CN107523179B - A kind of water-base epoxy insulated paint and the preparation method and application thereof - Google Patents
A kind of water-base epoxy insulated paint and the preparation method and application thereof Download PDFInfo
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- CN107523179B CN107523179B CN201710601451.4A CN201710601451A CN107523179B CN 107523179 B CN107523179 B CN 107523179B CN 201710601451 A CN201710601451 A CN 201710601451A CN 107523179 B CN107523179 B CN 107523179B
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4207—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08G59/62—Alcohols or phenols
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/20—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
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- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- 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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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention discloses a kind of water-base epoxy insulated paint and preparation method thereof with answer.The preparation method is first to react polyethylene glycol with liquid epoxies to prepare active nonionic type emulsifier；Aliphatic anhydride and polyethylene glycol ring-opening reaction are generated into half ester again, then is reacted with liquid epoxies and prepares endurable active toughener；Then active nonionic type emulsifier, endurable active toughener are mixed with epoxy resin, imidazoles latent curing agent, deionized water and pigments and fillers, high speed dispersion prepares single-component water-based epoxy insulation varnish.The insulated paint overcomes most of water emulsifier and toughener is not involved in the curing reaction of epoxy resin, it can be migrated in the curing process to film coated surface, make film it is tacky, it is soaked after the shortcomings that easily whitening, with storing, low stabilization, solidification temperature, good insulation preformance, good corrosion resistance and wearability are strong, greatly prolong the service life of insulated paint.
Description
Technical field
The present invention relates to a kind of water paints, and in particular to a kind of water-base epoxy insulated paint and the preparation method and application thereof；
The water-base epoxy insulated paint function admirable, has excellent hardness and chemical resistance at stable storing, can be widely applied to wood
The fields such as device, automobile, building.
Background technique
Epoxy resin has many advantages, such as that adhesive force is high, chemical resistance is good, wearability is good and good insulation preformance, in insulated paint
Field is widely applied.Common epoxy resin insulating varnish is mostly solvent based coating, is existed containing 50% or more organic solvent
It is discharged into atmosphere in production and work progress, pollution environment and threat human health.With increasingly strict, the water of environmental regulation
Property epoxy coating is more and more taken seriously.Existing waterborne epoxy coatings is unstable in the presence of storing, and film performance is bad, needs double groups
The key technology difficulties such as subpackage dress and construction inconvenience.
The preparation of aqueous epoxy resins mainly uses self-emulsification and two kinds of outer emulsion process, and wherein self-emulsification is frequently with change
Method introduces hydrophilic radical in asphalt mixtures modified by epoxy resin fat chain, through acid or alkali neutralization at salt, and water emulsification is added to be prepared.Method preparation
Aqueous epoxy resins are not necessarily to additional emulsifier, and emulsion particle diameter is small, and stability is good, but the introducing of hydrophilic radical reduces epoxy resin
The water resistance of film also reduces its mechanical performance.
Outer emulsion process, which passes through additional emulsifier, is uniformly dispersed in epoxy resin in water, which has preparation process letter
Singly, the advantages that at low cost, become the main method of water-borne modification of epoxy resin.There are epoxy emulsion storage stability and film performances
The disadvantages of bad, needs further perfect.Outer emulsion process prepare epoxy emulsion key be emulsifier selection, commonly use emulsifier
There are OP-10, SP-60, neopelex etc..Wherein nonionic emulsifier such as OP-10 is due to by ion concentration, pH value
Phenomena such as equal influences are smaller, good with other water-base resin compatibilities, are not in demulsification, becomes the first choice of emulsion epoxy resin.
Nonionic emulsifier, which is generally reacted by hydrophobic compound such as nonyl phenol with hydrophilic compounds such as polyethylene glycol, to be made.But this
Class emulsifier is not involved in the curing reaction of epoxy, can migrate to film coated surface in the curing process, keeps film tacky, easy after soaked
Whiten, reduces the water resistance and chemical resistance of film.
Epoxy resin film is firmly crisp, not impact resistance, needs to add the impact flexibility that toughener improves film.Common plasticizers
Improve impact flexibility, plasticizer does not react in film forming procedure with curing agent, film will be slow after a period of use
It is precipitated, is that film coated surface is tacky, film becomes fragile, and shortens the service life of film.
Summary of the invention
Present invention aims to overcome that problem of the existing technology, it is quickly solid to provide a kind of environmental protection, one-component, medium temperature
Change, high-performance water-based epoxy lotion insulated paint and preparation method thereof.
