CN107523179A - A kind of water-base epoxy insulated paint and preparation method and application - Google Patents
A kind of water-base epoxy insulated paint and preparation method and application Download PDFInfo
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- CN107523179A CN107523179A CN201710601451.4A CN201710601451A CN107523179A CN 107523179 A CN107523179 A CN 107523179A CN 201710601451 A CN201710601451 A CN 201710601451A CN 107523179 A CN107523179 A CN 107523179A
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2003/2237—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 answering.The preparation method is that first prepared by polyethylene glycol and liquid epoxies reaction into active nonionic type emulsifying agent；Aliphatic anhydride and polyethylene glycol ring-opening reaction are generated into half ester again, then endurable active toughener is prepared with liquid epoxies reaction；Then active nonionic type emulsifying agent, endurable active toughener are mixed with epoxy resin, imidazoles latent curing agent, deionized water and color stuffing, it is scattered at a high speed to prepare single-component water-based epoxy insulation varnish.The insulated paint overcomes the curing reaction that most of water emulsifier and toughener are not involved in epoxy resin, it can migrate in the curing process to film coated surface, make film it is tacky, it is soaked after the shortcomings that easily turning white, 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 paint, and in particular to a kind of water-base epoxy insulated paint and preparation method and application；
The water-base epoxy insulated paint function admirable, stable storing, there are excellent hardness and chemical resistance, can be widely applied to wood
The fields such as device, automobile, building.
Background technology
Epoxy resin has the advantages that adhesive force is high, chemical resistance is good, wearability is good and good insulation preformance, in insulated paint
Field is widely applied.Conventional epoxy resin insulating varnish is mostly solvent based coating, is existed containing more than 50% organic solvent
It is discharged into production and work progress in air, 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 difficulty such as subpackage dress and construction inconvenience.
The preparation of aqueous epoxy resins mainly uses two kinds of self-emulsification and outer emulsion process, and wherein self-emulsification is frequently with change
Method introduces hydrophilic radical in asphalt mixtures modified by epoxy resin fat chain, is neutralized through acid or alkali into salt, and adds water emulsification to be prepared.Prepared by the method
Aqueous epoxy resins are without additional emulsifying agent, 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 reduce its mechanical performance.
Outer emulsion process makes epoxy resin be uniformly dispersed in water by additional emulsifying agent, and the method has preparation technology simple
Singly, low cost and other advantages, the main method of water-borne modification of epoxy resin is turned into.Epoxy emulsion bin stability and film performance be present
The shortcomings of bad, is, it is necessary to further perfect.The key that outer emulsion process prepares epoxy emulsion is the selection of emulsifying agent, commonly uses emulsifying agent
There are OP-10, SP-60, neopelex etc..Wherein nonionic emulsifier such as OP-10 is due to by ion concentration, pH value
It is smaller Deng influence, be not in demulsification phenomena such as good with other water-base resin compatibilities, turn into the first choice of emulsion epoxy resin.
Nonionic emulsifier is typically reacted by hydrophobic compound such as nonyl phenol and hydrophilic compounds such as polyethylene glycol to be made.But this
Class emulsifying agent is not involved in the curing reaction of epoxy, can migrate to film coated surface in the curing process, makes film tacky, easy after soaked
Turn white, reduce the water resistance and chemical resistance of film.
Epoxy resin film is firmly crisp, and not impact resistance is, it is necessary to add the impact flexibility that toughener improves film.Common plasticizers
To improve impact flexibility, plasticizer does not react in film forming procedure with curing agent, and film can be slow after using a period of time
Separate out, be that film coated surface is tacky, film becomes fragile, and shortens the service life of film.
The content of the invention
Present invention aims to overcome that the problem of prior art is present, there is provided a kind of environmental protection, one-component, medium temperature are quickly solid
Change, high-performance water-based epoxy emulsion insulated paint and preparation method thereof.
Another object of the present invention is the application for providing the aqueous epoxy emulsion insulated paint.
The present invention is prepared a kind of new by synthesizing activity emulsifying agent and endurable active toughener, preferably latent curing agent
High-performance water-based epoxy emulsion insulated paint.
