CN106590325A - Water-borne organic and inorganic hybrid anticorrosive paint containing aromatic curing agent and preparation method thereof - Google Patents

Water-borne organic and inorganic hybrid anticorrosive paint containing aromatic curing agent and preparation method thereof Download PDF

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CN106590325A
CN106590325A CN201610998217.5A CN201610998217A CN106590325A CN 106590325 A CN106590325 A CN 106590325A CN 201610998217 A CN201610998217 A CN 201610998217A CN 106590325 A CN106590325 A CN 106590325A
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curing agent
aromatic curing
anticorrosive paint
water
quality
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CN106590325B (en
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高延敏
陈亮
左银泽
周岳珅
吴双
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Hebei Chenyang Industry and Trade Group Co Ltd
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Jiangsu University of Science and Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00—Preparation of carboxylic acid amides
    • C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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    • C08G59/54—Amino amides>
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    • C08K5/00—Use of organic ingredients
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    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
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    • 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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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C08K3/20—Oxides; Hydroxides
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Abstract

The invention discloses water-borne organic and inorganic hybrid anticorrosive paint containing an aromatic curing agent and a preparation method thereof, wherein the general structure formula of the aromatic curing agent is shown as the accompanying drawing, wherein m=1 to 6. 1,5-naphthalenediamine is used as raw materials and is firstly subjected to dehydration condensation with oxalic acid; then, thionyl chloride is added for substituting molecular chain terminal hydroxyls; finally, acylation reaction with polyamine is performed; the aromatic curing agent is obtained. The water-borne organic and inorganic hybrid anticorrosive paint is prepared from the following ingredients in percentage by mass: 43 to 62 percent of water-borne epoxy resin, 5 to 9 percent of aromatic curing agents, 2 to 4 percent of coalescing agents, 21 to 38 percent of fillers, 1 to 2 percent of corrosion inhibitors and 5 to 8 percent of compound coupling agents. The water-borne organic and inorganic hybrid anticorrosive paint has high mechanical strength, high dispersibility and high stability, and can be cured into a film in short time; the salt spray resistant performance is good.

Description

Aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent and preparation method
Technical field
It is more particularly to a kind of the invention belongs to paint field, and in particular to a kind of aqueous organic inorganic hybridization anticorrosive paint Using aromatic compound as curing agent, possesses the coating of high mechanical properties, polymolecularity, high corrosion-resistant.
Background technology
It is surprising to corrode the loss caused in human being's production life, and the whole world is every year because the economic loss that corrosion is caused reaches 1000000000000 dollars.China is due to corroding the economic loss for causing up to 300,000,000,000 RMB every year, so huge national economy Loss, just urgently supervises the development of anticorrosive paint industry.General anticorrosive paint is by resin, filler, auxiliary agent, organic solvent group Into.Due to the presence of organic solvent, during construction and production, easily cause volatilization and pollute environment, therefore develop with Water will become emphasis at present and in the future for the environment-friendly type coating of solvent.CN 102746766B disclose one kind in water-base epoxy Add Ludox to improve corrosion proof method in resin, salt-fog resistant time greatly improved.CN 102719121A disclose one kind The method that silane metal is added in water paint, greatly improved corrosion resistance and adhesive force.
In all kinds of water paint, epoxy water paint causes the concern of people with good corrosion resistance.Use at present Aqueous epoxy coating is usually that being can be with the state of self-emulsifying with epoxy-ester or epoxy resin as skeleton by epoxy resin modification. In method of modifying, one kind is by introducing hydrophilic radical, the epoxy radicals of this method meeting large losses, epoxy with epoxy reaction Therefore resin also can lose good antiseptic property；Another is exactly to be reacted using the hydroxyl in epoxy backbone, Hydrophilic polar group is introduced after production epoxy-ester, but corrosion resistance times so declines to a great extent.
It is different from solvent type epoxy resin, for the curing agent of aqueous epoxy resins, except wanting aqueous epoxy resins to have Outside good compatibility, can also emulsify in water.Water-soluble nitrogen-containing organic compound is usually taken as curing agent, Such as diethylenetriamine, but poor compatibility is because, coating occurs layering and affects the physics and chemical property of coating.Cause This, needs to control the fusion performance between aqueous epoxy resin curing agent and epoxy resin.
