CN104788627B - Water-base epoxy/emulsion acrylic resin of core shell structure and its preparation method and application - Google Patents
Water-base epoxy/emulsion acrylic resin of core shell structure and its preparation method and application Download PDFInfo
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Abstract
The invention discloses water-base epoxy/emulsion acrylic resin of a kind of core shell structure and preparation method thereof and it is used as water-base epoxy/amino acrylic baking paint application.By the way that the prepolymer of acrylic monomer and vinyl monomer and modified epoxy are carried out into graft copolymerization under the action of the solvent, then emulsified, obtain the epoxy/acrylic acid amino resin emulsion for the core shell structure that solid content is 20 ~ 30%.Then the component of following mass parts is mixed：Solid content is 100 parts of water-base epoxy/emulsion acrylic resin of 20 ~ 30% core shell structure；90~200 parts of water；90~200 parts of waterborne curing agent；0.01~0.5 part of aqueous promoter, obtains a kind of paint film high mechanical strength, green water-base epoxy/amino acrylic baking paint, and alternative solvent epoxy coatings use as priming paint.The present invention has wide range of applications, circuit coil, PCB suitable for electronic applications, and the protective coating of the metal framework structure such as building automobile.
Description
Technical field
The present invention relates to water-base epoxy/emulsion acrylic resin of a kind of nucleocapsid structure and preparation method thereof and as water
Property epoxy/acrylic acid amino Baking Paint application, belongs to organic chemistry filed.
Background technology
Traditional anti-corrosive paint is mostly solvent type paint, covers alcohol acids, acrylic compounds, phenolic, polyurethanes, ring
The kinds such as oxygen class.However, due to containing substantial amounts of organic solvent in the paint of these types, solvent will be evaporate into greatly in construction
In gas, the health of workmen is harmful to, but also pollutes environment, in recent years, with the continuous enhancing of common people's environmental consciousness, generation
Limitation of the environmental regulation of various countries of boundary to VOC in coating (VOC) content is increasingly strict, coatings industry towards
Low stain, energy-saving direction are developed.So from the consideration of environmental protection and public health, country and the common people it is expected to push away
Enter the Water-borne modification of coating.Water paint is with one of important directions and study hotspot that its environment friendly is always paint development.
Composition epoxy resin is applying because the engineering properties, corrosion resistance, adaptation of resulting solidfied material etc. are excellent
It is widely used in each fields such as material, bonding agent, laminate, electronic unit purposes, and Water-borne modification epoxy resin, conventional method are
Using surfactant, epoxy resin latex is prepared by high-speed stirred, but epoxy resin latex is due to the original of surfactant
Cause, exist poor water resistance, with the problems such as adaptation of base material or upper coated coating is poor, mechanical stability difference.Epoxy/acrylic acid is total to
Polymers both has epoxy resin high mechanical strength, the characteristics of antiseptic property is excellent, have again acrylic resin weather resistance it is excellent,
The advantages of good decorative property, after amino resin crosslinked, hardness and antiseptic property further improve, using it as painting made from base-material
Material has excellent combination property, is expected to be used widely in industries such as building materials, automobile, household electrical appliances, instrument.Develop water-based ring
Oxygen/Acrylic Anticorrosive Coatings can save a large amount of solvents, mitigate environmental pollution, and huge economic benefit and society will be brought to imitate
Benefit.
As the epoxy resin of Water-borne modification, for example, disclosed in Chinese patent CN102675859A using polyglycol ether,
Product obtained from isocyanates reaction.In addition, disclosed in Chinese patent CN102977376A direct using diisocyanate
Performed polymer is made it is further continued for reacting with the pendant hydroxyl group in epoxy resin with the terminal hydroxy group reaction in poly glycol monomethyl ether and is produced
Thing, disclosed in Japanese Patent Laid-Open 2-38443 publications containing epoxy resin more than two functions and polyphenol and by
The condensation product that more than aliphatic polyol and two functions epoxy resin and list and polyisocyanates are formed.However, these materials
Material crosslink density caused by being remained in because of the primary hydroxyl of polyethylene glycol in fraction compositions such as does not improve at the reason, has
The shortcomings that poor water resistance, anticorrosive property are poor, alkali resistance is poor, water dispersible is low, stability of emulsion is poor.
