CN107903755A - A kind of preparation method of graphene oxide modified aqueous acrylic acid anticorrosive paint - Google Patents
A kind of preparation method of graphene oxide modified aqueous acrylic acid anticorrosive paint Download PDFInfo
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- CN107903755A CN107903755A CN201711430964.XA CN201711430964A CN107903755A CN 107903755 A CN107903755 A CN 107903755A CN 201711430964 A CN201711430964 A CN 201711430964A CN 107903755 A CN107903755 A CN 107903755A
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- graphene oxide
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- anticorrosive paint
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- acrylic acid
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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
- C09D133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
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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
Abstract
A kind of preparation method of graphene oxide modified aqueous acrylic acid anticorrosive paint, it is related to anticorrosive paint preparation field, by N, N dimethylformamides, graphene oxide, catalyst and glycidyl neodecanoate mixing, reacted under the conditions of 120~150 DEG C, then centrifuged after reaction mass is cooled down again, obtain solid phase vacuum drying, obtain modified graphene oxide；After modified graphene oxide, coalescents, hydroxyl acrylic emulsion and defoamer are ground in three-roll grinder, 325 amino resins of U.S. cyanogen spy Cymel is added, then is ground, obtains graphene oxide modified aqueous acrylic acid anticorrosive paint.The present invention reduces the Van der Waals force between graphene oxide layer by modifying surface of graphene oxide, and introduces long alkyl chain, thus improve graphene oxide dispersion stabilization and coating to the screening abilities of eroded elements.
Description
Technical field
The present invention relates to anticorrosive paint preparation field, and in particular to a kind of graphene oxide modified aqueous acrylic acid anti-corrosion applies
The preparation method of material.
Background technology
Just greatly paid close attention to since grapheme material self-discovery, in fields such as the energy, electronics, sensor, catalysis
Through obtaining significant achievement.Graphene is chemically inert material, and physics barrier layer can be formed between metal and medium, hinders oxygen
Contact of the gas with metal, effectively prevents corrosion of the metal in solution and air.Graphene is applied to anticorrosive paint, it is higher
Intensity and hardness, good electric conductivity and sheet overlap joint performance so that graphene anticorrosive paint is compared with other anticorrosive paints
There is obvious advantage in salt fog resistance, electric conductivity, mechanical performance, suitable for oil and gas transmission, petrochemical industry, bridge work
The severe corrosive environment such as journey and shipbuilding industry, is a kind of ideal new anti-corrosion coating.
Water-borne acrylic coatings have the advantages that quality of forming film is high, and preparation process is simple, are widely used in each metalloid and prevent
Rotten finishing coat and middle paint.But the property of graphene uniqueness, is not easy dispersed in aqueous systems or acrylic resin systems, it is difficult to logical
Cross physical blending or home position polymerization reaction grafted in acrylic resin strand, cause graphene be difficult to play its physics every
Disconnected effect, or even holiday is formed, the further genralrlization application to graphene causes great difficulty.
The content of the invention
The invention aims to overcome the deficiencies of the prior art and provide a kind of graphene oxide modified aqueous acrylic acid to prevent
The preparation method of rotten coating.
The present invention includes the following steps：
1）N,N-Dimethylformamide, graphene oxide, catalyst and glycidyl neodecanoate are mixed, at 120~150 DEG C
Under the conditions of react, centrifuged after then reaction mass is cooled down again, obtain solid phase vacuum drying, obtain modified graphene oxide；
2）The modified graphene oxide, coalescents, hydroxyl acrylic emulsion and defoamer are ground in three-roll grinder
Afterwards, 325 amino resins of U.S. cyanogen spy Cymel is added, then is ground, obtains graphene oxide modified aqueous acrylic acid anticorrosive paint.
The present invention is by modifying surface of graphene oxide, the Van der Waals force between reduction graphene oxide layer,
And introduce long alkyl chain so that improve graphene oxide dispersion stabilization and coating to the screening abilities of eroded elements.
Advantageous effect of the invention：
1st, the nonpolar graphene of tradition is replaced to improve its point in water phase as modified material using hydrophilic graphene oxide
The ability of dissipating.
2nd, using glycidyl neodecanoate as coating material, the active epoxy functional group in its structure is in catalyst
Effect is lower to be bonded with the carboxyl of surface of graphene oxide, hydroxyl open loop.Being introduced in surface of graphene oxide has ten carbon atoms
Alkyl chain, formed physics cushion, prevent graphene oxide from reuniting in dispersion process.
3rd, the graphene oxide after modifying utilizes the activity hydroxy on its surface, can effectively be scattered in aqueous acrylic emulsion
In, and reaction is crosslinked with amino resins when forming a film curing, form equally distributed composite coating.