Water paint during not yet film forming is contacted with metal, will accelerate corrosion of metal because aqueous, make metal Surface produce flash rusting.Therefore, water paint will control the flash rusting problem during drying and forming-film.To solve this problem, Coating is needed rapidly to be attached to metal surface, coating film forming speed will as far as possible avoid soon connecing for metal surface and air Touch, the filler in coating be able to will well mix with resin hole can not occurs.In order to meet above-mentioned requirements, general way It is to add the curing agent that can play rapid shaping in coating, conventional curing agent is the amine-type cure for possessing a large amount of reactive hydrogens Agent, this curing agent can play quick-setting effect, but coating is often more crisp, and insufficient strength is high, and easily cracking.
Generally speaking, using aqueous epoxy resins prepare anticorrosive paint on adhesive force, anti-corrosion and chemical-resistance with Oiliness epoxy coating also has quite poor away from its salt spray resistance is typically at 500 hours or so.Therefore, in order to improve aqueous ring The corrosion resistance of oxygen tree fat, the selection of curing agent is very crucial with preparation.
The content of the invention
The technical problem of solution：In order to overcome the defect of prior art, obtain a kind of not only with high mechanical properties, high score Scattered property and high stability, while curing of coatings speed is fast, toughness is high, the water paint that salt spray resistance is good, the present invention is provided A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent and preparation method.
Technical scheme：A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, by mass percentage by Component：Aqueous epoxy resins 43～62%, aromatic curing agent 5～9%, coalescents 2～4%, filler 21～38%, inhibition Agent 1～2%, coupling agent 5～8% is constituted, wherein the molecular structural formula of the aromatic curing agent is as follows：
In formula, m=1～6.
The preparation method of the described aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, comprising following step Suddenly：
1st step, adopts 1,5- naphthylenediamines as raw material, first carries out dehydrating condensation with oxalic acid, adds thionyl chloride replacement Molecule chain end hydroxyl, finally carries out acylation reaction with polyamine, obtains aromatic curing agent；
2nd step, by epoxy resin and diethanol amine ring-opening polymerisation is carried out, then is obtained in product and into salt with Bronsted acid The emulsifying agent of epoxy resin, is then mixed in emulsifying agent, epoxy resin, water, obtains aqueous epoxy resins；
3rd step, after weighing filler, is ground to particle diameter for 0.1～3 μm in grinder, by the coupling agent of 1/2 mass with fill out Material mixing, adds the water of packing quality 20～30%, and 3～5h is then stirred at normal temperatures, and 50～60 are positioned over after stirring DEG C baking oven in 25～35h of heat preservation and dryness, obtain coupling agent modified filler；
4th step, by aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining Coupling agent mixes, and 5～7h of uniform stirring obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
Preferably, the preparation process of acquisition aromatic curing agent is in the 1st step：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and N, N- dimethyl methyl In the environment solution of acid amides equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:5～7；Solution upon mixing The dicyclohexylcarbodiimide of middle addition 15～25% is warming up to 50～65 DEG C of 10～12h of stirring as catalyst；Subsequently will be molten Liquid is warming up to 135 DEG C of 30～50min of insulation and evaporates dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 4～6 times of quality, adds mixed The thionyl chloride of solution quality 15～25% is closed, 35～45 DEG C of 7～9h of stirring are warming up to；Subsequently solution is warming up to into 100 DEG C of guarantors 40～70min of temperature evaporates remaining thionyl chloride；
Phase III, in previous step product, the polyamine of its quality 10～15% is added, solution upon mixing The middle DMAP for adding its quality 5～10% is warming up to 90～130 DEG C of 20～35h of stirring as catalyst；Subsequently Solution is warming up to into 175 DEG C of 20～40min of insulation to evaporate DMAP, while part N is evaporated, N- dimethyl Formamide solvent, obtains the aromatic curing agent of concentration.
Preferably, the aqueous epoxy resins are emulsifying agent, epoxy resin, the mixture of water, wherein per the breast of 1 part of quality Agent, the epoxy resin and 2～3 parts of water for needing 5～7 parts is mixed.
Preferably, the coalescents are butyl glycol ether, ethanol, the mixture of butanol, wherein the second two per 1 part of quality Alcohol butyl ether, the ethanol and 3～5 parts of butanol for needing 7～10 parts is mixed.