As the water-dispersible epoxy resins for improving these shortcomings, one kind is disclosed in Chinese patent CN103254376A
The preparation method of waterborne epoxy modified polyaminoester emulsion, in UV after Epocryl and urethane acrylate are mixed
Aqueous acrylic modified epoxy ester resin is made in the lower copolymerization of effect.The resin good mechanical performance, but due to the resin point of preparation
Still substantial amounts of ester bond is included in sub- main chain, is easier to hydrolytic cleavage, thus largely limits its extensive use.China
Patent CN102358815A discloses a kind of one-component self-drying acrylic acid grafted epoxy ester water dispersible coatings and preparation method.
The coating has the characteristics that outstanding mechanical performance, water resistance and corrosion resistance, but because the patent system is standby in asphalt mixtures modified by epoxy resin
The molecular weight of fat is relatively low, and obtained paint film flexibility, impact resistance and Corrosion Protection are poor, and brittle fracture easily occurs, only
The relatively low metal surface structure of requirement can be used to use, can not still fully meet high-performance water-based epoxy anticorrosive paint and size
The urgent need of technology.
The content of the invention
The invention aims to eliminate harm of the organic solvent to environment and the mankind, there is provided a kind of green, water
The excellent water-base epoxy baking vanish of dispersiveness and preparation method, and it is further able to access coating strength or corrosion resistance is more excellent consolidates
The water-dispersible epoxy resins of compound and the water-dispersible epoxy resins composition containing the water-dispersible epoxy resins.The present invention
It was found that by importing acrylic acid and vinyl prepolymer on epoxy resin side chain, obtain that there is excellent water dispersible and breast
The aqueous epoxy resins composition of liquid stability, it is possible to increase crosslink density during solidification, obtain water-fast, coating strength and anti-corrosion
Property excellent aqueous epoxy resins composition solidfied material, the baking vanish have paint film high mechanical strength, fast drying, adhesive force it is strong,
Water-acid resistance, it is non-ignitable, storage stability is good, safe and non-toxic, easy to operate the advantages that.Alternative solvent epoxy coatings conduct
Priming paint uses, and can use a variety of method constructions such as brushing, spray, leaching, applied widely.
For the above-mentioned purpose, the invention provides water-base epoxy/emulsion acrylic resin of nucleocapsid structure and its preparation side
Method and conduct water-base epoxy/amino acrylic baking paint application.
A kind of preparation method of water-base epoxy/emulsion acrylic resin of nucleocapsid structure, comprises the following steps：By propylene
The prepolymer of acrylic monomer and vinyl monomer carries out graft copolymerization under the action of the solvent with modified epoxy, so
After emulsified.
Specifically include following steps：
(1) vinyl monomer of 6~20 mass parts and the initiator of 0.1~2 mass parts are added into reactor, is added
Solvent dissolves, and is then well mixed the acrylic monomer of 30~90 mass parts with the polymerization inhibitor of 1~5 mass parts, slowly drop
It is added in reactor, solvent load is 1~5 times of monomer gross mass, and reaction temperature is 70~130 DEG C, condensing reflux, during reaction
Between be 1~5 hour；
(2) modified epoxy is added in the reactor of step (1), in 90~120 DEG C of stirring reactions 1 after being well mixed
~3 hours；Then, reaction system is cooled to 40-70 DEG C, the pH value regulator for adding 5~20 mass parts continues 30 points of stirring
Clock, add the water high-speed stirred of 1~5 times of monomer gross mass, produce solid content be 20~30% nucleocapsid structure epoxy/
Acrylic-amino resin emulsion.
Preferably, described acrylic monomer is acrylic acid, methacrylic acid, methyl methacrylate, acrylic acid second
In ester, butyl acrylate, isobutyl acrylate, butyl methacrylate, Hydroxyethyl Acrylate, hydroxyethyl methacrylate
It is one or more of；Described vinyl monomer is the one or more in styrene, vinyltoluene, α-methylstyrene.