The present invention solves the defects of outer emulsion process using active emulsifier, and so-called active emulsifier refers to polyethylene glycol
Be grafted to etc. non-ionic hydrophilic group 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 emulsifying agent, 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, its raw material components composition is：Epoxy resin 15-25%, activity
Nonionic emulsifier 5-10%, endurable active toughener 5-10%, imidazoles latent curing agent 5-10%, color stuffing 15-20%, auxiliary agent 2-
5%, remaining is deionized water；
Described active nonionic emulsifying agent is prepared via a method which：By liquid epoxies and polyethylene glycol by mole
Compare 1.5-2.0:1 adds in reactor, 80-85 DEG C of heating water bath, and after question response system is well mixed, potassium sulfate catalysis is added dropwise
Agent, drip off and be incubated 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 emulsifying agent；Potassium sulfate catalyst amount is the 2-5% of epoxy resin quality；
Described endurable active toughener is prepared via a method which：By aliphatic anhydride and polyethylene glycol according to 1：1.5-2.0
Mol ratio carries out ring-opening reaction 2-4h at 90-130 DEG C, when the acid number of detection architecture is to theoretical value, adds aliphatic anhydride mole
1.5-2.0 times several of liquid epoxies and the 3-5% of aliphatic anhydride molal quantity normal-butyl ammonium bromide catalyst,
90-130 DEG C of reaction 4-6h, acid number to below 5mgKOH/g, the cooling for determining resin obtain endurable active toughener；
Further to realize the object of the invention, it is preferable that described 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 anhydrides, pentamethylene -1,1- diethyls acid anhydrides and 2,2- dimethyl succinates
It is one or more in acid anhydride.
Preferably, described 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 described 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, described epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol S type epoxy tree
In fat, 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 is：1- benzyls -2-methylimidazole, 1-cyanoethyl-2-phenylimidazole are inclined
Trimellitate, 2,4- diaminourea -6- [2 '-methylimidazolyl-(1) '] ethyl-S- triazines, 2,4- diaminourea -6- [2 '-hendecyls
Imidazole radicals-(1) '] ethyl-S- triazines, 2,4- diaminourea -6- [2 '-ethyl -4-methylimidazole base-(1) '] ethyl-S- triazines,
1- dodecyl -2- methyl-3-benzyl imidazoles chloride, 1,3- dibenzyl -2-methylimidazole chloride or 2- phenyl -4- methyl -
The one or more such as 5- hydroxy methylimidazoles；
The color stuffing is made up of pigment and filler, and the mass ratio of pigment and filler is 1:1.5-3.0；Wherein pigment is titanium
In vain, the one or more in lithopone, iron oxide red, toluidine red, lead chromate yellow, barba hispanica, iron oxide black；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 bactericide；
The aqueous defoamer includes organic silicon type defoamer BYK-018, polyether-type defoamer BYK-019 and polyether-modified
One or more in the high TEGO-810 of silicon type defoamer enlightening；
The aqueous levelling agent includes modified polyether class levelling agent TEGO-450 and modified organic silicon class levelling agent BYK-306
In one or more；
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 companies；
The bactericide includes substituted arene series bactericidal agent pentachloronitrobenzene, heterocyclic compound series bactericidal agent methyl-isothiazol
One or more in quinoline ketone, aminated compounds series bactericidal agent fenfuram.
The preparation method of the water-base epoxy insulation paint film：By epoxy resin, active nonionic emulsifying agent, active toughness reinforcing
Agent, imidazoles latent curing agent, color stuffing, auxiliary agent and deionized water mixing, high-speed stirred 3-5h, to fineness be less than 20 microns with
Under, obtain single-component water-based epoxy insulation varnish；Solids content is 50-60wt%.
The application of the water-base epoxy insulated paint：By described water-base epoxy insulated paint spraying or dip-coating in substrate surface,
Solidify 60-120 minutes at 110-130 DEG C.The bin stability of the water-base epoxy insulation paint film of formation is not less than 1 year；Film is hard
It is 0 grade to spend for 2H-3H, impact resistance >=50cm, adhesive force；Pass through 96h water resistance tests；Insulating properties reaches B-F levels, 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《Electric insulation the 6th part of paint：Environment-friendly type aqueous dipping
Paint》Standard.