Preferably, described filler be trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcous mixture, wherein Per the trbasic zinc phosphate of 1 part of quality, 3～5 parts of zinc molybdate, 2～4 parts of aluminium triphosphate, 1～2 part of titanium dioxide and 1～2 is needed The talcum powder of part is mixed.
Preferably, the corrosion inhibiter be dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, the mixture of phenylpropyl alcohol triazole, Wherein per the dinonyl naphthalene sulfonate barium of 1 part of quality, 2～4 parts of dodecenylsuccinic acids and 3～5 parts of phenylpropyl alcohol triazoles are needed to carry out Mixing.
Specific embodiment
Following examples further illustrate present disclosure, but should not be construed as limiting the invention.Without departing substantially from In the case of spirit of the invention and essence, the modification made to the inventive method, step or condition and replacement belong to the present invention Scope.If not specializing, the conventional meanses that technological means used is well known to those skilled in the art in embodiment.
Embodiment 1
A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the coating is by quality hundred by component Divide ratio：Aqueous epoxy resins 56%, aromatic curing agent 8%, coalescents 4%, filler 25%, corrosion inhibiter 1%, coupling agent 6% composition.
The preparation method of the described aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, comprising following step Suddenly：
1st step, adopts 1,5- naphthylenediamines as raw material, first carries out dehydrating condensation with oxalic acid, adds thionyl chloride replacement Molecule chain end hydroxyl, finally carries out acylation reaction with polyamine, obtains aromatic curing agent；
2nd step, by epoxy resin and diethanol amine ring-opening polymerisation is carried out, then is obtained in product and into salt with Bronsted acid The emulsifying agent of epoxy resin, is then mixed in emulsifying agent, epoxy resin, water, obtains aqueous epoxy resins；
3rd step, after weighing filler, is ground to particle diameter for 0.1～3 μm in grinder, by the coupling agent of 1/2 mass with fill out Material mixing, adds the water of packing quality 20%, and 3h is then stirred at normal temperatures, is positioned over after stirring in 55 DEG C of baking oven and protects Temperature is dried 30h, obtains coupling agent modified filler；
4th step, by aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining Coupling agent mixes, uniform stirring 5h, obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
The preparation process of the aromatic curing agent is as follows：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and N, N- dimethyl methyl In the environment solution of acid amides equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:5；Add in solution upon mixing Enter 15% dicyclohexylcarbodiimide as catalyst, be warming up to 65 DEG C of stirring 10h；Subsequently solution is warming up to into 135 DEG C of guarantors Warm 40min evaporates dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 5 times of quality, adds mixing molten The thionyl chloride of liquid quality 15%, is warming up to 35 DEG C of stirring 9h；Subsequently solution is warming up to into 100 DEG C of insulation 50min will be remaining Thionyl chloride is evaporated；
Phase III, in previous step product, the polyamine of its quality 10% is added, added in solution upon mixing Enter the DMAP of its quality 5% as catalyst, be warming up to 90 DEG C of stirring 35h；Subsequently solution is warming up to into 175 DEG C Insulation 20min evaporates DMAP, while evaporating part DMF solvent, obtains concentration Aromatic curing agent.
The aqueous epoxy resins are emulsifying agent, epoxy resin, water according to mass ratio 1:7:3 mixture.
The coalescents are butyl glycol ether, ethanol, butanol according to mass ratio 1:9:4 mixture.
Described filler is trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcum powder according to mass ratio 1:5:2:2:1 Mixture.
The corrosion inhibiter is dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, phenylpropyl alcohol triazole according to mass ratio 1:3:5 Mixture.
Embodiment 2
A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the coating is by quality hundred by component Divide ratio：Aqueous epoxy resins 43%, aromatic curing agent 6%, coalescents 3%, filler 38%, corrosion inhibiter 2%, coupling agent 8% composition.
The preparation method of the described aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the same embodiment of step 1, wherein in the 3rd step, after weighing filler, particle diameter is ground in grinder for 0.1～3 μm, by the coupling agent of 1/2 mass with Filler mixes, and adds the water of packing quality 25%, 5h is then stirred at normal temperatures, during 50 DEG C of baking oven is positioned over after stirring Heat preservation and dryness 35h, obtains coupling agent modified filler.
By aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining coupling agent Mixing, uniform stirring 7h obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
The preparation process of the aromatic curing agent is as follows：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and N, N- dimethyl methyl In the environment solution of acid amides equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:6；Add in solution upon mixing Enter 25% dicyclohexylcarbodiimide as catalyst, be warming up to 50 DEG C of stirring 11h；Subsequently solution is warming up to into 135 DEG C of guarantors Warm 50min evaporates dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 4 times of quality, adds mixing molten The thionyl chloride of liquid quality 25%, is warming up to 45 DEG C of stirring 9h；Subsequently solution is warming up to into 100 DEG C of insulation 70min will be remaining Thionyl chloride is evaporated；
Phase III, in previous step product, the polyamine of its quality 15% is added, added in solution upon mixing Enter the DMAP of its quality 10% as catalyst, be warming up to 130 DEG C of stirring 20h；Subsequently solution is warming up to into 175 DEG C insulation 30min DMAP is evaporated, while evaporating part DMF solvent, concentrated Aromatic curing agent.
The aqueous epoxy resins are emulsifying agent, epoxy resin, water according to mass ratio 1:5:3 mixture.
The coalescents are butyl glycol ether, ethanol, butanol according to mass ratio 1:7:5 mixture.
Described filler is trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcum powder according to mass ratio 1:3:4:1:2 Mixture.
The corrosion inhibiter is dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, phenylpropyl alcohol triazole according to mass ratio 1:2:5 Mixture.
Embodiment 3
A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the coating is by quality hundred by component Divide ratio：Aqueous epoxy resins 62%, aromatic curing agent 8%, coalescents 3%, filler 21%, corrosion inhibiter 1%, coupling agent 5% composition.
The preparation method of the described aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the same embodiment of step 1, wherein in the 3rd step, after weighing filler, particle diameter is ground in grinder for 0.1～3 μm, by the coupling agent of 1/2 mass with Filler mixes, and adds the water of packing quality 30%, 4h is then stirred at normal temperatures, during 60 DEG C of baking oven is positioned over after stirring Heat preservation and dryness 25h, obtains coupling agent modified filler.
By aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining coupling agent Mixing, uniform stirring 7h obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
The preparation process of the aromatic curing agent is as follows：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and N, N- dimethyl methyl In the environment solution of acid amides equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:5；Add in solution upon mixing Enter 20% dicyclohexylcarbodiimide as catalyst, be warming up to 60 DEG C of stirring 12h；Subsequently solution is warming up to into 135 DEG C of guarantors Warm 30min evaporates dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 6 times of quality, adds mixing molten The thionyl chloride of liquid quality 25%, is warming up to 40 DEG C of stirring 7h；Subsequently solution is warming up to into 100 DEG C of insulation 40min will be remaining Thionyl chloride is evaporated；
Phase III, in previous step product, the polyamine of its quality 14% is added, added in solution upon mixing Enter the DMAP of its quality 7% as catalyst, be warming up to 120 DEG C of stirring 25h；Subsequently solution is warming up to into 175 DEG C insulation 40min DMAP is evaporated, while evaporating part DMF solvent, concentrated Aromatic curing agent.
The aqueous epoxy resins are emulsifying agent, epoxy resin, water according to mass ratio 1:6:2 mixture.
The coalescents are butyl glycol ether, ethanol, butanol according to mass ratio 1:10:5 mixture.
Described filler is trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcum powder according to mass ratio 1:5:4:1:1 Mixture.
The corrosion inhibiter is dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, phenylpropyl alcohol triazole according to mass ratio 1:4:5 Mixture.
Embodiment 4
A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the coating is by quality hundred by component Divide ratio：Aqueous epoxy resins 55%, aromatic curing agent 9%, coalescents 4%, filler 24%, corrosion inhibiter 2%, coupling agent 6% composition.
The preparation method of the described aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the same embodiment of step 1, wherein in the 3rd step, after weighing filler, particle diameter is ground in grinder for 0.1～3 μm, by the coupling agent of 1/2 mass with Filler mixes, and adds the water of packing quality 20%, 5h is then stirred at normal temperatures, during 50 DEG C of baking oven is positioned over after stirring Heat preservation and dryness 25h, obtains coupling agent modified filler.
By aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining coupling agent Mixing, uniform stirring 5h obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
The preparation process of the aromatic curing agent is as follows：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and N, N- dimethyl methyl In the environment solution of acid amides equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:7；Add in solution upon mixing Enter 15% dicyclohexylcarbodiimide as catalyst, be warming up to 65 DEG C of stirring 11h；Subsequently solution is warming up to into 135 DEG C of guarantors Warm 45min evaporates dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 5 times of quality, adds mixing molten The thionyl chloride of liquid quality 15%, is warming up to 45 DEG C of stirring 8h；Subsequently solution is warming up to into 100 DEG C of insulation 60min will be remaining Thionyl chloride is evaporated；
Phase III, in previous step product, the polyamine of its quality 13% is added, added in solution upon mixing Enter the DMAP of its quality 8% as catalyst, be warming up to 110 DEG C of stirring 25h；Subsequently solution is warming up to into 175 DEG C insulation 35min DMAP is evaporated, while evaporating part DMF solvent, concentrated Aromatic curing agent.
The aqueous epoxy resins are emulsifying agent, epoxy resin, water according to mass ratio 1:6:3 mixture.
The coalescents are butyl glycol ether, ethanol, butanol according to mass ratio 1:7:3 mixture.
Described filler is trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcum powder according to mass ratio 1:5:4:2:2 Mixture.
The corrosion inhibiter is dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, phenylpropyl alcohol triazole according to mass ratio 1:2:3 Mixture.
Embodiment 5
A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the coating is by quality hundred by component Divide ratio：Aqueous epoxy resins 48%, aromatic curing agent 8%, coalescents 2%, filler 33%, corrosion inhibiter 2%, coupling agent 7% composition.
The preparation method of the described aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the same embodiment of step 1, wherein in the 3rd step, after weighing filler, particle diameter is ground in grinder for 0.1～3 μm, by the coupling agent of 1/2 mass with Filler mixes, and adds the water of packing quality 25%, 4h is then stirred at normal temperatures, during 60 DEG C of baking oven is positioned over after stirring Heat preservation and dryness 30h, obtains coupling agent modified filler.
By aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining coupling agent Mixing, uniform stirring 6h obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
The preparation process of the aromatic curing agent is as follows：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and N, N- dimethyl methyl In the environment solution of acid amides equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:7；Add in solution upon mixing Enter 15% dicyclohexylcarbodiimide as catalyst, be warming up to 50 DEG C of stirring 12h；Subsequently solution is warming up to into 135 DEG C of guarantors Warm 45min evaporates dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 4～6 times of quality, adds mixed The thionyl chloride of solution quality 20% is closed, 35 DEG C of stirring 9h are warming up to；Subsequently solution being warming up to into 100 DEG C of insulation 70min will remain Remaining thionyl chloride is evaporated；
Phase III, in previous step product, the polyamine of its quality 10% is added, added in solution upon mixing Enter the DMAP of its quality 10% as catalyst, be warming up to 130 DEG C of stirring 25h；Subsequently solution is warming up to into 175 DEG C insulation 40min DMAP is evaporated, while evaporating part DMF solvent, concentrated Aromatic curing agent.
The aqueous epoxy resins are emulsifying agent, epoxy resin, water according to mass ratio 1:7:3 mixture.
The coalescents are butyl glycol ether, ethanol, butanol according to mass ratio 1:7:5 mixture.
Described filler is trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcum powder according to mass ratio 1:5:2:1:2 Mixture.
The corrosion inhibiter is dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, phenylpropyl alcohol triazole according to mass ratio 1:4:3 Mixture.
Embodiment 6
A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the coating is by quality hundred by component Divide ratio：Aqueous epoxy resins 44%, aromatic curing agent 5%, coalescents 4%, filler 37%, corrosion inhibiter 2%, coupling agent 8% composition.
The preparation method of the described aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the same embodiment of step 1, wherein in the 3rd step, after weighing filler, particle diameter is ground in grinder for 0.1～3 μm, by the coupling agent of 1/2 mass with Filler mixes, and adds the water of packing quality 30%, 5h is then stirred at normal temperatures, during 50 DEG C of baking oven is positioned over after stirring Heat preservation and dryness 35h, obtains coupling agent modified filler.
By aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining coupling agent Mixing, uniform stirring 7h obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
The preparation process of the aromatic curing agent is as follows：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and N, N- dimethyl methyl In the environment solution of acid amides equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:7；Add in solution upon mixing Enter 15% dicyclohexylcarbodiimide as catalyst, be warming up to 65 DEG C of stirring 10h；Subsequently solution is warming up to into 135 DEG C of guarantors Warm 50min evaporates dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 4 times of quality, adds mixing molten The thionyl chloride of liquid quality 15%, is warming up to 45 DEG C of stirring 8h；Subsequently solution is warming up to into 100 DEG C of insulation 70min will be remaining Thionyl chloride is evaporated；
Phase III, in previous step product, the polyamine of its quality 15% is added, added in solution upon mixing Enter the DMAP of its quality 5% as catalyst, be warming up to 90 DEG C of stirring 35h；Subsequently solution is warming up to into 175 DEG C Insulation 30min evaporates DMAP, while evaporating part DMF solvent, obtains concentration Aromatic curing agent.
The aqueous epoxy resins are emulsifying agent, epoxy resin, water according to mass ratio 1:5:2 mixture.
The coalescents are butyl glycol ether, ethanol, butanol according to mass ratio 1:7:5 mixture.
Described filler is trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcum powder according to mass ratio 1:3:4:1:2 Mixture.
The corrosion inhibiter is dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, phenylpropyl alcohol triazole according to mass ratio 1:4:4 Mixture.
Embodiment 7
A kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the coating is by quality hundred by component Divide ratio：Aqueous epoxy resins 51%, aromatic curing agent 7%, coalescents 3%, filler 32%, corrosion inhibiter 1%, coupling agent 6% composition.
The preparation method of the described aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, the same embodiment of step 1, wherein in the 3rd step, after weighing filler, particle diameter is ground in grinder for 0.1～3 μm, by the coupling agent of 1/2 mass with Filler mixes, and adds the water of packing quality 25%, 4h is then stirred at normal temperatures, during 55 DEG C of baking oven is positioned over after stirring Heat preservation and dryness 30h, obtains coupling agent modified filler.
By aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining coupling agent Mixing, uniform stirring 6h obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
The preparation process of the aromatic curing agent is as follows：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and N, N- dimethyl methyl In the environment solution of acid amides equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:6；Add in solution upon mixing Enter 20% dicyclohexylcarbodiimide as catalyst, be warming up to 55 DEG C of stirring 11h；Subsequently solution is warming up to into 135 DEG C of guarantors Warm 40min evaporates dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 5 times of quality, adds mixing molten The thionyl chloride of liquid quality 20%, is warming up to 40 DEG C of stirring 8h；Subsequently solution is warming up to into 100 DEG C of insulation 55min will be remaining Thionyl chloride is evaporated；
Phase III, in previous step product, the polyamine of its quality 12% is added, added in solution upon mixing Enter the DMAP of its quality 7% as catalyst, be warming up to 110 DEG C of stirring 25h；Subsequently solution is warming up to into 175 DEG C insulation 30min DMAP is evaporated, while evaporating part DMF solvent, concentrated Aromatic curing agent.
The aqueous epoxy resins are emulsifying agent, epoxy resin, water according to mass ratio 1:5:2 mixture.
The coalescents are butyl glycol ether, ethanol, butanol according to mass ratio 1:9:4 mixture.
Described filler is trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcum powder according to mass ratio 1:4:3:2:1 Mixture.
The corrosion inhibiter is dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, phenylpropyl alcohol triazole according to mass ratio 1:3:4 Mixture.
Above-mentioned coating is formed is tested after coating, as a result as shown in the table:

Claims (7)

1. a kind of aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent, it is characterised in that by mass percentage by Component：Aqueous epoxy resins 43～62%, aromatic curing agent 5～9%, coalescents 2～4%, filler 21～38%, inhibition Agent 1～2%, coupling agent 5～8% is constituted, wherein the molecular structural formula of the aromatic curing agent is as follows：
In formula, m=1～6.