Described initiator is benzoyl peroxide, peroxidized t-butyl perbenzoate, azodiisobutyronitrile and the isobutyric acid diformazan of azo two
One or more in ester；Described polymerization inhibitor be hydroquinones, 1,4-benzoquinone, phenothiazine, beta-phenyl naphthylamines, to tert-butyl o
One or more in benzenediol, 1,1- diphenyl -2- trinitrophenyl-hydrazines, 2,2,6,6- tetramethyl piperidine nitrogen oxygen free radicals；Institute
The solvent stated is n-butanol, isobutanol, propylene glycol monomethyl ether, butyl glycol ether, propandiol butyl ether, glycerine methyl ether, DPG
One or more in butyl ether；Described pH value regulator is ammoniacal liquor, triethylamine, N, one kind or several in N- dimethylethanolamines
Kind；The rotating speed of the high-speed stirred is 3000rpm.
Described modified epoxy is made by following methods：By the epoxy resin of 80~150 mass parts, 16~36 mass
The dibasic acid anhydride of part and the catalyst input reactor of 0.1~1 mass parts carry out ring-opening reaction, and reaction temperature is 90~140 DEG C,
Work as acid number<It is reaction end during 8mg K0H/g；Then, the aliphatic acid of 20~40 mass parts is added, temperature is 80~150 DEG C, cold
Solidifying backflow, reacts 1.5~4 hours, that is, obtains modified epoxy.Described epoxy resin is bisphenol A type epoxy resin, phenolic aldehyde
One or more in epoxy resin, orthoresol formaldehyde epoxy resin, polyol shrinkaging glycerin ether epoxy resin；Described binary
Acid anhydrides is phthalic anhydride, M-phthalic acid, terephthalic acid (TPA), THPA, maleic anhydride, fumaric acid, amber
One or more in amber acid anhydrides；Described catalyst be dimethylethanolamine, diethanol amine, ethylenediamine, dimethyl-ethylenediamine,
One or more in three (2- ethoxys) amine；Described aliphatic acid is capric acid, laurate, myristic acid, stearic acid leukotrienes, castor
One or more in sesame oil acid, palmitoleic acid, eleostearic acid, Chinese catalpa oleic acid, linoleic acid, nisinic acid, lauroleic acid.
Described epoxy resin is the one or more in E-20 epoxy resin, E-12 epoxy resin, E-44 epoxy resin.
A kind of water-base epoxy/emulsion acrylic resin of nucleocapsid structure, is prepared by above-mentioned preparation method.
Application of the water-base epoxy/emulsion acrylic resin of described nucleocapsid structure in paint field.
A kind of water-base epoxy/amino acrylic baking paint, is uniformly mixed so as to obtain by the component of following mass parts：Solid content be 20~
100 parts of water-base epoxy/emulsion acrylic resin of 30% nucleocapsid structure；90~200 parts of water；Waterborne curing agent 90~200
Part；0.01~0.5 part of aqueous promoter.
Preferably：The melmac that described waterborne curing agent is methanol, butanol or isobutyl are etherified, cyanamid dimerization
Methylal resin, the one or more in melamine-urea methylal resin；Described aqueous promoter be aqueous defoamer,
One or more in water-based wetting dispersing agent, aqueous levelling agent.
The present invention has advantages below and beneficial effect：
(1) the epoxy segment by the prolonged action of maleic anhydride so that be available for the hydroxyl of grafting on small molecule epoxy segment
Radix amount increase, while hydroxyl quantity increase be advantageous to improve product Adhering capacity.
(2) grafting copolymerization process is linked the modified epoxy ester resin of preparation in a manner of carbon-carbon bond and effectively overcomes tradition
In water-soluble resin the problem of not hydrolysis caused by ester bond connected mode, epoxy is combined using acrylic acid-grafted epoxy-ester
Ester resin adhesive force is strong, water-fast corrosion resistance is excellent and acrylic resin good film-forming property, the advantages of glossiness is high.
(3) design technology of self-emulsification is employed, the water-soluble acrylic modified epoxy ester resin molecule being grafted can
The epoxy-ester not being grafted is emulsified and provides water solubility by the emulsifying agent for serving as macromolecule, therefore substantially increases the water of resin
Dispersive property and storage stability.
