CN109554072A - A kind of water-based anticorrosive paint preparation method - Google Patents
A kind of water-based anticorrosive paint preparation method Download PDFInfo
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- CN109554072A CN109554072A CN201811396508.2A CN201811396508A CN109554072A CN 109554072 A CN109554072 A CN 109554072A CN 201811396508 A CN201811396508 A CN 201811396508A CN 109554072 A CN109554072 A CN 109554072A
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
-
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention relates to a kind of water-based anticorrosive paint preparation methods, step are as follows: prepare distributed graphene first, again by epoxy resin, curing agent, dibutyl ester, nano-titanium dioxide, trbasic zinc phosphate and the distributed graphene ratio of 80-100:5-8:1-3:7-9:8-11:1-6 in mass ratio are blended, and water-based anticorrosive paint is prepared.The distributed graphene that the present invention uses has good photoelectric properties, it is modified to have passed through the surfaces such as class fluid, graphene can have better compatibility with polymer, improve the filming performance of water-based anticorrosive paint, and graphene can make coating conductive, play the role of antisepsis simultaneously, nano-titanium dioxide can play disinfection and shielding ultraviolet rays.
Description
Technical field
The present invention relates to preparation method for coating, and in particular to a kind of water-based anticorrosive paint preparation method.
Background technique
Practical application shows that aqueous industrial anticorrosive coating can in extreme conditions be effectively protected steel offer.
Since water is primary solvent, water can also be used to clean and dilute water paint, they almost without solvent taste, meanwhile, make
Lower cost can also be brought to user with water paint, if quick-drying can save the time, low flame properties can reduce insurance premium,
Less room ventilation can reduce energy consumption, and not need the cost on solvent and cleaning agent, mating using signal layer coating, can
To save the expense etc. of downtime and erecting scaffold.
The shortcomings that the characteristics of due to water itself, water-base resin first is that moisture evaporation is slow in low temperature and high relative humidity.
Since the surface tension of water is high, it also must be introduced into some auxiliary agents in formula and moistened to improve paint film to pigment and base-material
Property.These auxiliary agents have negative impact to the water resistance and permeability of paint film, in addition compared with solvent based coating, water paint
Influence of the filming performance to coating property is most important.
Summary of the invention
The technical problems to be solved by the invention provide a kind of water-based anticorrosive paint preparation method of good film-forming property.
The technical scheme to solve the above technical problems is that
A kind of water-based anticorrosive paint preparation method, comprising the following steps:
Step 1 prepares distributed graphene;
Epoxy resin, curing agent, dibutyl ester, nano-titanium dioxide, trbasic zinc phosphate and distributed graphene are pressed matter by step 2
It measures the ratio than 80-100:5-8:1-3:7-9:8-11:1-6 to be blended, water-based anticorrosive paint is prepared.
Further, the distributed graphene in the step 1 preparation method the following steps are included:
Step 1.11 prepares functional graphene oxide or stannic oxide/graphene nano particle using graphene oxide;
The stannic oxide/graphene nano particle or functional graphene oxide do not dried after washing are dispersed nothing by step 1.12
In water-ethanol, wherein the mass ratio of dehydrated alcohol and the graphene oxide in step 1 is 80-100:40-60, is carried out to mixed liquor
Uniform and stable functional graphene oxide dispersion liquid is obtained after ultrasonic treatment;
Hydrazine hydrate, the oxygen in the hydrazine hydrate and step 1 are added into functional graphene oxide dispersion liquid for step 1.13
The mass ratio of graphite alkene is 1-5:100, and at 50-60 DEG C, the reaction was continued under room temperature for 24 hours, then is washed with anhydrous and deionization
Products therefrom is washed to neutrality;
Step 1.14 will not dry product obtained in the previous step and be mixed into ethanol water, aqueous acetone solution or N, N '-two
It in methylformamide aqueous solution, and is ultrasonically treated, obtains distributed graphene;The ethanol water, aqueous acetone solution
And in N, N '-dimethylformamide in water, the volume ratio of solute and water is 8-10:1.