2. a kind of preparation side of the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent according to claim 1 Method, it is characterised in that comprise the steps of：
1st step, adopts 1,5- naphthylenediamines as raw material, first carries out dehydrating condensation with oxalic acid, adds thionyl chloride and replaces molecule Last-in-chain(LIC) terminal hydroxy group, finally carries out acylation reaction with polyamine, obtains aromatic curing agent；
2nd step, by epoxy resin and diethanol amine ring-opening polymerisation is carried out, then obtains epoxy by product and into salt with Bronsted acid The emulsifying agent of resin, is then mixed in emulsifying agent, epoxy resin, water, obtains aqueous epoxy resins；
3rd step, after weighing filler, is ground to particle diameter for 0.1～3 μm in grinder, and the coupling agent of 1/2 mass and filler are mixed Close, add the water of packing quality 20～30%, 3～5h is then stirred at normal temperatures, 50～60 DEG C are positioned over after stirring 25～35h of heat preservation and dryness in baking oven, obtains coupling agent modified filler；
4th step, by aqueous epoxy resins, aromatic curing agent, coalescents, corrosion inhibiter, modified filler and remaining coupling Agent mixes, 5～7h of uniform stirring, obtains the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent.
3. the preparation method of the aqueous organic inorganic hybridization anticorrosive paint containing aromatic curing agent according to claim 2, Characterized in that, the preparation process that aromatic curing agent is obtained in the 1st step is：
First stage, by raw material 1,5- naphthylenediamines are 1 according to mol ratio with oxalic acid:2, put into water and DMF In the environment solution of equal-volume composition, wherein the mass ratio of raw material and environment solution is 1:5～7；Add in solution upon mixing Enter 15～25% dicyclohexylcarbodiimide as catalyst, be warming up to 50～65 DEG C of 10～12h of stirring；Subsequently by solution liter Temperature to 135 DEG C of 30～50min of insulation evaporate dicyclohexylcarbodiimide；
Second stage, previous step product is put in the DMF of 4～6 times of quality, adds mixing molten The thionyl chloride of liquid quality 15～25%, is warming up to 35～45 DEG C of 7～9h of stirring；Subsequently solution is warming up to into 100 DEG C of insulations 40 ～70min evaporates remaining thionyl chloride；
Phase III, in previous step product, the polyamine of its quality 10～15% is added, added in solution upon mixing Enter the DMAP of its quality 5～10% as catalyst, be warming up to 90～130 DEG C of 20～35h of stirring；Subsequently will be molten Liquid is warming up to 175 DEG C of 20～40min of insulation and evaporates DMAP, while part N is evaporated, N- dimethyl formyls Amine solvent, obtains the aromatic curing agent of concentration.
4. it is according to claim 2 containing compounding coupling agent aqueous organic inorganic hybridization anticorrosive paint preparation method, its It is characterised by, the aqueous epoxy resins are emulsifying agent, epoxy resin, the mixture of water, wherein per the emulsifying agent of 1 part of quality, The epoxy resin and 2～3 parts of water for needing 5～7 parts is mixed.
5. it is according to claim 2 containing compounding coupling agent aqueous organic inorganic hybridization anticorrosive paint preparation method, its It is characterised by, the coalescents are butyl glycol ether, ethanol, the mixture of butanol, wherein per the ethylene glycol fourth of 1 part of quality Ether, the ethanol and 3～5 parts of butanol for needing 7～10 parts is mixed.
6. it is according to claim 2 containing compounding coupling agent aqueous organic inorganic hybridization anticorrosive paint preparation method, its It is characterised by, described filler is trbasic zinc phosphate, zinc molybdate, aluminium triphosphate, titanium dioxide, talcous mixture, wherein per 1 part of matter The trbasic zinc phosphate of amount, needs 3～5 parts of zinc molybdate, 2～4 parts of aluminium triphosphate, 1～2 part of titanium dioxide and 1～2 part of talcum Powder is mixed.
7. it is according to claim 2 containing compounding coupling agent aqueous organic inorganic hybridization anticorrosive paint preparation method, its It is characterised by, the corrosion inhibiter is dinonyl naphthalene sulfonate barium, dodecenylsuccinic acid, the mixture of phenylpropyl alcohol triazole, wherein per 1 The dinonyl naphthalene sulfonate barium of part quality, needs 2～4 parts of dodecenylsuccinic acids and 3～5 parts of phenylpropyl alcohol triazoles to be mixed.
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