(4) modified epoxy/acrylic resin prepared directly can be diluted with running water, added curing agent and obtained water-based ring
Oxygen/amino acrylic baking paint, it can be dried at 105-115 DEG C in 50-70min, film forming light is smooth, and properties reach
The technical merit of solvent based product.
(5) coating prepared, it is easy to use, suitable for brushing, spraying, a variety of construction means works such as soaking.With appropriate amount
Color stuffing can prepare assorted aqueous self-drying industrial coating, can be widely applied to circuit coil, the PCB of electronic applications,
And the protective coating of the metal framework structure such as building automobile.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
(1) preparation of modified epoxy：By 136.2g E-20 epoxy resin, 22.2g phthalic anhydride and
In 0.41g dimethyl-ethylenediamine input reactor A, stir and be to slowly warm up to 130 DEG C, acid number is detected in course of reaction, when
Acid number<It is reaction end during 8mg K0H/g.Then, add 33g capric acid and be cooled to 120 DEG C and start to be esterified, esterification is protected
Temperature is held as 115-120 DEG C, condensing reflux, reaction stops reaction after 1.5~4 hours.
(2) preparation of the epoxy/acrylic acid amino resin emulsion of nucleocapsid structure：12.5g α-first is added in reactor B
Base styrene monomer and 4.1g benzoyl peroxide (BPO), dissolved with 40g propylene glycol monomethyl ethers, be warming up to 70 DEG C, treat that BPO is complete
Fully dissolved, then 45g acrylic acid, 35g methacrylic acid are well mixed with 0.2g hydroquinones, using the side of dropwise addition
Formula is slowly added into reactor B.90 DEG C are warming up to after being added dropwise, continues reaction 3 hours, by the modification ring in reactor A
Oxygen tree fat is added in reactor B, is reacted 1.5 hours at 110 DEG C after stirring.Then, reaction system is cooled to 55 DEG C, added
The triethylamine for entering 40g stirs 30 minutes, and the water high-speed stirred that 1.5 times of monomer gross mass is added after solvent, rotating speed are taken in decompression away
For 3000rpm, epoxy/acrylic acid amino resin emulsion of the solid content for 20~30% nucleocapsid structure is produced.
(3) preparation of water-base epoxy/amino acrylic baking paint：Take the nucleocapsid structure that above-mentioned solid content is 20~30%
Epoxy/acrylic acid amino resin emulsion 100g, add 10g curing agent, 0.42g wetting agent BYK-346 and 0.21g defoamers
BYK-028, water-base epoxy/amino acrylic baking paint is made after being stirred with adjustable high-speed dispersion machine.
Embodiment 2
(1) preparation of modified epoxy：By 100g E-12 epoxy resin, 31g E-44 epoxy resin, 47g four
Hydrogen phthalic anhydride and 0.3g three (2- ethoxys) amine input reactor A carry out ring-opening reaction, stir and are to slowly warm up to reaction temperature
For 130 DEG C, work as acid number<It is reaction end during 8mg K0H/g.Then, the castor oil acid for adding 28g carries out esterification, reaction 3
Hour, keeping temperature is 105 DEG C.
(2) preparation of the epoxy/acrylic acid amino resin emulsion of nucleocapsid structure：15g styrene is added in reactor B
With 0.9g benzoyl peroxide (BPO), dissolved with 20g propylene glycol monomethyl ethers, be warming up to 70 DEG C, treat that BPO is completely dissolved, then will
60g acrylic acid, 30g methyl methacrylate, 0.15g 1,4-benzoquinone and 20g propylene glycol monomethyl ether are well mixed, using drop
The mode added is slowly added into reactor B.85 DEG C are warming up to after being added dropwise, continues reaction 3 hours, by reactor A
Modified epoxy is added in reactor B, is reacted 3 hours at 110 DEG C after stirring.Then, reaction system is cooled to 55
DEG C, the triethylamine for adding 42g stirs 30 minutes, and the water high-speed stirred that 1.5 times of monomer gross mass is added after solvent is taken in decompression away,
Rotating speed is 3000rpm, produces the epoxy/acrylic acid amino resin emulsion for the nucleocapsid structure that solid content is 20~30%.
