomer and acrylic monomers are added initiator azodiisobutyronitrile, stir evenly at room temperature, be warming up to 70 DEG C, constant temperature is anti-
5h is answered, the aluminum paste to get fluorinated acrylate and silica double-coating is filtered.
Further, the partial size of the opal shale micro mist is 10-20 μm.
Further, the opal shale micro mist loads TiO2The preparation method comprises the following steps: (1) opal shale micro mist in horse
3h is not calcined in furnace under the conditions of 300 DEG C, it is 15% phosphoric acid that calcined opal shale micro mist, which is then immersed in mass concentration,
In solution for 24 hours, it filters and washs to neutral spare；(2) titanyl sulfate is added in distilled water, heating stirring, until completely molten
It is filtered after solution, takes filtrate, opal shale micro mist made from step (1) is added in filtrate；(3) by mixed filtrate water
Bath is warming up to 75 DEG C, and precipitating reagent weak aqua ammonia is added dropwise, and after measuring pH=10, stops being added dropwise, continues water-bath 1h, filtering, gained
Filter residue is placed in baking oven dry 2h, and drying temperature is 120 DEG C, finally takes out and grinds to obtain the final product.
Further, the dispersing agent is sodium polycarboxylate dipersant；The levelling agent is hyperbranched type organosilicon levelling
Agent；The defoaming agent is Siloxane-Oxyalkylene Copolymers defoaming agent.
A kind of preparation method of aluminum paste fluorocarbon coating, comprising the following steps:
Step 1: the addition of 6 parts of deionized waters is fed intake in kettle, sequentially add water aluminum-silver slurry, opal shale micro mist,
Titanate esters modified graphene, silane coupling agent, after mixing evenly, ultrasonic treatment obtains aluminum paste pre-dispersed liquid；
Step 2: remaining 11 parts of deionized waters are added into blend tank, water-based fluorocarbon resin, polyurethane tree is then added
Rouge, ethylene glycol, opal shale micro mist load TiO2, after mixing evenly, aluminum paste pre-dispersed liquid obtained by step 1 is added and is adjusted
In distribution tank, continue to stir, add dispersing agent, levelling agent, defoaming agent and pH adjusting agent, continues to stir, obtain seasoning liquid；
Step 3: seasoning liquid after mixing evenly is crossed 200 meshes to get aluminum paste fluorocarbon coating.
Further, the power being ultrasonically treated in step 1 is 200W, time 45min.
Embodiment 3
A kind of aluminum paste fluorocarbon coating, including following component based on parts by weight: 30 parts of water-based fluorocarbon resin, polyurethane
20 parts of resin, 0.8 part of titanate esters modified graphene, 0.9 part of silane coupling agent, 19 parts of water aluminum-silver slurry, opal shale micro mist 2
Part, opal shale micro mist loads TiO24 parts, 8 parts of ethylene glycol, 1 part of dispersing agent, 1 part of levelling agent, 1 part of defoaming agent, pH is adjusted
0.5 part of agent, 23 parts of deionized water.
Further, the titanate esters modified graphene the preparation method comprises the following steps: graphite oxide is placed in reactor, ultrasound
Processing after graphite to be oxidized is completely dispersed, adjusts pH to 9-10,80 DEG C of constant temperature, hydrazine hydrate and titanate esters coupling is then added
Agent TM-200S reacts 8h, filters, wash while hot repeatedly, until filtrate is in neutrality to get titanate esters modified graphene.
Further, graphene oxide and titanate coupling agent TM-200S in the preparation method of titanate esters modified graphene
Mass ratio be 1:7.
Further, the water aluminum-silver slurry is double-coating aluminum paste, preparation method are as follows: by coated with silica aluminium
Silver paste disperses in ethanol, to sequentially add methyl methacrylate monomer, Butyl Acrylate Monomer, Hexafluorobutyl mathacrylate
Then monomer and acrylic monomers are added initiator azodiisobutyronitrile, stir evenly at room temperature, be warming up to 70 DEG C, constant temperature is anti-
5h is answered, the aluminum paste to get fluorinated acrylate and silica double-coating is filtered.
Further, the partial size of the opal shale micro mist is 10-20 μm.