Further, step 1 of the present invention）Middle N,N-dimethylformamide, graphene oxide, catalyst and neodecanoic acid
The mass ratio that feeds intake of ethylene oxidic ester is 100: 20~60: 1~3: 2~5.Graphene oxide is fully dispersed in N, N- dimethyl
Formamide, can improve the reaction efficiency of graphene oxide and glycidyl neodecanoate.The activity hydroxy of surface of graphene oxide,
Carboxyl functional group need not be reacted with glycidyl neodecanoate completely, it is only necessary to form the position of Long carbon chain in surface of graphene oxide
Hinder structure.On the one hand glycidyl neodecanoate dosage, the remaining hydroxyl of another aspect graphene surface and carboxyl-functional are reduced
Group may participate in the condensation reaction of base polyurethane prepolymer for use as.
The step 1）Middle catalyst is any one in triethylamine, N- methylimidazoles, triphenylphosphine.Three can make
For the catalyst of epoxy addition, the grafting efficiency of glycidyl neodecanoate is improved.
The step 1）In be cooled to 30 DEG C after centrifuge.Dispersion liquid of the graphene oxide in N,N-dimethylformamide is high
Temperature is lower to be presented muddy, and Brownian movement is very fast, is unfavorable for centrifuging.
The step 1）Described in vacuum drying temperature be 80 DEG C, pressure≤20Pa.The boiling of N,N-dimethylformamide
Higher, the slow drying speed of point, energy consumption is larger, is dried under reduced pressure the rate of drying that can significantly improve material.
The step 2）Described in modified graphene oxide, coalescents, hydroxyl acrylic emulsion, defoamer and U.S.'s cyanogen
The mass ratio that feeds intake of special 325 amino resins of Cymel is 0.1~0.5: 2~5: 80~100: 0.1~0.5: 1~5.It is modified oxidized
Graphene is dispersed in hydroxyl acrylic emulsion under the auxiliary of coalescents, with 325 amino trees of U.S. cyanogen spy Cymel
Fat high temperature is cured the corrosion-inhibiting coating that cross-linking reaction forms even compact.
The step 2）Described in coalescents be Lauryl Alcohol ester, propylene glycol monomethyl ether, one kind in butyl glycol ether.Three
Kind coalescents all contain hydrophily ester bond or ehter bond, can be wrapped in modified graphene oxide surface, improve in aqueous systems
Dispersiveness.
The step 2）Described in hydroxyl acrylic emulsion, hydroxyl value is 50~100mg KOH/g.Hydroxyl value crosses low cross-linking
Degree deficiency, the excessive resin viscosity of hydroxyl value is excessive, is not easy to form a film.
The step 2）Described in defoamer be BYK 028, the peaceful FoamStar ST 2410AC or TEGO of BASF section
One kind in foamex1488.Three kinds of defoamers can be adapted for high gloss finishing coat, have outstanding defoaming and brokenly bubble
Performance, while be not easy to form flake or shrinkage cavity in coating surface, ensure coutinuity of coating and integrality.
Embodiment
Technical scheme is further described with reference to embodiments.
Graphene oxide is purchased from Suzhou Tan Feng graphenes Science and Technology Ltd., 0.5~5 micron of lamella size, thickness 0.6
~1.0 nanometers.Hydroxyl acrylic emulsion is purchased from Ahmedabad richness company.
Embodiment 1
100 mass parts N,N-dimethylformamides, 20 mass parts graphene oxides, 1 mass parts three are sequentially added in the reactor
Ethamine, 2 mass parts glycidyl neodecanoates, when 130 DEG C of reactions 4 are small, are cooled to 30 DEG C by reaction mass, centrifuge, from
Heart filter cake is placed in 80 DEG C of vacuum desiccators, controls absolute pressure≤20Pa, and drying 4 obtains modified graphene oxide when small.
Modified graphene oxide, 2 mass parts propylene glycol monomethyl ethers, the 90 mass parts hydroxyl values that 0.3 mass parts step 1 is obtained
For 50mg KOH/g hydroxyl acrylic emulsions, 0.4 mass parts BYK 028, when being collectively disposed at that grinding 5 is small in three-roll grinder, add
Enter 2 mass parts U.S. cyanogen spy Cymel, 325 amino resins, continue grinding and obtain graphene oxide modified aqueous acrylic acid in 10 minutes
Anticorrosive paint.
Comparative example 1
It is 50mg KOH/g hydroxyl acrylic emulsions by 2 mass parts propylene glycol monomethyl ethers, 90 mass parts hydroxyl values, 0.4 mass parts BYK
028, be collectively disposed in three-roll grinder grinding 5 it is small when, add 2 mass parts U.S. cyanogen spy Cymel, 325 amino resins, continue to grind
Mill obtains graphene oxide modified aqueous acrylic acid anticorrosive paint in 10 minutes.