Further, in the step 1.11, the specific method of graphene oxide preparation functional graphene oxide is utilized
The following steps are included:
Step 1.111a, it takes graphene oxide to be mixed into dehydrated alcohol and forms mixed liquor, wherein graphene oxide and anhydrous second
The mass ratio of alcohol is 80-100:40-60, obtains uniform dispersion after being ultrasonically treated to mixed liquor;
Step 1.112a, HC l is added into uniform dispersion, the pH for adjusting dispersion liquid is 3-4;
Step 1.113a, 95% second containing Silane coupling reagent KH-570 is added in the dispersion liquid after adjusting one step up
The mass ratio of graphene oxide in alcoholic solution, the Silane coupling reagent KH-570 and step 1.111a is 0.1-0.5:100, institute
The mass ratio for stating dehydrated alcohol in 95% ethanol solution and step 1.111a is 1:5-7;
Step 1.113a, mixed liquor obtained in the previous step the reaction was continued under the conditions of 50-60 DEG C of temperature for 24 hours after centrifugation point
From, then wash repeatedly with anhydrous and deionized water, cleaning solution, the removing unreacted KH-570 of cleaning solution are obtained, and adjust washing
Liquid obtains functional graphene oxide to neutrality.
Further, in the step 1.11, the specific side of stannic oxide/graphene nano particle is prepared using graphene oxide
Method the following steps are included:
Step 1.111b, it takes graphene oxide to be mixed into dehydrated alcohol and forms mixed liquor, wherein graphene oxide and anhydrous second
The mass ratio of alcohol is 80-100:40-60, obtains uniform dispersion after being ultrasonically treated to mixed liquor;
Step 1.112b, the DC5700 methanol that mass fraction is 30-50% is added in the dispersion liquid after adjusting one step up
Solution;
Step 1.113b, mixed liquor obtained in the previous step is aged for 24 hours at room temperature, with intermittent oscillation when ageing,
Solvent is removed after ageing to obtain solid, solid is washed with water repeatedly, then is washed repeatedly with ethyl alcohol, is dried in vacuo at 50-70 DEG C
24 hours, obtain the stannic oxide/graphene nano particle of DC5700 grafting.
The invention has the benefit that the distributed graphene that the present invention uses there are good photoelectric properties, class have passed through
The surfaces such as fluid are modified, and graphene can have better compatibility with polymer, improve the filming performance of water-based anticorrosive paint, and
And graphene can make coating conduction, while play antisepsis, nano-titanium dioxide can play disinfection and shielding ultraviolet rays
Effect.
Specific embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
1, the preparation of distributed graphene
A, graphene oxide is prepared using hummers method
Hummers method prepares graphene oxide, and reaction is easy, when length, experiment safety is preferable, very to the pollution of environment
It is low.Therefore, it has become the conventional preparation methods of graphene oxide.
It is 98% to pour into 1000mL flask by the concentration of 300mL, 6g crystalline flake graphite is put into flask and made
It is stirred with ice-water bath;In next step, the ratio for being 1: 3.5 according to graphite and potassium permanganate mass ratio a small amount of, multiple in 20min
21g potassium permanganate is added, solution becomes blackish green at this time.Ice-water bath persistently stirs 15-20min, then unloads ice bath, in room temperature
Lower stirring is for 24 hours.
Reaction continue stirred under the conditions of ice-water bath, 500ml deionized water is added into flask, at this time color appearance by
It is blackish green to become brownish red, and generate bubble;The hydrogen peroxide of 10ml or more is slowly added dropwise again, color becomes bright orange from brownish red
Color.It is filtered in next step with sand core funnel, using 3% hydrochloric acid of 1L and the deionized water of 1L, product is oxidation stone for washing
Black alkene.It after product is freeze-dried, is dispersed in water with the concentration of 1g/L, then be freeze-dried, final product is graphite oxide
Alkene.