Further, the opal shale micro mist loads TiO2The preparation method comprises the following steps: (1) opal shale micro mist in horse
3h is not calcined in furnace under the conditions of 300 DEG C, it is 15% phosphoric acid that calcined opal shale micro mist, which is then immersed in mass concentration,
In solution for 24 hours, it filters and washs to neutral spare；(2) titanyl sulfate is added in distilled water, heating stirring, until completely molten
It is filtered after solution, takes filtrate, opal shale micro mist made from step (1) is added in filtrate；(3) by mixed filtrate water
Bath is warming up to 75 DEG C, and precipitating reagent weak aqua ammonia is added dropwise, and after measuring pH=10, stops being added dropwise, continues water-bath 1h, filtering, gained
Filter residue is placed in baking oven dry 2h, and drying temperature is 120 DEG C, finally takes out and grinds to obtain the final product.
Further, the dispersing agent is sodium polycarboxylate dipersant；The levelling agent is hyperbranched type organosilicon levelling
Agent；The defoaming agent is Siloxane-Oxyalkylene Copolymers defoaming agent.
A kind of preparation method of aluminum paste fluorocarbon coating, comprising the following steps:
Step 1: the addition of 8 parts of deionized waters is fed intake in kettle, sequentially add water aluminum-silver slurry, opal shale micro mist,
Titanate esters modified graphene, silane coupling agent, after mixing evenly, ultrasonic treatment obtains aluminum paste pre-dispersed liquid；
Step 2: remaining 15 parts of deionized waters are added into blend tank, water-based fluorocarbon resin, polyurethane tree is then added
Rouge, ethylene glycol, opal shale micro mist load TiO2, after mixing evenly, aluminum paste pre-dispersed liquid obtained by step 1 is added and is adjusted
In distribution tank, continue to stir, add dispersing agent, levelling agent, defoaming agent and pH adjusting agent, continues to stir, obtain seasoning liquid；
Step 3: seasoning liquid after mixing evenly is crossed 200 meshes to get aluminum paste fluorocarbon coating.
Further, the power being ultrasonically treated in step 1 is 200W, time 50min.
Embodiment 4
A kind of aluminum paste fluorocarbon coating, including following component based on parts by weight: 35 parts of water-based fluorocarbon resin, polyurethane
24 parts of resin, 1 part of titanate esters modified graphene, 1 part of silane coupling agent, 23 parts of water aluminum-silver slurry, 3 parts of opal shale micro mist,
Opal shale micro mist loads TiO25 parts, 9 parts of ethylene glycol, 1.5 parts of dispersing agent, 1.5 parts of levelling agent, 1.5 parts of defoaming agent, pH tune
0.6 part of agent, 28 parts of deionized water of section.
Further, the titanate esters modified graphene the preparation method comprises the following steps: graphite oxide is placed in reactor, ultrasound
Processing after graphite to be oxidized is completely dispersed, adjusts pH to 9-10,80 DEG C of constant temperature, hydrazine hydrate and titanate esters coupling is then added
Agent TM-200S reacts 8h, filters, wash while hot repeatedly, until filtrate is in neutrality to get titanate esters modified graphene.
Further, graphene oxide and titanate coupling agent TM-200S in the preparation method of titanate esters modified graphene
Mass ratio be 1:7.
Further, the water aluminum-silver slurry is double-coating aluminum paste, preparation method are as follows: by coated with silica aluminium
Silver paste disperses in ethanol, to sequentially add methyl methacrylate monomer, Butyl Acrylate Monomer, Hexafluorobutyl mathacrylate
Then monomer and acrylic monomers are added initiator azodiisobutyronitrile, stir evenly at room temperature, be warming up to 70 DEG C, constant temperature is anti-
5h is answered, the aluminum paste to get fluorinated acrylate and silica double-coating is filtered.
Further, the partial size of the opal shale micro mist is 10-20 μm.