Another object of the present invention is to provide the application of the aqueous epoxy emulsion insulated paint.
The present invention is prepared a kind of novel by synthesizing activity emulsifier and endurable active toughener, preferably latent curing agent
High-performance water-based epoxy lotion insulated paint.
The present invention solves the defect of outer emulsion process using active emulsifier, and so-called active emulsifier refers to polyethylene glycol
Etc. non-ionic hydrophilics group be grafted in asphalt mixtures modified by epoxy resin fat chain, can not only emulsion epoxy resin, may also participate in the solidification of epoxy resin.
Molecular weight by changing polyethylene glycol can regulate and control the HLB value of emulsifier, obtain excellent emulsifying effectiveness.
The present invention is realized by following technical proposal:
A kind of water-base epoxy insulated paint, in terms of mass fraction, raw material components composition are as follows: epoxy resin 15-25%, activity
Nonionic emulsifier 5-10%, endurable active toughener 5-10%, imidazoles latent curing agent 5-10%, pigments and fillers 15-20%, auxiliary agent 2-
5%, remaining is deionized water；
The active nonionic emulsifier is prepared via a method which: by liquid epoxies and polyethylene glycol by mole
It is added in reaction kettle than 1.5-2.0:1,80-85 DEG C of heating water bath, after mixing to reaction system, potassium sulfate catalysis is added dropwise
Agent drips off and keeps the temperature 0.5-1.0h at 80-85 DEG C, after be warming up to 180-200 DEG C, when the epoxide number of system remains unchanged, drop
Temperature discharging, synthesizes water-base epoxy emulsifier；Potassium sulfate catalyst amount is the 2-5% of epoxy resin quality；
The endurable active toughener is prepared via a method which: by aliphatic anhydride and polyethylene glycol according to 1:1.5-2.0
When the acid value of detection architecture is to theoretical value, aliphatic anhydride mole is added in 90-130 DEG C of progress ring-opening reaction 2-4h in molar ratio
The normal-butyl ammonium bromide catalyst of the 3-5% of several 1.5-2.0 times of liquid epoxies and aliphatic anhydride molal quantity,
90-130 DEG C of reaction 4-6h measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains endurable active toughener；
To further realize the object of the invention, it is preferable that the aliphatic anhydride is cis-butenedioic anhydride, succinic anhydride, adipic acid
Acid anhydride, itaconic anhydride, glutaric anhydride, tung oil acid anhydride, dodecyl succinic anhydride, cyclobutanetetracarboxylic acid anhydride, dimethyl maleic anhydride,
1,1- cyclohexyl maleic anhydride, cyclobutane -1,2- dicarboxylic acid anhydride, pentamethylene -1,1- diethyl acid anhydrides and 2,2- dimethyl succinate
It is one or more in acid anhydride.
Preferably, the liquid epoxies be bisphenol A type epoxy resin E55, E51, E44, E42, E39, E35 and
It is one or more in E31.
Preferably, the molecular weight of the polyethylene glycol is 200,300,400,600,1000,1500,2000,3000,
It is a kind of and a variety of in 4000,5000,6000,8000,10000,12000,14000,16000,18000 and 20000.
Preferably, the epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol S type epoxy tree
In rouge, novolac epoxy resin, glycidyl ester type epoxy resin, cycloaliphatic epoxy resin and aliphatic epoxy resin it is a kind of or
It is a variety of；
Model E12, E20, E42, E-44 or E-51 of the bisphenol A type epoxy resin；
The model CYDF-170 of the bisphenol f type epoxy resin or 6458；
The model 185S or 300SS of the bisphenol-s epoxy resin；
Model JF-45, F-44 or F-51 of the novolac epoxy resin；
The model FA-68 of the glycidyl ester type epoxy resin or 711；
The model ZH68-01 or ZH206 of ring race epoxy resin；
The aliphatic epoxy resin is aliphatic epoxy resin 2000.