By in 100mg graphene oxide 60ml dehydrated alcohol, ultrasound formed uniform dispersion after 1 hour.To dispersion
The middle DC5700 methanol solution (mass fraction 40%) that 10ml is added, and be aged 24 hours at room temperature, with intermittent oscillation.It will
Solvent removes, and solid is washed with water 3 times, then is washed twice with ethyl alcohol, is dried in vacuo 24 hours at 60 DEG C, obtains DC5700 grafting
Stannic oxide/graphene nano particle.
B, take 100mg graphene oxide in 60ml dehydrated alcohol, ultrasound formed uniform dispersion after 1 hour, added
A certain amount of HCl, adjusts dispersion liquid pH=3-4, and 95% ethyl alcohol that 10ml is then contained 0.3gKH-570 is slow under stiring
It is added, at 60 DEG C, the reaction was continued for 24 hours, centrifuge separation, then is washed repeatedly with anhydrous and deionized water, completely removes unreacted
KH-570, and make cleaning solution to neutrality, obtaining product is functional graphene oxide.
C, to disperse 60ml for the stannic oxide/graphene nano particle or functional graphene oxide do not dried after washing anhydrous
Ultrasound formed uniform and stable functional graphene oxide dispersion liquid after 1 hour in ethyl alcohol, 1g hydrazine hydrate was then added, in 60
Reductase 12 4 hours at DEG C, then products therefrom is washed to neutrality with dehydrated alcohol and deionized water, the product that do not dry is surpassed respectively
It is the ethanol/water of 9:1 (V/V), acetone/water, in n,N-Dimethylformamide/water mixed solution that sound, which is scattered in volume ratio, most
Distributed graphene is obtained eventually.
2, nano-TiO2The preparation of powder
At room temperature, 10ml tetrabutyl titanate is measured, is slowly dropped into 35 milliliters of dehydrated alcohols, uses magnetic agitation
Device strong stirring 10min is uniformly mixed, and forms yellow clear solution A.4 milliliters of glacial acetic acid and 10 milliliters of distilled water are added to separately
It in 35 milliliters of dehydrated alcohols, is vigorously stirred, obtains solution B, instill 1-2 milliliters of hydrochloric acid, adjusting pH value makes pH≤3.
Under room-temperature water bath, with vigorous stirring, the solution A having been moved into constant pressure funnel is slowly dropped into solution B, is added dropwise
Speed is about 3mlmin-1.Pale yellow solution is obtained after being added dropwise, and is continued after stirring half an hour, 40 DEG C of heating water baths, 2
White gels are obtained after hour, is placed at 80 DEG C and dries, about 20 hours, obtain yellow crystals, grinds, obtains pale yellow powder.
It is heat-treated 2 hours for (300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C) at different temperature, obtains different titania powders.
3, by 80 grams of epoxy resin E-44,5 grams of curing agent, 2 grams of dibutyl ester, nano-TiO28 grams, 10 grams of trbasic zinc phosphate, point
It dissipates 1-6 grams of type graphene to be blended, water-based anticorrosive paint is prepared.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of water-based anticorrosive paint preparation method, which comprises the following steps:
Step 1 prepares distributed graphene;
Step 2, by epoxy resin, curing agent, dibutyl ester, nano-titanium dioxide, trbasic zinc phosphate and distributed graphene are in mass ratio
The ratio of 80-100:5-8:1-3:7-9:8-11:1-6 is blended, and water-based anticorrosive paint is prepared.