The technical principle of the present invention is as follows：
1) preparation of reactive nonionic emulsion agent：
Prepared by polyethylene glycol (nonionic emulsifier) and the liquid epoxies reaction of suitable molecular weight with conjunction
The high-efficiency activated emulsifying agent of suitable HLB value, its end group are the epoxy radicals that can participate in reaction, and the emulsifying agent can effectively reduce 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
Epoxy radicals is introduced on product end group with liquid epoxies reaction, contains a certain amount of flexible base on the product molecule chain of preparation
Group or resin, the toughness after epoxy resin cure is improved, improve the shortcomings of really up to the mark and excessively crisp after pure epoxy resin solidifies.
Compared to prior art, the present invention has advantages below：
1) present invention is prepared with suitable HLB value by the polyethylene glycol and epoxy resin reaction for selecting suitable molecular weight
High-efficiency activated emulsifying agent, effectively reduce 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 active toughness reinforcing is prepared with liquid epoxies reaction
Agent, the toughness after epoxy resin cure is improved, improve the shortcomings of really up to the mark and excessively crisp after pure epoxy resin solidifies；Overcome major part
Emulsifying agent is not involved in the curing reaction of epoxy with toughener, can migrate to film coated surface in the curing process, make film tacky, steeps
The shortcomings that easily turning white after water, greatly prolong painting membrane lifetime.
3) active nonionic type emulsifying agent all has prepared by liquid epoxies with endurable active toughener, because having with epoxy resin
There is similar structure, they have preferable compatibility with main body epoxy resin, can guarantee that the film of preparation and have outside preferably
Sight and physical and mechanical properties；Another active nonionic type emulsifying agent cooperates 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, without small molecule hydrophilic substance or hydrophilic group
Group, water resistance, the chemical resistance of film can be improved, moreover it is possible to greatly prolong the service life of film；
4) the invention belongs to non-ion aqueous emulsion painting, it is not necessary to neutralize into salt treatment, reduce to metallic substrates
Corrosion, insulated paint is insensitive to pH, improves the stability of storage.
Embodiment
To more fully understand the present invention, with reference to embodiment the present invention will be further described, it is necessary to explanation,
Embodiment does not form limiting the scope of the present invention.The relevant method for testing performance being related in embodiment is as follows：
According to national standard《The measure of GB/T 4612-2008 plastics epoxide epoxide equivalents》In assay method detection
The epoxide number of reaction system, detect 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-
2016th, GB/T6753-1986 test respectively the solid content of coating, viscosity, glossiness, pencil hardness, impact strength, adhesive force,
Insulating properties, water absorption rate, acid number and bin stability, the advanced drawing pencil that pencil produces for Shanghai China Pencil Factory No.1, 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 emulsifying agent
By liquid epoxies (E-55) and polyethylene glycol (PEG-2000) in molar ratio 1.5:1 adds in reactor, and 80
DEG C heating water bath, after question response system is well mixed, potassium sulfate catalyst (the 3% of epoxy resin quality) is slowly added dropwise, drips off
Be incubated 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, per the epoxide number of 0.5h detection architectures, when the ring of system
When oxygen value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifying agent.
(2) preparation of active epoxy toughening agent
First by cis-butenedioic anhydride and polyethylene glycol (PFG-10000) according to 1：2 mol ratios carry out ring-opening reaction 2h, detection at 110 DEG C
When the acid number 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 are added
Catalyst, 4h is reacted at 120 DEG C, acid number to below 5mgKOH/g, the cooling for determining resin obtains endurable active toughener.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 1
Table 1
Preparation process：
By epoxy resin, active nonionic emulsifying agent, endurable active toughener, curing agent, pigment, filler, bactericide, levelling
Agent, thickener, defoamer and deionized water mixing, high-speed stirred 3h, are less than less than 20 microns to fineness, obtain single-component water-based
Epoxy insulation varnish, solid content 60%, bin stability are 12 months, and film obtains after solidifying 60 minutes in 130 DEG C in substrate
Paint film.