Preferably, the imidazoles latent curing agent are as follows: 1- benzyl -2-methylimidazole, 1-cyanoethyl-2-phenylimidazole are inclined
Trimellitate, 2,4- diamino -6- [2 '-methylimidazolyls-(1) '] ethyl-S- triazine, 2,4- diamino -6- [2 '-hendecyls
Imidazole radicals-(1) '] ethyl-S- triazine, 2,4- diamino -6- [2 '-ethyls -4-methylimidazole base-(1) '] ethyl-S- triazine,
1- dodecyl -2- methyl-3-benzyl imidazole chloride, 1,3- dibenzyl -2-methylimidazole chloride or 2- phenyl -4- methyl -
5- hydroxy methylimidazole etc. is one or more；
The pigments and fillers are made of pigment and filler, and the mass ratio of pigment and filler is 1:1.5-3.0；Wherein pigment is titanium
One of white, lithopone, iron oxide red, toluidine red, lead chromate yellow, barba hispanica, iron oxide black are a variety of；Filler is calcium carbonate, barium sulfate, silicon
It is one or more in lime, talcum powder, alumina powder, silicon nitride powder, mica powder and porous konilite.
Preferably, the auxiliary agent includes aqueous defoamer, aqueous levelling agent, water-based thickener and fungicide；
The aqueous defoamer includes organic silicon type defoaming agent BYK-018, polyether-type defoaming agent BYK-019 and polyether-modified
One of silicon type defoaming agent Digao TEGO-810 or a variety of；
The aqueous levelling agent includes modified polyether class levelling agent TEGO-450 and modified organic silicon class levelling agent BYK-306
One of or it is a variety of；
The water-based thickener includes cellulose thickener Natrosol HEC, agent for polyacrylic acid thickening VISCOLAM
It is one or more in the RM-8W of 330 and polyurethanes thickener DOW company；
The fungicide includes substituted arene class fungicide pentachloronitrobenzene, heterocycles fungicide methyl-isothiazol
One of quinoline ketone, aminated compounds class fungicide fenfuram are a variety of.
The preparation method of the water-base epoxy insulation paint film: by epoxy resin, active nonionic emulsifier, active toughening
Agent, imidazoles latent curing agent, pigments and fillers, auxiliary agent and deionized water mixing, high-speed stirred 3-5h, until fineness less than 20 microns with
Under, obtain single-component water-based epoxy insulation varnish；Solid content is 50-60wt%.
The application of the water-base epoxy insulated paint: by the described water-base epoxy insulated paint spraying or dip-coating in substrate surface,
110-130 DEG C solidification 60-120 minutes.The storage stability of the water-base epoxy insulation paint film of formation is not less than 1 year；Film is hard
Degree is 2H-3H, and impact resistance >=50cm, adhesive force is 0 grade；Pass through 96h water resistance test；Insulating properties reaches B-F grades, wherein body
Under product resistivity normality >=1013Ω m, electrical strength >=25MV/m under the normality of continuous method test of boosting；Dielectric dissipation factor
Under normality≤1%；Other performances meet GB/T 1981.6-2014, and " electric insulation paints the 6th part: environment-friendly type aqueous dipping
Paint " standard.
Technical principle of the invention is as follows:
1) preparation of the non-ionic emulsion agent of reactivity:
It prepares to have by polyethylene glycol (nonionic emulsifier) and the liquid epoxies reaction of suitable molecular weight and close
The high-efficiency activated emulsifier of suitable HLB value, end group are the epoxy group that can participate in reaction, which can be effectively reduced product cut size
And particle diameter distribution, improve product shelf life and dilution stability.
2) preparation of reactive toughening agent:
Half ester (end group is carboxyl) is generated by the polyethylene glycol and aliphatic anhydride ring-opening reaction of suitable molecular weight, then
It is reacted with liquid epoxies and introduces epoxy group on product end group, a certain amount of flexible base is contained on the product molecule chain of preparation
Group or resin, the toughness after improving epoxy resin cure improve the disadvantages of really up to the mark and excessively crisp after pure epoxy resin solidifies.
Compared with the prior art, the invention has the following advantages that
1) present invention is prepared by the polyethylene glycol and epoxy resin reaction of selection suitable molecular weight with suitable HLB value
High-efficiency activated emulsifier, be effectively reduced product cut size and particle diameter distribution, improve product shelf life and dilution stability.
2) half ester is produced by acid anhydrides and polyethylene glycol ring-opening reaction, then reacts the active toughening of preparation with liquid epoxies
Agent, the toughness after improving epoxy resin cure improve the disadvantages of really up to the mark and excessively crisp after pure epoxy resin solidifies；Overcome major part
Emulsifier and toughener are not involved in the curing reaction of epoxy, can migrate to film coated surface in the curing process, keep film tacky, steep
The shortcomings that easily whitening after water greatly prolongs painting membrane lifetime.