Further, the opal shale micro mist loads TiO2The preparation method comprises the following steps: (1) opal shale micro mist in horse
3h is not calcined in furnace under the conditions of 300 DEG C, it is 15% phosphoric acid that calcined opal shale micro mist, which is then immersed in mass concentration,
In solution for 24 hours, it filters and washs to neutral spare；(2) titanyl sulfate is added in distilled water, heating stirring, until completely molten
It is filtered after solution, takes filtrate, opal shale micro mist made from step (1) is added in filtrate；(3) by mixed filtrate water
Bath is warming up to 75 DEG C, and precipitating reagent weak aqua ammonia is added dropwise, and after measuring pH=10, stops being added dropwise, continues water-bath 1h, filtering, gained
Filter residue is placed in baking oven dry 2h, and drying temperature is 120 DEG C, finally takes out and grinds to obtain the final product.
Further, the dispersing agent is sodium polycarboxylate dipersant；The levelling agent is hyperbranched type organosilicon levelling
Agent；The defoaming agent is Siloxane-Oxyalkylene Copolymers defoaming agent.
A kind of preparation method of aluminum paste fluorocarbon coating, comprising the following steps:
Step 1: 10 parts of deionized water additions are fed intake in kettle, it is micro- to sequentially add water aluminum-silver slurry, opal shale
Powder, titanate esters modified graphene, silane coupling agent, after mixing evenly, ultrasonic treatment obtains aluminum paste pre-dispersed liquid；
Step 2: remaining 18 parts of deionized waters are added into blend tank, water-based fluorocarbon resin, polyurethane tree is then added
Rouge, ethylene glycol, opal shale micro mist load TiO2, after mixing evenly, aluminum paste pre-dispersed liquid obtained by step 1 is added and is adjusted
In distribution tank, continue to stir, add dispersing agent, levelling agent, defoaming agent and pH adjusting agent, continues to stir, obtain seasoning liquid；
Step 3: seasoning liquid after mixing evenly is crossed 200 meshes to get aluminum paste fluorocarbon coating.
Further, the power being ultrasonically treated in step 1 is 200W, time 60min.
Comparative example 1
In addition to titanate esters modified graphene replaces with graphene oxide, remaining is the same as embodiment 3.
Comparative example 2
In addition to water aluminum-silver slurry replaces with coated with silica aluminum paste, remaining operation is the same as embodiment 3.
Comparative example 3
Except the aluminum paste of water aluminum-silver slurry, that is, fluorinated acrylate and silica double-coating replace with acrylate and
Outside coated with silica aluminum paste, remaining operation is the same as embodiment 3.
Comparative example 4
Without opal shale micro mist, opal shale micro mist is loaded into TiO2It replaces with and loaded TiO2Etc. quality
TiO2Nanoparticle, remaining operation is the same as embodiment 3.
Comparative example 5
Removing protein stone shale micro mist replaces with outside the opal shale without activation processing, remaining operation is the same as embodiment 3.
Comparative example 6
In addition to without polyethylene glycol, remaining operation is the same as embodiment 3.
Comparative example 7
It does not carry out the pre-dispersed component i.e. in addition to auxiliary agent of aluminum paste to be added in blend tank together, remaining operates same embodiment
3。
Performance test
The tinplate ground for choosing same treatment carries out embodiment 1-4 and comparative example 1-7 products obtained therefrom in surface of bottom material
Brush construction, brush with a thickness of 30 μm spray standing or it is 5-10 minute air-dried, later spontaneously dry be obtain aluminum paste fluorine carbon apply
Layer, it does solid work 24 hours, is completely dried 7 days under room temperature.
Acid resistance test: coating is in 0.05mol/L H2SO4It is impregnated 1 day in solution；
Alkali resistance test: coating impregnates 1 day in 0.1mol/L NaOH solution；
And other performance tests are carried out to coating according to relevant criterion, the results are shown in Table 1.