(4) performance test, respectively prepared by water-base epoxy the insulated paint ISOPOXYR-771 and Wen Hong standby with BACK company systems
Solvent type epoxy insulated paint varnish JG-16-2 performances be compared, it is 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
In the case of substantially equivalent, insulating properties performance is excellent, and glossiness is high, the advantages such as VOC emission is low, Environmental Safety, reduces pair
The pollution of air, ample resources is saved, meets the requirement of sustainable development.Compared with water-based insulating paint on the market, the present invention
In solid content, bin 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 that the storage of water-base epoxy insulated paint is stable, storage period is again
More than 1 year, the solidification of epoxy resin is may also participate in, effectively reduces product cut size and particle diameter distribution, improves 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 emulsification
Agent participates in the curing reaction of epoxy with toughener, is greatly prolonged so that applying membrane lifetime.On the other hand the present invention is by acid anhydrides
Half ester is produced with polyethylene glycol ring-opening reaction, then endurable active toughener is prepared with liquid epoxies reaction, epoxy resin is improved and consolidates
Toughness after change, improve the mechanical performance after epoxy resin cure.
Embodiment 2
(1) preparation of active nonionic type emulsifying agent
By liquid epoxies (E-51) and polyethylene glycol (PEG-400) in molar ratio 1.6:1 adds in reactor, 85 DEG C
Heating water bath, after question response system is well mixed, potassium sulfate catalyst (the 2% of epoxy resin quality) is slowly added dropwise, drips off
Be incubated 1.0h at 85 DEG C, after be warming up to 200 DEG C, after reaction 4 hours, per the epoxide number of 0.5h detection architectures, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifying agent.
(2) preparation of active epoxy toughening agent
First by maleic anhydride and polyethylene glycol (PEG-6000) according to 1：1.5 mol ratios carry out ring-opening reaction 4h at 90 DEG C,
When the acid number 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 are added
Change ammonium catalyst, react 5h at 130 DEG C, acid number to below 5mgKOH/g, the cooling for determining resin obtains endurable active toughener.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 3
Table 3
Preparation process：
By epoxy resin, active nonionic emulsifying agent, endurable active toughener, curing agent, pigment, filler, bactericide, levelling
Agent, thickener, defoamer and deionized water mixing, high-speed stirred 4h, are less than less than 20 microns to fineness, obtain single-component water-based
Epoxy insulation varnish, solid content 51%, film obtain paint film after solidifying 120 minutes at 110 DEG C in substrate.
(4) the performance test results such as table 4
Table 4
Embodiment 3
(1) preparation of active nonionic type emulsifying agent
By liquid epoxies (E-31) and polyethylene glycol (PEG-10000) in molar ratio 2.0:1 adds in reactor, and 82
DEG C heating water bath, after question response system is well mixed, potassium sulfate catalyst (the 5% of epoxy resin quality) is slowly added dropwise, drips off
Be incubated 0.5h at 82 DEG C, after be warming up to 190 DEG C, after reaction 4 hours, per the epoxide number of 0.5h detection architectures, when the ring of system
When oxygen value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifying agent.
(2) preparation of active epoxy toughening agent
First by itaconic anhydride and polyethylene glycol (PEG-4000) according to 1：1.8 mol ratios carry out ring-opening reaction 3h at 100 DEG C,
When the acid number 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 are added
Change ammonium catalyst, react 4h at 120 DEG C, acid number to below 5mgKOH/g, the cooling for determining resin obtains endurable active toughener.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 5
Table 5
Preparation process：
By epoxy resin, active nonionic emulsifying agent, endurable active toughener, curing agent, pigment, filler, bactericide, levelling
Agent, thickener, defoamer and deionized water, high-speed stirred 4h, it is less than less than 20 microns to fineness, obtains single-component water-based epoxy
Insulated paint, solid content 55%, film obtain paint film after solidifying 80 minutes at 120 DEG C in substrate.