3) active nonionic type emulsifier and endurable active toughener all have liquid epoxies to prepare, because having with epoxy resin
There is similar structure, they and main body epoxy resin have preferable compatibility, and it is preferable outer to can guarantee that the film of preparation has
Sight and physical mechanical property；Another active nonionic type emulsifier is cooperateed with endurable active toughener, so that in aqueous epoxy resins film
Without small-molecular emulsifier and plasticizer, there is no small-molecule substance precipitation after film forming, is free of small molecule hydrophilic substance or hydrophilic group
Group, can improve water resistance, the chemical resistance of film, moreover it is possible to greatly prolong the service life of film；
4) it the invention belongs to non-ion aqueous lotion painting, does not need to be neutralized into salt treatment, reduce to metallic substrates
Corrosion, insulated paint is insensitive to pH, improves the stability of storage.
Specific embodiment
For a better understanding of the invention, below with reference to embodiment, the present invention will be further described, it should be noted that
Embodiment does not constitute limiting the scope of the present invention.Related method for testing performance involved in embodiment is as follows:
According to the measuring method detection in national standard " measurement of GB/T 4612-2008 plastics epoxide epoxide equivalent "
The epoxide number of reaction system is detected according to GB/T 1725-1979, GB/T 1723-1979, GB/T 9754-2007, GB/T
6739-2006、GB/T 1732-1993、GB/T 9286-1998、HG2-59-78、GB/T 5209-1985、GB/T 33328-
2016, GB/T6753-1986 test respectively the solid content of coating, viscosity, glossiness, pencil hardness, impact strength, adhesive force,
Insulating properties, water absorption rate, acid value and storage stability, pencil are the advanced drawing pencil that Shanghai China Pencil Factory No.1 produces, instrument used
Device is Tianjin Jingke's production；Coating VOC content is tested according to GB/T 23985-2009.
Embodiment 1
(1) preparation of active nonionic type emulsifier
By liquid epoxies (E-55) and polyethylene glycol (PEG-2000), 1.5:1 is added in reaction kettle in molar ratio, and 80
DEG C heating water bath after mixing to reaction system is slowly added dropwise potassium sulfate catalyst (the 3% of epoxy resin quality), drips off
Keep the temperature 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, the epoxide number of every 0.5h detection architecture, when the ring of system
When oxygen value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifier.
(2) preparation of active epoxy toughening agent
First by cis-butenedioic anhydride and polyethylene glycol (PFG-10000) according to 1:2 molar ratio in 110 DEG C of progresss ring-opening reaction 2h, detect
When the acid value of system is to theoretical value, 1.5 times of the liquid epoxies (E-44) and normal-butyl ammonium bromide of acid anhydrides molal quantity is added
Catalyst measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains endurable active toughener in 120 DEG C of reaction 4h.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 1
Table 1
Preparation step:
By epoxy resin, active nonionic emulsifier, endurable active toughener, curing agent, pigment, filler, fungicide, levelling
Agent, thickener, defoaming agent and deionized water mixing, high-speed stirred 3h, until fineness is less than 20 microns hereinafter, obtaining single-component water-based
Epoxy insulation varnish, solid content 60%, storage stability are 12 months, and film obtains after sixty minutes in 130 DEG C of solidifications in substrate
Paint film.
(4) performance test, respectively water-base epoxy the insulated paint ISOPOXYR-771 and Wen Hong standby with BACK corporation preparation
Solvent type epoxy insulated paint varnish JG-16-2 performance be compared, as a result as shown in table 2 below:
Table 2
Water-base epoxy insulated paint of the invention is compared to solvent type epoxy insulated paint as can be seen from Table 2, in mechanical performance
The advantages such as in the case where substantially equivalent, insulation performance is excellent in, and glossiness is high, and VOC emission is low, Environmental Safety reduce pair
The pollution of atmosphere saves vast resources, meets the requirement of sustainable development.Compared with water-based insulating paint on the market, the present invention
In solid content, storage stability, mechanical performance, water resistance and insulating properties suffer from clear superiority.The one side present invention passes through
The polyethylene glycol and epoxy resin reaction for selecting suitable molecular weight prepare the active emulsifier with suitable HLB value, by poly- second
Glycol is grafted in asphalt mixtures modified by epoxy resin fat chain, can not only emulsion epoxy resin, ensure water-base epoxy insulated paint storage stablize, storage period is again
It 1 year or more, may also participate in the solidification of epoxy resin, be effectively reduced product cut size and particle diameter distribution, improve product shelf life and dilute
Stability is released, compared with ionic water paint, water resistance and insulating properties, which have, to be greatly improved.The invention enables most of emulsifications
Agent and toughener participate in the curing reaction of epoxy, so that painting membrane lifetime be made to greatly prolong.On the other hand the present invention is by acid anhydrides
Half ester is produced with polyethylene glycol ring-opening reaction, then is reacted with liquid epoxies and prepares endurable active toughener, it is solid to improve epoxy resin
Toughness after change, the mechanical performance after improving epoxy resin cure.