(3) preparation of water-base epoxy/amino acrylic baking paint：Take the nucleocapsid structure that above-mentioned solid content is 20~30%
Epoxy/acrylic acid amino resin emulsion 100g, add 10g curing agent, 0.42g wetting agent BYK-346 and 0.21g defoamers
BYK-028, water-base epoxy/amino acrylic baking paint is made after being stirred with adjustable high-speed dispersion machine.
Embodiment 3
(1) preparation of modified epoxy：By 100g E-20 epoxy resin, 31g E-44 epoxy resin, 47g it is suitable
Anhydride maleique and 0.3g ethylenediamine amine input reactor A carry out ring-opening reaction, stir and are to slowly warm up to reaction temperature and are
130 DEG C, work as acid number<It is reaction end during 8mg K0H/g.Then, the oleic acid for adding 28g carries out esterification, reacts 3 hours,
Keeping temperature is 105 DEG C.
(2) preparation of the epoxy/acrylic acid amino resin emulsion of nucleocapsid structure：15g styrene is added in reactor B
With 0.9g benzoyl peroxide (BPO), dissolved with 20g propylene glycol monomethyl ethers, be warming up to 70 DEG C, treat that BPO is completely dissolved, then will
60g acrylic acid, 30g methyl methacrylate, 0.15g 1,4-benzoquinone and 20g propylene glycol monomethyl ether are well mixed, using drop
The mode added is slowly added into reactor B.85 DEG C are warming up to after being added dropwise, continues reaction 3 hours, by reactor A
Modified epoxy is added in reactor B, is reacted 3 hours at 110 DEG C after stirring.Then, reaction system is cooled to 55
DEG C, the triethylamine for adding 42g stirs 30 minutes, and the water high-speed stirred that 1.5 times of monomer gross mass is added after solvent is taken in decompression away,
Rotating speed is 3000rpm, produces the epoxy/acrylic acid amino resin emulsion for the nucleocapsid structure that solid content is 20~30%.
(3) preparation of water-base epoxy/amino acrylic baking paint：Take the nucleocapsid structure that above-mentioned solid content is 20~30%
Epoxy/acrylic acid amino resin emulsion 100g, add 10g curing agent, 0.42g wetting agent BYK-346 and 0.21g defoamers
BYK-028, water-base epoxy/amino acrylic baking paint is made after being stirred with adjustable high-speed dispersion machine.
Performance after 110 DEG C of the film drying 1 hour of above-mentioned prepared water-base epoxy/amino acrylic baking paint is seen below
Table.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. the preparation method of water-base epoxy/emulsion acrylic resin of a kind of nucleocapsid structure, it is characterised in that including following step
Suddenly：
（1）The vinyl monomer of 6 ~ 20 mass parts and the initiator of 0.1 ~ 2 mass parts are added into reactor, it is molten to add solvent
The acrylic monomer of 30 ~ 90 mass parts, is then well mixed, is slowly dropped to reaction by solution with the polymerization inhibitor of 1 ~ 5 mass parts
In kettle, solvent load is 1 ~ 5 times of monomer gross mass, and reaction temperature is 70 ~ 130 DEG C, condensing reflux, and the reaction time is 1 ~ 5 small
When；Described acrylic monomer is acrylic acid, methacrylic acid, methyl methacrylate, ethyl acrylate, acrylic acid fourth
One or more in ester, isobutyl acrylate, butyl methacrylate, Hydroxyethyl Acrylate, hydroxyethyl methacrylate；
Described vinyl monomer is the one or more in styrene, vinyltoluene, α-methylstyrene；
（2）Modified epoxy is added into step（1）Reactor in, be well mixed after it is small in 90 ~ 120 DEG C of stirring reactions 1 ~ 3
When；Then, reaction system is cooled to 40-70 DEG C, the pH value regulator for adding 5 ~ 20 mass parts continues stirring 30 minutes, then adds
Enter the water high-speed stirred of 1 ~ 5 times of monomer gross mass, produce the epoxy/acrylic acid resin for the nucleocapsid structure that solid content is 20 ~ 30%
Emulsion；
Described modified epoxy is made by following methods：By the epoxy resin of 80 ~ 150 mass parts, 16 ~ 36 mass parts two
First acid anhydrides and the catalyst of 0.1 ~ 1 mass parts input reactor carry out ring-opening reaction, and reaction temperature is 90 ~ 140 DEG C, works as acid number<
It is reaction end during 8mg KOH/g；Then, the aliphatic acid of 20 ~ 40 mass parts is added, temperature is 80 ~ 150 DEG C, condensing reflux, instead
Answer 1.5 ~ 4 hours, that is, obtain modified epoxy.
