CN108424680A - A kind of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection and preparation method - Google Patents
A kind of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection and preparation method Download PDFInfo
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- CN108424680A CN108424680A CN201810266209.0A CN201810266209A CN108424680A CN 108424680 A CN108424680 A CN 108424680A CN 201810266209 A CN201810266209 A CN 201810266209A CN 108424680 A CN108424680 A CN 108424680A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4407—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained by polymerisation reactions involving only carbon-to-carbon unsaturated bonds
- C09D5/4411—Homopolymers or copolymers of acrylates or methacrylates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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Abstract
The invention discloses a kind of formulas of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection, include the raw material of following parts by weight：15~25 parts of acrylic resin, 0.3~1 part of neutralizer, 0.1~0.2 part of environment-friendly type catalyst, 0.1~0.5 part of coalescents, 1~2 part of mill base, 60~70 parts of deionized water；The synthesis material of the acrylic resin includes：Monomer, initiator and solvent, the initiator include：1~3 part of azodiisobutyronitrile, the solvent include：One or more of isopropanol, ethylene glycol ethyl ether, butyl glycol ether, ethyl acetate, butyl acetate, ethyl cellosolve acetate；The environment-friendly type catalyst includes：One or two kinds of compounding in isooctyl acid bismuth, aphthenic acids yttrium.The present invention also provides a kind of preparation methods, can prepare high glaze, and hardness and film thickness can reach the cathode electrodip painting of user demand, can effectively reduce the VOC in coating, alleviate load of the coating to environment.
Description
Technical field
The present invention relates to cathode electrodip painting technical field more particularly to a kind of high-performance self-crosslinking acrylic resin environment-friendly types
Cathode electrodip painting and preparation method.
Background technology
With the development of society, requirement of the countries in the world for volatile organic matter (VOC) is increasingly stringenter, water paint
It the advantages that with its asepsis environment-protecting, odorlessness, low, nonflammable explosive VOC content, is widely used.Wherein, electrophoretic coating
By its adhesive force is good, hardness is high, wearability is strong, chemical resistance is good and impact resistance is excellent, have been widely used in each neck
In domain, and develop into a very important kind in paint field.
In electrophoretic coating, cathode electrophoresis dope compared to anode electrophoresis dope, with its very excellent corrosion resistance,
High throwing power and coulombic efficiency is widely used.Especially in high-decoration field.Currently, acrylic resin is cloudy
Pole electrophoretic coating mainly introduces the function monomer with certain functional group (such as hydroxyl) in matrix resin, and in strand
Isocyanates progress crosslinking curing is added in upper introducing amino during painting.The thermoset acrylics ability cathode electrophoresis of external crosslinking
Paint is with superior richness, high rigidity, high glaze, solvent resistance, weatherability.And the acrylic CED paint of self-crosslinking by
It is not mature enough in the development of its production technology, in gloss, film thickness, hardness etc., some aspect of performance may be not met by related use
The requirement at family.Meanwhile currently, in cathode electrophoresis dope, most widely employed is organic tin catalyst, such catalyst
It is toxic, has certain harm for the health of production and construction personnel and affect to environment.
Invention content
The purpose of the present invention is to solve there are glossiness in prior art preparation self-crosslinking acrylic resin inadequate, films
Thick, hardness cannot meet the shortcomings that the needs of associated user, and a kind of high-performance self-crosslinking acrylic resin environment-friendly type proposed
Cathode electrodip painting and preparation method.
A kind of formula of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection, includes the original of following parts by weight
Material：15~25 parts of acrylic resin, 0.3~1 part of neutralizer, 0.1~0.2 part of environment-friendly type catalyst, coalescents 0.1~0.5
Part, 1~2 part of mill base, 60~70 parts of deionized water；
The synthesis material of the acrylic resin includes：Monomer, initiator and solvent, the monomer include following parts by weight
Raw material：13~18 parts of Dimethylaminoethyl Methacrylate, 13~18 parts of hydroxy propyl methacrylate, N- methylol acryloyls
4~8 parts of amine, 20~25 parts of methyl methacrylate, 20~30 parts of butyl acrylate, 10~15 parts of styrene, the initiator
Including：1~3 part of azodiisobutyronitrile, the solvent include：Isopropanol, ethylene glycol ethyl ether, butyl glycol ether, ethyl acetate, vinegar
One or more of acid butyl ester, ethyl cellosolve acetate；
The neutralizer includes：One kind in formic acid, acetic acid, lactic acid；
The environment-friendly type catalyst includes：One or two kinds of compounding in isooctyl acid bismuth, aphthenic acids yttrium；
The coalescents include：Ethylene glycol ethyl ether, propylene-glycol ethyl ether, butyl glycol ether, propandiol butyl ether, isopropanol,
One or more of sec-butyl alcohol.
Preferably, the monomer includes the raw material of following parts by weight：15 parts of Dimethylaminoethyl Methacrylate, methyl-prop
16 parts of olefin(e) acid hydroxypropyl acrylate, 5 parts of N hydroxymethyl acrylamide, 20 parts of methyl methacrylate, 30 parts of butyl acrylate, styrene 14
Part.