Embodiment 2
(1) preparation of active nonionic type emulsifier
By liquid epoxies (E-51) and polyethylene glycol (PEG-400), 1.6:1 is added in reaction kettle in molar ratio, and 85 DEG C
Heating water bath after mixing to reaction system is slowly added dropwise potassium sulfate catalyst (the 2% of epoxy resin quality), drips off
Keep the temperature 1.0h at 85 DEG C, after be warming up to 200 DEG C, after reaction 4 hours, the epoxide number of every 0.5h detection architecture, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifier.
(2) preparation of active epoxy toughening agent
First by maleic anhydride and polyethylene glycol (PEG-6000) according to 1:1.5 molar ratio in 90 DEG C of progress ring-opening reaction 4h,
When the acid value of detection architecture is to theoretical value, 1.7 times of the liquid epoxies (E-39) and n-butyl bromide of acid anhydrides molal quantity is added
Change ammonium catalyst, in 130 DEG C of reaction 5h, measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains endurable active toughener.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 3
Table 3
Preparation step:
By epoxy resin, active nonionic emulsifier, endurable active toughener, curing agent, pigment, filler, fungicide, levelling
Agent, thickener, defoaming agent and deionized water mixing, high-speed stirred 4h, until fineness is less than 20 microns hereinafter, obtaining single-component water-based
Epoxy insulation varnish, solid content 51%, film obtain paint film after solidifying 120 minutes in substrate at 110 DEG C.
(4) the performance test results such as table 4
Table 4
Embodiment 3
(1) preparation of active nonionic type emulsifier
By liquid epoxies (E-31) and polyethylene glycol (PEG-10000), 2.0:1 is added in reaction kettle in molar ratio, and 82
DEG C heating water bath after mixing to reaction system is slowly added dropwise potassium sulfate catalyst (the 5% of epoxy resin quality), drips off
Keep the temperature 0.5h at 82 DEG C, after be warming up to 190 DEG C, after reaction 4 hours, the epoxide number of every 0.5h detection architecture, when the ring of system
When oxygen value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifier.
(2) preparation of active epoxy toughening agent
First by itaconic anhydride and polyethylene glycol (PEG-4000) according to 1:1.8 molar ratio in 100 DEG C of progress ring-opening reaction 3h,
When the acid value of detection architecture is to theoretical value, 1.8 times of the liquid epoxies (E-55) and n-butyl bromide of acid anhydrides molal quantity is added
Change ammonium catalyst, in 120 DEG C of reaction 4h, measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains endurable active toughener.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 5
Table 5
Preparation step:
By epoxy resin, active nonionic emulsifier, endurable active toughener, curing agent, pigment, filler, fungicide, levelling
Agent, thickener, defoaming agent and deionized water, high-speed stirred 4h, until fineness is less than 20 microns hereinafter, obtaining single-component water-based epoxy
Insulated paint, solid content 55%, film obtain paint film after solidifying 80 minutes in substrate at 120 DEG C.
(4) the performance test results such as table 6
Table 6
Embodiment 4
(1) preparation of active nonionic type emulsifier
By liquid epoxies (E42) and polyethylene glycol (PEG-16000), 2:1 is added in reaction kettle in molar ratio, and 80 DEG C
Heating water bath after mixing to reaction system is slowly added dropwise potassium sulfate catalyst (the 5% of epoxy resin quality), drips off
Keep the temperature 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, the epoxide number of every 0.5h detection architecture, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifier.
(2) preparation of active epoxy toughening agent
First by tung oil acid anhydride and polyethylene glycol (PEG-6000) according to 1:2 molar ratio in 130 DEG C of progresss ring-opening reaction 2h, examine
When the acid value of survey system is to theoretical value, 2.0 times of the liquid epoxies (E44) and normal-butyl ammonium bromide of acid anhydrides molal quantity is added
Catalyst measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains endurable active toughener in 110 DEG C of reaction 4h.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 7
Table 7
Preparation step:
By epoxy resin, active nonionic emulsifier, endurable active toughener, curing agent, pigment, filler, fungicide, levelling
Agent, thickener, defoaming agent and deionized water, high-speed stirred 4h, until fineness is less than 20 microns hereinafter, obtaining single-component water-based epoxy
Insulated paint, solid content 58%, film obtain paint film after substrate solidifies 80 minutes at 120 DEG C.