(4) the performance test results such as table 6
Table 6
Embodiment 4
(1) preparation of active nonionic type emulsifying agent
By liquid epoxies (E42) and polyethylene glycol (PEG-16000) in molar ratio 2:1 adds in reactor, 80 DEG C
Heating water bath, after question response system is well mixed, potassium sulfate catalyst (the 5% of epoxy resin quality) is slowly added dropwise, drips off
Be incubated 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, per the epoxide number of 0.5h detection architectures, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifying agent.
(2) preparation of active epoxy toughening agent
First by tung oil acid anhydride and polyethylene glycol (PEG-6000) according to 1：2 mol ratios carry out ring-opening reaction 2h, inspection at 130 DEG C
When the acid number 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 are added
Catalyst, 4h is reacted at 110 DEG C, acid number to below 5mgKOH/g, the cooling for determining resin obtains endurable active toughener.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 7
Table 7
Preparation process：
By epoxy resin, active nonionic emulsifying agent, endurable active toughener, curing agent, pigment, filler, bactericide, levelling
Agent, thickener, defoamer and deionized water, high-speed stirred 4h, it is less than less than 20 microns to fineness, obtains 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 emulsifying agent
By liquid epoxies (E-39) and polyethylene glycol (PEG-200) in molar ratio 1.5:1 adds in reactor, 80 DEG C
Heating water bath, after question response system is well mixed, potassium sulfate catalyst (the 4% of epoxy resin quality) is slowly added dropwise, drips off
Be incubated 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, per the epoxide number of 0.5h detection architectures, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifying agent.
(2) preparation of active epoxy toughening agent
First by 2,2- dimethyl succinic anhydrides and polyethylene glycol (PFG-12000) according to 1：2 mol ratios are opened at 110 DEG C
Ring react 2h, when the acid number of detection architecture is to theoretical value, addition acid anhydrides molal quantity 1.6 times of liquid epoxies (E-42) and
Normal-butyl ammonium bromide catalyst, 4h is reacted at 100 DEG C, acid number to below 5mgKOH/g, the cooling for determining resin obtains active increasing
Tough dose.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 9
Table 9
Preparation process：
By epoxy resin, active nonionic emulsifying agent, endurable active toughener, curing agent, pigment, filler, bactericide, levelling
Agent, thickener, defoamer and deionized water mixing, high-speed stirred 4h, are less than less than 20 microns to fineness, obtain single-component water-based
Epoxy insulation varnish, solid content 57%, bin stability are 12 months, and film obtains after solidifying 60 minutes in 130 DEG C in substrate
Paint film.
(4) the performance test results such as table 10
Table 10
Embodiment 6
(1) preparation of active nonionic type emulsifying agent
By liquid epoxies (E-44) and polyethylene glycol (PEG-600) in molar ratio 1.5:1 adds in reactor, 80 DEG C
Heating water bath, after question response system is well mixed, potassium sulfate catalyst (the 5% of epoxy resin quality) is slowly added dropwise, drips off
Be incubated 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, per the epoxide number of 0.5h detection architectures, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifying agent.
(2) preparation of active epoxy toughening agent
First by cyclobutane -1,2- dicarboxylic acid anhydrides and polyethylene glycol (PEG-5000) according to 1：2 mol ratios are opened at 100 DEG C
Ring reacts 4h, when the acid number of detection architecture is to theoretical value, 2 times of the liquid epoxies (E-51) and just of addition acid anhydrides molal quantity
Butylammonium bromide catalyst, 6h is reacted at 110 DEG C, acid number to below 5mgKOH/g, the cooling for determining resin obtains active toughness reinforcing
Agent.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 11
Table 11
Preparation process：
By epoxy resin, active nonionic emulsifying agent, endurable active toughener, curing agent, pigment, filler, bactericide, levelling
Agent, thickener, defoamer and deionized water mixing, high-speed stirred 4h, are less than less than 20 microns to fineness, obtain single-component water-based
Epoxy insulation varnish, solid content 60%, film obtain paint film after solidifying 70 minutes at 110 DEG C in substrate.