1~6 coating sample the performance test results of 1 Examples 1 to 4 of table and comparative example
By test result in table 1 it is found that aluminum paste fluorocarbon coating provided by the invention, VOC burst size is low, there is bloom
Pool, high-dirt-resistance, mechanical property is good, and water resistance and acid-alkali-corrosive-resisting are strong, and ageing-resistant performance is excellent.Comparative example 1 is by titanate esters
Modified graphene replaces with graphene oxide, and graphene oxide and resin matrix do not have coupled action, is firmly combined degree decrease,
The mechanical strength of coating reduces, and aligning for aluminum paste is also impacted, and glossiness, hardness, the wearability of coating decline, resistance to
Acid-base property is also not as good as embodiment 3；Water aluminum-silver slurry is replaced with coated with silica aluminum paste by comparative example 2, coating abrasion performance, resistance to
Acid-base property and resistance to ag(e)ing are decreased significantly, and gloss and impact resistance also slightly reduce, and show fluorine-containing the third of aluminum paste outer layer
The effect of olefin(e) acid ester can play wear-resisting, isolation soda acid, and aluminum paste gloss is protected not reduce.3 fluorinated acrylate of comparative example and
The aluminum paste of silica double-coating replaces with acrylate and coated with silica aluminum paste, and the gloss of coating slightly drops
The advantages of low, resistance to ag(e)ing is also remarkably decreased, and film forming is fine and close this is because fluorinated acrylate has, good weatherability, can be right
Aluminum paste plays preferable protective effect, and acrylate film forming, not as good as fluorinated acrylate, aluminum paste is in preparation and coating
Oxygen and water may be contacted in the process, therefore glossiness is not as good as embodiment, and the resistance to ag(e)ing of its own is compared with fluorinated acrylate
Difference causes ageing-resistant performance to reduce.Comparative example 4 is free of opal shale micro mist, and VOC burst size is embodiment more than twice,
TiO2It is directly added using unsupported mode, gloss, hardness, the adhesive force of coating are remarkably decreased, and anti-impact force and fracture are stretched
Long rate also declines to a great extent, and water resistance and resistance to acid and alkali are deteriorated, and foaming phenomena occurs in resistance to ag(e)ing test, there is a crackle, discoloration and
Loss of gloss shows that opal shale is the key component for guaranteeing coating comprehensive performance, and chemical adsorption substantially reduces coating
VOC, moreover it is possible to it is cooperateed with titanate esters modified graphene, makes coating impact strength with higher, tensile strength, tearing strength, it can
Optimize the water resistance and corrosion resistance of coating, the porous structure having can alleviate coating stress, prevent the generation of crackle, non-
The TiO that mode of loading is added2Antiultraviolet ageing properties are much not as good as the TiO of opal shale load2.Comparative example 5 using without
The opal shale of activation processing, the specific surface area of opal shale greatly reduces compared with activated, to pernicious gas
The rate of adsorption and capacity are also not as good as activated opal shale, thus the VOC burst size of 5 coating of comparative example is significantly larger than implemented
Example 3, opposite with the binding site of titanate esters modified graphene, coating resin matrix to reduce, the TiO loaded2Amount decline, so that
4 properties of comparative example are not as good as embodiment.Comparative example 6 is free of polyethylene glycol, and aluminum paste pre-dispersed liquid mobility weakens, coating light
Damp obviously not as good as embodiment 3, coating dispersing uniformity in preparation and storage process declines, hardness, adhesive force, water resistance and resistance to
Acid-base property is remarkably decreased, and occurs blistering, peeling and loss of gloss phenomenon in anti-aging test, this may be due to polyethylene glycol and albumen
There is collaboration between stone shale and promote aluminum paste the effect of aligning, can enhance between coating composition in dope preparing process
Structuring ability.The glossiness of 7 coating of comparative example declines, and wearability also declines to a great extent, and resistance to acid and alkali is deteriorated, in anti-aging test
There is blistering, crackle, discoloration, loss of gloss phenomenon, this is because not carrying out pre-dispersed, aluminum paste and opal shale micro mist, silane
Binding force between coupling agent, titanate esters modified graphene is weaker, is formed by that network structure continuity is poor, and synergistic effect subtracts
It is weak, thus there is a series of performance decline.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, ability
Other modifications or equivalent replacement that domain those of ordinary skill makes technical solution of the present invention, without departing from skill of the present invention
The spirit and scope of art scheme, are intended to be within the scope of the claims of the invention.
Claims (9)
1. a kind of aluminum paste fluorocarbon coating, which is characterized in that including following component based on parts by weight: water-based fluorocarbon resin
18-35 parts, 13-24 parts of polyurethane resin, 0.5-1 parts of titanate esters modified graphene, 0.2-1 parts of silane coupling agent, aqueous aluminium silver
6-23 parts of slurry, 1-3 parts of opal shale micro mist, opal shale micro mist load TiO22-5 parts, 5-9 parts of ethylene glycol, dispersing agent
0.1-1.5 parts, 0.1-1.5 parts of levelling agent, 0.3-1.5 parts of defoaming agent, 0.1-0.6 parts of pH adjusting agent, 15-28 parts of deionized water.