(4) the performance test results such as table 8
Table 8
Embodiment 5
(1) preparation of active nonionic type emulsifier
By liquid epoxies (E-39) and polyethylene glycol (PEG-200), 1.5:1 is added in reaction kettle in molar ratio, and 80 DEG C
Heating water bath after mixing to reaction system is slowly added dropwise potassium sulfate catalyst (the 4% of epoxy resin quality), drips off
Keep the temperature 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, the epoxide number of every 0.5h detection architecture, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifier.
(2) preparation of active epoxy toughening agent
First 2,2- dimethyl succinic anhydride is opened according to 1:2 molar ratio at 110 DEG C with polyethylene glycol (PFG-12000)
Ring reacts 2h, when the acid value of detection architecture arrives theoretical value, 1.6 times of liquid epoxies (E-42) of addition acid anhydrides molal quantity and
Normal-butyl ammonium bromide catalyst measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains active increasing in 100 DEG C of reaction 4h
Tough dose.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 9
Table 9
Preparation step:
By epoxy resin, active nonionic emulsifier, endurable active toughener, curing agent, pigment, filler, fungicide, levelling
Agent, thickener, defoaming agent and deionized water mixing, high-speed stirred 4h, until fineness is less than 20 microns hereinafter, obtaining single-component water-based
Epoxy insulation varnish, solid content 57%, storage stability are 12 months, and film obtains after sixty minutes in 130 DEG C of solidifications in substrate
Paint film.
(4) the performance test results such as table 10
Table 10
Embodiment 6
(1) preparation of active nonionic type emulsifier
By liquid epoxies (E-44) and polyethylene glycol (PEG-600), 1.5:1 is added in reaction kettle in molar ratio, and 80 DEG C
Heating water bath after mixing to reaction system is slowly added dropwise potassium sulfate catalyst (the 5% of epoxy resin quality), drips off
Keep the temperature 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, the epoxide number of every 0.5h detection architecture, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifier.
(2) preparation of active epoxy toughening agent
First cyclobutane -1,2- dicarboxylic acid anhydride is opened according to 1:2 molar ratio at 100 DEG C with polyethylene glycol (PEG-5000)
Ring reacts 4h, when the acid value of detection architecture arrives theoretical value, 2 times of liquid epoxies (E-51) of addition acid anhydrides molal quantity and just
Butylammonium bromide catalyst measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains active toughening in 110 DEG C of reaction 6h
Agent.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 11
Table 11
Preparation step:
By epoxy resin, active nonionic emulsifier, endurable active toughener, curing agent, pigment, filler, fungicide, levelling
Agent, thickener, defoaming agent and deionized water mixing, high-speed stirred 4h, until fineness is less than 20 microns hereinafter, obtaining single-component water-based
Epoxy insulation varnish, solid content 60%, film obtain paint film after solidifying 70 minutes in substrate at 110 DEG C.
(4) the performance test results such as table 12
Table 12
Embodiment 7
(1) preparation of active nonionic type emulsifier
By liquid epoxies (E-35) and polyethylene glycol (PEG-20000), 1.9:1 is added in reaction kettle in molar ratio, and 80
DEG C heating water bath after mixing to reaction system is slowly added dropwise potassium sulfate catalyst (the 5% of epoxy resin quality), drips off
Keep the temperature 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, the epoxide number of every 0.5h detection architecture, when the ring of system
When oxygen value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifier.
(2) preparation of active epoxy toughening agent
It is first that dodecyl succinic anhydride is anti-in 110 DEG C of progress open loops according to 1:2 molar ratio with polyethylene glycol (PEG-300)
It answers 4h, when the acid value of detection architecture is to theoretical value, 1.7 times liquid epoxies (E-35) He Zhengding of acid anhydrides molal quantity is added
Base ammonium bromide catalyst measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains endurable active toughener in 100 DEG C of reaction 4h.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 13
Table 13
Preparation step:
By epoxy resin, active nonionic emulsifier, endurable active toughener, curing agent, pigment, filler, fungicide, levelling
Agent, thickener, defoaming agent and deionized water, high-speed stirred 3h, until fineness is less than 20 microns hereinafter, obtaining single-component water-based epoxy
Insulated paint, solid content 57%, film obtain paint film after solidifying 90 minutes in substrate at 120 DEG C.