Comparative example 2
It is 50mg by the commercially available unmodified graphene oxide of 0.3 mass parts, 2 mass parts propylene glycol monomethyl ethers, 90 mass parts hydroxyl values
KOH/g hydroxyl acrylic emulsions, 0.4 mass parts BYK 028, be collectively disposed in three-roll grinder grinding 5 it is small when, add 2 mass
Part 325 amino resins of U.S. cyanogen spy Cymel, continues grinding and obtains within 10 minutes the painting of graphene oxide modified aqueous acrylic acid anti-corrosion
Material.
Embodiment 2
100 mass parts N,N-dimethylformamides, 40 mass parts graphene oxides, 2 mass parts N- are sequentially added in the reactor
Methylimidazole, 4 mass parts glycidyl neodecanoates, when 120 DEG C of reactions 5 are small, are cooled to 30 DEG C, centrifugation point by reaction mass
From centrifugal filter cake is placed in 80 DEG C of vacuum desiccators, controls absolute pressure≤20Pa, and drying 4 obtains modified graphite oxide when small
Alkene.
Modified graphene oxide, 3 mass parts butyl glycol ethers, the 80 mass parts hydroxyl values that 0.1 mass parts step 1 is obtained
For 100mg KOH/g hydroxyl acrylic emulsions, the 0.3 peaceful FoamStar ST 2410AC of mass parts BASF section, three are collectively disposed at
When grinding 5 is small in roller mill, 1 mass parts U.S. cyanogen spy Cymel, 325 amino resins is added, continues grinding and obtains oxygen in 10 minutes
Graphite alkene modified aqueous acrylic acid anticorrosive paint.
Embodiment 3
100 mass parts N,N-dimethylformamides, 60 mass parts graphene oxides, 3 mass parts three are sequentially added in the reactor
Phenylphosphine, 3 mass parts glycidyl neodecanoates, when 150 DEG C of reactions 3 are small, are cooled to 30 DEG C by reaction mass, centrifuge,
Centrifugal filter cake is placed in 80 DEG C of vacuum desiccators, controls absolute pressure≤20Pa, and drying 4 obtains modified graphene oxide when small；
Modified graphene oxide, 5 mass parts Lauryl Alcohol esters, the 100 mass parts hydroxyl values that 0.4 mass parts step 1 is obtained are
90mg KOH/g hydroxyl acrylic emulsions, 0.1 mass parts TEGO foamex1488, it is small to be collectively disposed at grinding 5 in three-roll grinder
When, 5 mass parts U.S. cyanogen spy Cymel, 325 amino resins is added, continues grinding and obtains graphene oxide modified water-soluble in 10 minutes
Acrylic Anticorrosive Coatings.
Embodiment 4
100 mass parts N,N-dimethylformamides, 30 mass parts graphene oxides, 2 mass parts N- are sequentially added in the reactor
Methylimidazole, 5 mass parts glycidyl neodecanoates, when 140 DEG C of reactions 4 are small, are cooled to 30 DEG C, centrifugation point by reaction mass
From centrifugal filter cake is placed in 80 DEG C of vacuum desiccators, controls absolute pressure≤20Pa, and drying 4 obtains modified graphite oxide when small
Alkene.
Modified graphene oxide, 4 mass parts propylene glycol monomethyl ethers, the 90 mass parts hydroxyl values that 0.5 mass parts step 1 is obtained
For 80mg KOH/g hydroxyl acrylic emulsions, 0.5 mass parts BYK 028, when being collectively disposed at that grinding 5 is small in three-roll grinder, add
Enter 3 mass parts U.S. cyanogen spy Cymel, 325 amino resins, continue grinding and obtain graphene oxide modified aqueous acrylic acid in 10 minutes
Anticorrosive paint.
By coating even application prepared by above-described embodiment in being surface-treated according to GB/T 9271-2008 standards
Tinplate test plate (panel), when drying at room temperature 24 is small, 140 DEG C are toasted 30 minutes, and thickness of dry film controls 30-50 microns, progressive after edge sealing
It can test, test result is shown in Table 1.
1 sample tests of table
As seen from the above table：Acid coated compared to the aqueous acrylamide for being not added with graphene oxide, modified graphene oxide significantly improves
The wet adhesion of water soluble acrylic acid, water resistance, resistance to ag(e)ing and salt spray corrosion resistance.Unmodified graphene is due to being difficult to
Dispersed, although playing certain shielding action, graphene agglomeration body easily leads to film forming defect, causes oozing for eroded elements
Thoroughly.