(4) the performance test results such as table 12
Table 12
Embodiment 7
(1) preparation of active nonionic type emulsifying agent
By liquid epoxies (E-35) and polyethylene glycol (PEG-20000) in molar ratio 1.9:1 adds in reactor, and 80
DEG C heating water bath, after question response system is well mixed, potassium sulfate catalyst (the 5% of epoxy resin quality) is slowly added dropwise, drips off
Be incubated 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, per the epoxide number of 0.5h detection architectures, when the ring of system
When oxygen value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifying agent.
(2) preparation of active epoxy toughening agent
First by dodecyl succinic anhydride and polyethylene glycol (PEG-300) according to 1：2 mol ratios are anti-in 110 DEG C of progress open loops
4h is answered, when the acid number of detection architecture is to theoretical value, adds 1.7 times of liquid epoxies (E-35) of acid anhydrides molal quantity and positive fourth
Base ammonium bromide catalyst, 4h is reacted at 100 DEG C, acid number to below 5mgKOH/g, the cooling for determining resin obtains endurable active toughener.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 13
Table 13
Preparation process：
By epoxy resin, active nonionic emulsifying agent, endurable active toughener, curing agent, pigment, filler, bactericide, levelling
Agent, thickener, defoamer and deionized water, high-speed stirred 3h, it is less than less than 20 microns to fineness, obtains single-component water-based epoxy
Insulated paint, solid content 57%, film obtain paint film after solidifying 90 minutes at 120 DEG C in substrate.
(4) the performance test results such as table 14
Table 14
Embodiment 8
(1) preparation of active nonionic type emulsifying agent
By liquid epoxies (E51) and polyethylene glycol (PEG-18000) in molar ratio 2:1 adds in reactor, 80 DEG C
Heating water bath, after question response system is well mixed, potassium sulfate catalyst (the 2% of epoxy resin quality) is slowly added dropwise, drips off
Be incubated 0.5h at 80 DEG C, after be warming up to 180 DEG C, after reaction 4 hours, per the epoxide number of 0.5h detection architectures, when the epoxy of system
When value remains unchanged, cooling discharge synthesizes water-base epoxy emulsifying agent.
(2) preparation of active epoxy toughening agent
First by glutaric anhydride and polyethylene glycol (PEG-14000) according to 1：2 mol ratios carry out ring-opening reaction 3h at 120 DEG C,
When the acid number of detection architecture is to theoretical value, 1.9 times of the liquid epoxies (E55) and normal-butyl bromination of acid anhydrides molal quantity are added
Ammonium catalyst, 4h is reacted at 110 DEG C, acid number to below 5mgKOH/g, the cooling for determining resin obtains endurable active toughener.
(3) preparation of water-base epoxy insulated paint
Raw material such as table 15
Table 15
Preparation process：
By epoxy resin, active nonionic emulsifying agent, endurable active toughener, curing agent, pigment, filler, bactericide, levelling
Agent, thickener, defoamer and deionized water, high-speed stirred 6h, it is less than less than 20 microns to fineness, obtains 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 technological thought of above example only to illustrate the invention, it is impossible to protection scope of the present invention is limited with this, it is every
According to technical though proposed by the present invention, any change done on the basis of technical scheme, the scope of the present invention is each fallen within
Within.
Claims (10)
1. a kind of water-base epoxy insulated paint, it is characterised in that in terms of mass fraction, its raw material components composition is：Epoxy resin 15-
25%th, active nonionic emulsifying agent 5-10%, endurable active toughener 5-10%, imidazoles latent curing agent 5-10%, color stuffing 15-
20%th, auxiliary agent 2-5%, remaining is deionized water；
Described active nonionic emulsifying agent is prepared via a method which：By liquid epoxies and polyethylene glycol in molar ratio
1.5-2.0:1 adds in reactor, 80-85 DEG C of heating water bath, and after question response system is well mixed, potassium sulfate catalyst is added dropwise,
Drip off and be incubated 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 and
Material, synthesize water-base epoxy emulsifying agent；Potassium sulfate catalyst amount is the 2-5% of epoxy resin quality；
Described endurable active toughener is prepared via a method which：By aliphatic anhydride and polyethylene glycol according to 1：1.5-2.0 mole
Than carrying out ring-opening reaction 2-4h at 90-130 DEG C, when the acid number of detection architecture is to theoretical value, aliphatic anhydride molal quantity is added
The normal-butyl ammonium bromide catalyst of 1.5-2.0 times of liquid epoxies and the 3-5% of aliphatic anhydride molal quantity, in 90-130
DEG C reaction 4-6h, determines the acid number of resin to below 5mgKOH/g, cooling and obtains endurable active toughener.