(4) the performance test results such as table 14
Table 14
Embodiment 8
(1) preparation of active nonionic type emulsifier
By liquid epoxies (E51) and polyethylene glycol (PEG-18000), 2:1 is added in reaction kettle in molar ratio, and 80 DEG C
Heating water bath after mixing to reaction system is slowly added dropwise potassium sulfate catalyst (the 2% of epoxy resin quality), drips off
Keep the temperature 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, the epoxide number of every 0.5h detection architecture, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifier.
(2) preparation of active epoxy toughening agent
First by glutaric anhydride and polyethylene glycol (PEG-14000) according to 1:2 molar ratio in 120 DEG C of progress ring-opening reaction 3h,
When the acid value of detection architecture is to theoretical value, 1.9 times of the liquid epoxies (E55) and normal-butyl bromination of acid anhydrides molal quantity is added
Ammonium catalyst measures the acid value of resin to 5mgKOH/g hereinafter, cooling obtains endurable active toughener in 110 DEG C of reaction 4h.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 15
Table 15
Preparation step:
By epoxy resin, active nonionic emulsifier, endurable active toughener, curing agent, pigment, filler, fungicide, levelling
Agent, thickener, defoaming agent and deionized water, high-speed stirred 6h, until fineness is less than 20 microns hereinafter, obtaining single-component water-based epoxy
Insulated paint, solid content 52%, film obtain paint film after substrate solidifies 100 minutes at 120 DEG C.
(4) the performance test results such as table 16.
Table 16
The above examples only illustrate the technical idea of the present invention, and this does not limit the scope of protection of the present invention, all
According to technical though proposed by the present invention, any changes made on the basis of the technical scheme each falls within the scope of the present invention
Within.
Claims (10)
1. a kind of water-base epoxy insulated paint, which is characterized in that in terms of mass fraction, raw material components composition are as follows: epoxy resin 15-
25%, active nonionic emulsifier 5-10%, endurable active toughener 5-10%, imidazoles latent curing agent 5-10%, pigments and fillers 15-
20%, auxiliary agent 2-5%, remaining is deionized water；
The active nonionic emulsifier is prepared via a method which: in molar ratio by liquid epoxies and polyethylene glycol
1.5-2.0:1 is added in reaction kettle, 80-85 DEG C of heating water bath, after mixing to reaction system, potassium sulfate catalyst is added dropwise,
Drip off and keep the temperature 0.5-1.0h at 80-85 DEG C, after be warming up to 180-200 DEG C, when the epoxide number of system remains unchanged, cool down out
Material synthesizes water-base epoxy emulsifier；Potassium sulfate catalyst amount is the 2-5% of epoxy resin quality；
The endurable active toughener is prepared via a method which: by aliphatic anhydride and polyethylene glycol according to 1:1.5-2.0 moles
Than in 90-130 DEG C of progress ring-opening reaction 2-4h, when the acid value of detection architecture is to theoretical value, aliphatic anhydride molal quantity is added
The normal-butyl ammonium bromide catalyst of the 3-5% of 1.5-2.0 times of liquid epoxies and aliphatic anhydride molal quantity, in 90-130
DEG C reaction 4-6h, measure the acid value of resin to 5mgKOH/g hereinafter, cooling obtain endurable active toughener.
2. water-base epoxy insulated paint according to claim 1, which is characterized in that the aliphatic anhydride is cis-butenedioic anhydride, fourth
Dicarboxylic anhydride, adipic anhydride, itaconic anhydride, glutaric anhydride, tung oil acid anhydride, dodecyl succinic anhydride, cyclobutanetetracarboxylic acid anhydride, two
Methyl maleic anhydride, 1,1- cyclohexyl maleic anhydride, cyclobutane -1,2- dicarboxylic acid anhydride, pentamethylene -1,1- diethyl acid anhydrides and 2,2-
It is one or more in dimethyl succinic anhydride.
3. water-base epoxy insulated paint according to claim 1, which is characterized in that the liquid epoxies is bisphenol-A
It is one or more in type epoxy resin E55, E51, E44, E42, E39, E35 and E31.