2. water-based anticorrosive paint preparation method according to claim 1, which is characterized in that the dispersion in the step 1
The preparation method of type graphene the following steps are included:
Step 1.11 prepares functional graphene oxide or stannic oxide/graphene nano particle using graphene oxide;
The stannic oxide/graphene nano particle or functional graphene oxide do not dried after washing are dispersed anhydrous second by step 1.12
In alcohol, wherein the mass ratio of dehydrated alcohol and the graphene oxide in step 1 is 80-100:40-60, carries out ultrasound to mixed liquor
Uniform and stable functional graphene oxide dispersion liquid is obtained after processing;
Hydrazine hydrate, the oxidation stone in the hydrazine hydrate and step 1 are added into functional graphene oxide dispersion liquid for step 1.13
The mass ratio of black alkene is 1-5:100, and at 50-60 DEG C, the reaction was continued under room temperature for 24 hours, then washs institute with anhydrous and deionized water
Product is obtained to neutrality;
Step 1.14 will not dry product obtained in the previous step and be mixed into ethanol water, aqueous acetone solution or N, N '-dimethyl
It in formyl amine aqueous solution, and is ultrasonically treated, obtains distributed graphene;The ethanol water, aqueous acetone solution and N,
In N '-dimethylformamide in water, the volume ratio of solute and water is 8-10:1.
3. water-based anticorrosive paint preparation method according to claim 2, which is characterized in that in the step 1.11, utilize
Graphene oxide prepare functional graphene oxide specific method the following steps are included:
Step 1.111a, it takes graphene oxide to be mixed into dehydrated alcohol and forms mixed liquor, wherein graphene oxide and dehydrated alcohol
Mass ratio is 80-100:40-60, obtains uniform dispersion after being ultrasonically treated to mixed liquor;
Step 1.112a, HC l is added into uniform dispersion, the pH for adjusting dispersion liquid is 3-4;
Step 1.113a, it is molten that 95% ethyl alcohol containing Silane coupling reagent KH-570 is added in the dispersion liquid after adjusting one step up
The mass ratio of graphene oxide in liquid, the Silane coupling reagent KH-570 and step 1.111a is 0.1-0.5:100, described
The mass ratio of dehydrated alcohol is 1:5-7 in 95% ethanol solution and step 1.111a;
Step 1.113a, mixed liquor obtained in the previous step is centrifugated after the reaction was continued under the conditions of 50-60 DEG C of temperature for 24 hours,
Wash repeatedly with anhydrous and deionized water again, obtains cleaning solution, the removing unreacted KH-570 of cleaning solution, and adjust cleaning solution to
Neutrality obtains functional graphene oxide.
4. water-based anticorrosive paint preparation method according to claim 2, which is characterized in that in the step 1.11, utilize
Graphene oxide prepare the specific method of stannic oxide/graphene nano particle the following steps are included:
Step 1.111b, it takes graphene oxide to be mixed into dehydrated alcohol and forms mixed liquor, wherein graphene oxide and dehydrated alcohol
Mass ratio is 80-100:40-60, obtains uniform dispersion after being ultrasonically treated to mixed liquor;
Step 1.112b, the DC5700 methanol solution that mass fraction is 30-50% is added in the dispersion liquid after adjusting one step up;
Step 1.113b, mixed liquor obtained in the previous step is aged for 24 hours at room temperature, with intermittent oscillation, ageing when ageing
Solvent is removed afterwards to obtain solid, solid is washed with water repeatedly, then is washed repeatedly with ethyl alcohol, it is small that 24 are dried in vacuo at 50-70 DEG C
When, obtain the stannic oxide/graphene nano particle of DC5700 grafting.
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Cited By (2)
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GB2583503A (en) * | 2019-04-30 | 2020-11-04 | !Obac Ltd | Heated floor or wall coating system |
CN112239625A (en) * | 2020-09-25 | 2021-01-19 | 上海大学 | Silicon dioxide-graphene oxide/polyurethane acrylic resin anticorrosion coating |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB2583503A (en) * | 2019-04-30 | 2020-11-04 | !Obac Ltd | Heated floor or wall coating system |
CN112239625A (en) * | 2020-09-25 | 2021-01-19 | 上海大学 | Silicon dioxide-graphene oxide/polyurethane acrylic resin anticorrosion coating |
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Application publication date: 20190402 |