2. water-base epoxy insulated paint according to claim 1, it is characterised in that described 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 anhydrides, pentamethylene -1,1- diethyls acid anhydrides and 2,2-
It is one or more in dimethyl succinic anhydride.
3. water-base epoxy insulated paint according to claim 1, it is characterised in that described 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, it is characterised in that the molecular weight of described polyethylene glycol is
200th, 300,400,600,1000,1500,2000,3000,4000,5000,6000,8000,10000,12000,14000,
16000th, it is a kind of and a variety of in 18000 and 20000.
5. water-base epoxy insulated paint according to claim 1, it is characterised in that described epoxy resin is bisphenol-A type ring
Oxygen tree fat, 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 ring race epoxy resin；
The aliphatic epoxy resin is aliphatic epoxy resin 2000.
6. water-base epoxy insulated paint according to claim 1, it is characterised in that the imidazoles latent curing agent is：1- benzene
Methyl -2-methylimidazole, 1-cyanoethyl-2-phenylimidazole trimellitic acid salt, 2,4- diaminourea -6- [2 '-methylimidazolyl -
(1) '] ethyl-S- triazines, 2,4- diaminourea -6- [2 '-undecylimidazole base-(1) '] ethyl-S- triazines, 2,4- diaminourea -6-
[2 '-ethyl -4-methylimidazole base-(1) '] ethyl-S- triazines, 1- dodecyl -2- methyl-3-benzyl imidazoles chloride, 1,3-
Dibenzyl-the one or more such as 2-methylimidazole chloride or 2 phenyl 4 methyl 5 hydroxy methylimidazole；
The color stuffing is made up of pigment and filler, and the mass ratio of pigment and filler is 1:1.5-3.0；Wherein pigment be titanium white,
One or more in lithopone, iron oxide red, toluidine red, lead chromate yellow, barba hispanica, iron oxide black；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, it is characterised in that the auxiliary agent includes aqueous defoamer, water
Property levelling agent, water-based thickener and bactericide；
The aqueous defoamer includes organic silicon type defoamer BYK-018, polyether-type defoamer BYK-019 and polyether-modified silicon type
One or more in the high TEGO-810 of defoamer enlightening；
The aqueous levelling agent is included 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 one or more in the RM-8W of polyurethanes thickener DOW companies；
The bactericide includes substituted arene series bactericidal agent pentachloronitrobenzene, heterocyclic compound series bactericidal agent methylisothiozoline
One or more in ketone, aminated compounds series bactericidal agent fenfuram.
8. described in claim 1 water-base epoxy insulation paint film preparation method, it is characterised in that by epoxy resin, activity it is non-from
Sub- emulsifying agent, endurable active toughener, imidazoles latent curing agent, color stuffing, auxiliary agent and deionized water mixing, high-speed stirred 3-5h, extremely
Fineness is less than less than 20 microns, obtains single-component water-based epoxy insulation varnish；Solids content is 50-60wt%.
9. the application of water-base epoxy insulated paint described in claim 1, it is characterised in that by the water-base epoxy described in claim 1
Insulated paint sprays or dip-coating is in substrate surface, solidifies 60-120 minutes at 110-130 DEG C.
10. the application of water-base epoxy insulated paint according to claim 9, it is characterised in that the water-base epoxy insulated paint of formation
The bin 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
Water-based test；Insulating properties reaches B-F levels, wherein under specific insulation normality >=1013Ω m, the normality of continuous method test of boosting
Lower electrical strength >=25MV/m；Under dielectric dissipation factor normality≤1%；Other performances meet GB/T 1981.6-2014《Electrically
Insulation the 6th part of paint：Environment-friendly type aqueous impregnating varnish》Standard.
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