4. water-base epoxy insulated paint according to claim 1, which is characterized in that the molecular weight of the polyethylene glycol is
200,300,400,600,1000,1500,2000,3000,4000,5000,6000,8000,10000,12000,14000,
16000, a kind of and a variety of in 18000 and 20000.
5. water-base epoxy insulated paint according to claim 1, which is characterized in that the epoxy resin is bisphenol-A type ring
Oxygen resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, novolac epoxy resin, glycidyl ester type epoxy resin, alicyclic ring
It is one or more in race's epoxy resin and aliphatic epoxy resin；
Model E12, E20, E42, E-44 or E-51 of the bisphenol A type epoxy resin；
The model CYDF-170 of the bisphenol f type epoxy resin or 6458；
The model 185S or 300SS of the bisphenol-s epoxy resin；
Model JF-45, F-44 or F-51 of the novolac epoxy resin；
The model FA-68 of the glycidyl ester type epoxy resin or 711；
The model ZH68-01 or ZH206 of the cycloaliphatic epoxy resin；
The aliphatic epoxy resin is aliphatic epoxy resin 2000.
6. water-base epoxy insulated paint according to claim 1, which is characterized in that the imidazoles latent curing agent are as follows: 1- benzene
Methyl -2-methylimidazole, 1-cyanoethyl-2-phenylimidazole trimellitic acid salt, 2,4- diamino -6- [2 '-methylimidazolyls -
(1) '] ethyl-S- triazine, 2,4- diamino -6- [2 '-undecylimidazole bases-(1) '] ethyl-S- triazine, 2,4- diamino -6-
[2 '-ethyls -4-methylimidazole base-(1) '] ethyl-S- triazine, 1- dodecyl -2- methyl-3-benzyl imidazole chloride, 1,3-
Dibenzyl -2-methylimidazole chloride or 2 phenyl 4 methyl 5 hydroxy methylimidazole etc. is one or more；
The pigments and fillers are made of pigment and filler, and the mass ratio of pigment and filler is 1:1.5-3.0；Wherein pigment be titanium white,
One of lithopone, iron oxide red, toluidine red, lead chromate yellow, barba hispanica, iron oxide black are a variety of；Filler is calcium carbonate, barium sulfate, silica
It is one or more in ash, talcum powder, alumina powder, silicon nitride powder, mica powder and porous konilite.
7. water-base epoxy insulated paint according to claim 1, which is characterized in that the auxiliary agent includes aqueous defoamer, water
Property levelling agent, water-based thickener and fungicide；
The aqueous defoamer includes organic silicon type defoaming agent BYK-018, polyether-type defoaming agent BYK-019 and polyether-modified silicon type
One of defoaming agent Digao TEGO-810 or a variety of；
The aqueous levelling agent includes in modified polyether class levelling agent TEGO-450 and modified organic silicon class levelling agent BYK-306
It is one or more；
The water-based thickener includes cellulose thickener Natrosol HEC, agent for polyacrylic acid thickening VISCOLAM 330
With it is one or more in the RM-8W of polyurethanes thickener DOW company；
The fungicide includes substituted arene class fungicide pentachloronitrobenzene, heterocycles fungicide methylisothiozoline
One of ketone, aminated compounds class fungicide fenfuram are a variety of.
8. the preparation method of water-base epoxy insulated paint described in claim 1, which is characterized in that by epoxy resin, active nonionic
Emulsifier, endurable active toughener, imidazoles latent curing agent, pigments and fillers, auxiliary agent and deionized water mixing, high-speed stirred 3-5h, until thin
Degree is less than 20 microns hereinafter, obtaining single-component water-based epoxy insulation varnish；Solid content is 50-60wt%.
9. the application of water-base epoxy insulated paint described in claim 1, which is characterized in that by water-base epoxy described in claim 1
Insulated paint spraying or dip-coating in substrate surface, 110-130 DEG C solidification 60-120 minutes.
10. the application of water-base epoxy insulated paint according to claim 9, which is characterized in that the water-base epoxy insulated paint of formation
The storage stability of film is not less than 1 year；Hardness of film is 2H-3H, impact resistance >=50cm, and adhesive force is 0 grade；It is resistance to by 96h
Aqueous test；Insulating properties reaches B-F grades, wherein under volume resistivity normality >=1013Ω m, the normality of continuous method test of boosting
Lower electrical strength >=25MV/m；Under dielectric dissipation factor normality≤1%；It is " electrical that other performances meet GB/T 1981.6-2014
Insulation the 6th part of paint: environment-friendly type aqueous impregnating varnish " standard.
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