Claims (9)
1. a kind of preparation method of graphene oxide modified aqueous acrylic acid anticorrosive paint, it is characterised in that include the following steps：
1）N,N-Dimethylformamide, graphene oxide, catalyst and glycidyl neodecanoate are mixed, at 120~150 DEG C
Under the conditions of react, centrifuged after then reaction mass is cooled down again, obtain solid phase vacuum drying, obtain modified graphene oxide；
2）The modified graphene oxide, coalescents, hydroxyl acrylic emulsion and defoamer are ground in three-roll grinder
Afterwards, 325 amino resins of U.S. cyanogen spy Cymel is added, then is ground, obtains graphene oxide modified aqueous acrylic acid anticorrosive paint.
2. preparation method according to claim 1, it is characterised in that the step 1）Middle N,N-dimethylformamide, oxidation
The mass ratio that feeds intake of graphene, catalyst and glycidyl neodecanoate is 100: 20~60: 1~3: 2~5.
3. preparation method according to claim 2, it is characterised in that the step 1）Middle catalyst is triethylamine, N- methyl
Any one in imidazoles, triphenylphosphine.
4. preparation method according to claim 2, it is characterised in that the step 1）In be cooled to 30 DEG C after centrifuge.
5. preparation method according to claim 3, it is characterised in that the step 1）Described in vacuum drying temperature be
80 DEG C, pressure≤20Pa.
6. preparation method according to claim 1, it is characterised in that the step 2）Described in modified graphene oxide, into
Film auxiliary agent, the mass ratio that feeds intake of 325 amino resins of hydroxyl acrylic emulsion, defoamer and U.S. cyanogen spy Cymel are 0.1~0.5
: 2~5: 80~100: 0.1~0.5: 1~5.
7. the preparation method according to claim 1 or 6, it is characterised in that the step 2）Described in coalescents be 12
One kind in carbon alcohol ester, propylene glycol monomethyl ether, butyl glycol ether.
8. the preparation method according to claim 1 or 6, it is characterised in that the step 2）Described in hydroxy yogurt
Liquid, hydroxyl value are 50-100mg KOH/g.
9. the preparation method according to claim 1 or 6, it is characterised in that the step 2）Described in defoamer be BYK
028th, one kind in peaceful FoamStar ST 2410AC or the TEGO foamex1488 of BASF section.
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| CN110886109A (en) * | 2019-12-20 | 2020-03-17 | 湖州拉杜拉塔服饰有限公司 | Environment-friendly dyeing method of modified nylon yarn |
| CN110886030A (en) * | 2019-12-20 | 2020-03-17 | 湖州拉杜拉塔服饰有限公司 | Preparation method of nylon yarn with good antibacterial and dyeing properties |
| CN111978771A (en) * | 2019-05-21 | 2020-11-24 | 中车唐山机车车辆有限公司 | Modified graphene oxide, preparation method thereof, anticorrosive paint containing modified graphene oxide and preparation method |
| CN112679683A (en) * | 2019-10-18 | 2021-04-20 | 广州大学 | Functionalized graphene oxide modified core-shell structure acrylate emulsion and preparation method thereof |
| CN112876925A (en) * | 2021-03-11 | 2021-06-01 | 国家电网有限公司 | Preparation method of low-temperature-resistant stretch-resistant anticorrosive paint |
| CN113388302A (en) * | 2021-06-08 | 2021-09-14 | 深圳市烯世传奇科技有限公司 | Conductive coating and preparation method thereof, electronic device and manufacturing method thereof |
| CN116082869A (en) * | 2022-12-29 | 2023-05-09 | 四川卡柏莱尼科技有限公司 | Carbon nano inorganic silicate anticorrosive paint |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111978771A (en) * | 2019-05-21 | 2020-11-24 | 中车唐山机车车辆有限公司 | Modified graphene oxide, preparation method thereof, anticorrosive paint containing modified graphene oxide and preparation method |
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| CN110886109A (en) * | 2019-12-20 | 2020-03-17 | 湖州拉杜拉塔服饰有限公司 | Environment-friendly dyeing method of modified nylon yarn |
| CN110886030A (en) * | 2019-12-20 | 2020-03-17 | 湖州拉杜拉塔服饰有限公司 | Preparation method of nylon yarn with good antibacterial and dyeing properties |
| CN112876925A (en) * | 2021-03-11 | 2021-06-01 | 国家电网有限公司 | Preparation method of low-temperature-resistant stretch-resistant anticorrosive paint |
| CN113388302A (en) * | 2021-06-08 | 2021-09-14 | 深圳市烯世传奇科技有限公司 | Conductive coating and preparation method thereof, electronic device and manufacturing method thereof |
| CN116082869A (en) * | 2022-12-29 | 2023-05-09 | 四川卡柏莱尼科技有限公司 | Carbon nano inorganic silicate anticorrosive paint |
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