2. aluminum paste fluorocarbon coating according to claim 1, which is characterized in that the preparation of the titanate esters modified graphene
Method are as follows: graphite oxide is placed in reactor, is ultrasonically treated, after graphite to be oxidized is completely dispersed, adjusts pH to 9-10, constant temperature
80 DEG C, hydrazine hydrate and titanate coupling agent TM-200S is then added, reacts 8 h, filters, wash repeatedly while hot, until filter
Liquid is in neutrality to get titanate esters modified graphene.
3. aluminum paste fluorocarbon coating according to claim 2, which is characterized in that the preparation method of titanate esters modified graphene
The mass ratio of middle graphene oxide and titanate coupling agent TM-200S are 1:7.
4. aluminum paste fluorocarbon coating according to claim 1, which is characterized in that the water aluminum-silver slurry is double-coating aluminium
Silver paste, preparation method are as follows: in ethanol by the dispersion of coated with silica aluminum paste, sequentially add methyl methacrylate list
Then two isobutyl of initiator azo is added in body, Butyl Acrylate Monomer, Hexafluorobutyl mathacrylate monomer and acrylic monomers
Nitrile stirs evenly at room temperature, is warming up to 70 DEG C, 5 h of isothermal reaction, filters double-deck to get fluorinated acrylate and silica
The aluminum paste of cladding.
5. aluminum paste fluorocarbon coating according to claim 1, which is characterized in that the partial size of the opal shale micro mist is
10-20 μm。
6. aluminum paste fluorocarbon coating according to claim 1, which is characterized in that the opal shale micro mist loads TiO2
The preparation method comprises the following steps: (1) opal shale micro mist calcines 3 h in Muffle furnace under the conditions of 300 DEG C, then by calcined egg
It is 24 h in 15% phosphoric acid solution that white stone shale micro mist, which is immersed in mass concentration, filters and washs to neutral spare；(2) by sulfuric acid
Oxygen titanium is added in distilled water, and heating stirring filters after being completely dissolved, and filtrate is taken, by opal shale made from step (1)
Micro mist is added in filtrate；(3) mixed filtrate water-bath is warming up to 75 DEG C, precipitating reagent weak aqua ammonia is added dropwise, measure pH=10
Afterwards, stopping being added dropwise, continue 1 h of water-bath, filtering, gained filter residue is placed in baking oven dry 2 h, and drying temperature is 120 DEG C,
It finally takes out and grinds to obtain the final product.
7. aluminum paste fluorocarbon coating according to claim 1, which is characterized in that the dispersing agent is polycarboxylate sodium's dispersion
Agent；The levelling agent is hyperbranched type organosilicon levelling agent；The defoaming agent is Siloxane-Oxyalkylene Copolymers defoaming agent.
8. a kind of preparation method of any one of according to claim 1 ~ 7 aluminum paste fluorocarbon coating, which is characterized in that including with
Lower step:
Step 1: portions of de-ionized water addition is fed intake in kettle, water aluminum-silver slurry, opal shale micro mist, titanium are sequentially added
Acid esters modified graphene, silane coupling agent, after mixing evenly, ultrasonic treatment obtains aluminum paste pre-dispersed liquid；
Step 2: remaining number deionized water is added into blend tank, water-based fluorocarbon resin, polyurethane resin, second is then added
Glycol, opal shale micro mist load TiO2, after mixing evenly, blend tank is added in aluminum paste pre-dispersed liquid obtained by step 1
In, continue to stir, add dispersing agent, levelling agent, defoaming agent and pH adjusting agent, continues to stir, obtain seasoning liquid；
Step 3: seasoning liquid after mixing evenly is crossed 200 meshes to get aluminum paste fluorocarbon coating.
9. the preparation method of aluminum paste fluorocarbon coating according to claim 8, which is characterized in that be ultrasonically treated in step 1
Power is 200 W, and the time is 40 ~ 60min.
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