2. the preparation method of water-base epoxy/emulsion acrylic resin of nucleocapsid structure according to claim 1, its feature
It is：Described initiator is benzoyl peroxide, peroxidized t-butyl perbenzoate, azodiisobutyronitrile and the isobutyric acid of azo two
One or more in dimethyl ester；Described polymerization inhibitor be hydroquinones, 1,4-benzoquinone, phenothiazine, beta-phenyl naphthylamines, to tertiary fourth
Base catechol, 1,1- diphenyl -2- trinitrophenyl-hydrazines, one kind in 2,2,6,6- tetramethyl piperidine nitrogen oxygen free radicals or several
Kind；Described solvent is n-butanol, isobutanol, propylene glycol monomethyl ether, butyl glycol ether, propandiol butyl ether, glycerine methyl ether, dipropyl
One or more in glycol butyl ether；Described pH value regulator is ammoniacal liquor, triethylamine, N, one in N- dimethylethanolamines
Kind is several；The rotating speed of the high-speed stirred is 3000 rpm.
3. the preparation method of water-base epoxy/emulsion acrylic resin of nucleocapsid structure according to claim 1, its feature
It is：Described epoxy resin is bisphenol A type epoxy resin, novolac epoxy resin, orthoresol formaldehyde epoxy resin, polyalcohol contracting
One or more in water glycerin ether epoxy resin；Described dibasic acid anhydride is phthalic anhydride, THPA, maleic two
One or more in acid anhydrides, succinic anhydride；Described catalyst is dimethylethanolamine, diethanol amine, ethylenediamine, dimethyl
One or more in ethylenediamine, three (2- ethoxys) amine；Described aliphatic acid is capric acid, laurate, myristic acid, stearic acid Asia
One or more in numb acid, castor oil acid, palmitoleic acid, eleostearic acid, Chinese catalpa oleic acid, linoleic acid, nisinic acid, lauroleic acid.
4. the preparation method of water-base epoxy/emulsion acrylic resin of nucleocapsid structure according to claim 3, its feature
It is：Described epoxy resin is the one or more in E-20 epoxy resin, E-12 epoxy resin, E-44 epoxy resin.
A kind of 5. water-base epoxy/emulsion acrylic resin of nucleocapsid structure, it is characterised in that：By any one of claim 1-4 institutes
The preparation method stated is prepared.
6. water-base epoxy/emulsion acrylic resin of the nucleocapsid structure described in claim 5 is in the application of paint field.
7. a kind of water-base epoxy/amino acrylic baking paint, it is characterised in that be uniformly mixed so as to obtain by the component of following mass parts：Power
Profit requires 100 parts of the water-base epoxy/emulsion acrylic resin for the nucleocapsid structure that the solid content described in 1 is 20 ~ 30%；Water 90~
200 parts；90~200 parts of waterborne curing agent；0.01~0.5 part of aqueous promoter；Described waterborne curing agent is methanol, butanol or different
The melmac of butanol etherification, cyanamid dimerization methylal resin, one kind or several in melamine-urea methylal resin
Kind；Described aqueous promoter is the one or more in aqueous defoamer, water-based wetting dispersing agent, aqueous levelling agent.
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| CN107793539B (en) * | 2017-09-18 | 2021-06-15 | 苏州吉人高新材料股份有限公司 | Aqueous dispersion of acrylic acid copolymerized epoxy ester and preparation method thereof |
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