The invention also provides a kind of preparation method of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection, packets
Include following steps：
S1, in 250 milliliters of four-hole boiling flasks equipped with blender, thermometer, reflux condensing tube and constant pressure funnel, first
Appropriate cosolvent ethyl acetate and butyl glycol ether is added, is heated to 75 DEG C；
S2, into the cosolvent obtained by step S1, add above-mentioned monomer and initiator in constant pressure funnel, stirring
It mixes down and maintains the temperature at 75~85 DEG C, monomer and initiator is made to be dripped in 3h or so；
S3, on the basis of step S2, add appropriate solvent and initiator be slowly added dropwise in constant pressure funnel,
10~20min or so is added dropwise to complete；
S4, the mixture obtained by step S3 is kept the temperature into 1.5h, waits for that reaction conversion ratio reaches requirement and starts to cool down, system drop
Temperature is to 40 DEG C or so；
S5, appropriate neutralizer and environment-friendly type catalyst are added into the reactant obtained by step S4, stir, waits for that resin is complete
Dissolving, obtains lurid self-crosslinking acrylic resin；
S6, suitable deionized water and aqueous color paste are added into the self-crosslinking acrylic resin obtained by step S5, are made into
Acrylic acid cathodic electrophoretic emulsion；
S7, by the acrylic acid cathodic electrophoretic emulsion obtained by step S6 in solid content in 12~13%, electrophoretic voltage 120V, electricity
Swim time 80s, 160 DEG C of solidification temperature, and hardening time 30min obtains paint film.
A kind of advantageous effect of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection proposed by the present invention has：
1, using acrylic monomer as raw material, by introducing with self-cross linking groups function monomer, to synthetic schemes into
Go process optimization, meanwhile, high glaze is prepared, hardness and film thickness can reach the cathode electrodip painting of user demand；
2, by acrylic resin paint Water-borne modification, the VOC in coating can be effectively reduced, coating is alleviated and environment is born
Lotus, and improve the health of the mankind；
3, it carries out being re-dubbed a kind of novel environment-friendly catalyst, compound proportion 1 using isooctyl acid bismuth and aphthenic acids yttrium：1
~1：3, high catalytic efficiency is nontoxic；
4, self-cross linking type environmental protection acrylic cathodic electrophoretic emulsion, can be mating with the Water-borne modification mill base of existing market,
Conveniently with toning, the advantages that construction is simple, operating aspect.
The invention also provides a kind of preparation method of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection, behaviour
Make simply, required material is simple and easy to get, is worthy to be popularized.
Specific implementation mode
The present invention is made further to explain with reference to specific embodiment.
Embodiment one
A kind of formula of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection proposed by the present invention, including it is following
The raw material of parts by weight：15~25 parts of acrylic resin, 0.3~1 part of neutralizer, 0.1~0.2 part of environment-friendly type catalyst, film forming help
0.1~0.5 part of agent, 1~2 part of mill base, 60~70 parts of deionized water；
The synthesis material of the acrylic resin includes：Monomer, initiator and solvent, the monomer include following parts by weight
Raw material：15 parts of Dimethylaminoethyl Methacrylate, 16 parts of hydroxy propyl methacrylate, 5 parts of N hydroxymethyl acrylamide, first
20 parts of base methyl acrylate, 30 parts of butyl acrylate, 14 parts of styrene, the initiator include：0.2 part of azodiisobutyronitrile,
The solvent includes：Isopropanol, ethylene glycol ethyl ether, butyl glycol ether, ethyl acetate, butyl acetate, ethyl cellosolve acetate
One or more of；
The neutralizer is formic acid；
The environment-friendly type catalyst is that isooctyl acid bismuth and aphthenic acids yttrium press 1:1 compounds；
The coalescents include：Ethylene glycol ethyl ether, propylene-glycol ethyl ether, butyl glycol ether, propandiol butyl ether, isopropanol,
One or more of sec-butyl alcohol.
Preparation method includes the following steps：
S1, in 250 milliliters of four-hole boiling flasks equipped with blender, thermometer, reflux condensing tube and constant pressure funnel, first
Appropriate cosolvent ethyl acetate and butyl glycol ether is added, is heated to 75 DEG C；
S2, into the cosolvent obtained by step S1, add above-mentioned monomer and initiator in constant pressure funnel, stirring
It mixes down and maintains the temperature at 75~85 DEG C, monomer and initiator is made to be dripped in 3h or so；
S3, on the basis of step S2, add 3 parts of ethyl acetate and 0.02 part of azodiisobutyronitrile leaked in constant pressure addition
It is slowly added dropwise in bucket, is added dropwise to complete in 10~20min or so；
S4, the mixture obtained by step S3 is kept the temperature into 1.5h, waits for that reaction conversion ratio reaches requirement and starts to cool down, system drop
Temperature is to 40 DEG C or so；
S5,0.3 part of formic acid is added into the reactant obtained by step S4, catalyst compounded 0.1 part, stirring waits for that resin is complete
Fully dissolved obtains lurid self-crosslinking acrylic resin；
S6, suitable deionized water and aqueous color paste are added into the self-crosslinking acrylic resin obtained by step S5, are made into
Acrylic acid cathodic electrophoretic emulsion；
S7, by the acrylic acid cathodic electrophoretic emulsion obtained by step S6 in solid content in 12~13%, electrophoretic voltage 120V, electricity
Swim time 80s, and 160 DEG C, hardening time 30min of solidification temperature obtains flat appearance, good luster, 20 μm of film thickness, the paint of hardness 5H
Film.
Embodiment two
A kind of formula of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection proposed by the present invention, including it is following
The raw material of parts by weight：15~25 parts of acrylic resin, 0.3~1 part of neutralizer, 0.1~0.2 part of environment-friendly type catalyst, film forming help
0.1~0.5 part of agent, 1~2 part of mill base, 60~70 parts of deionized water；
The synthesis material of the acrylic resin includes：Monomer, initiator and solvent, the monomer include following parts by weight
Raw material：15 parts of Dimethylaminoethyl Methacrylate, 16 parts of hydroxy propyl methacrylate, 5 parts of N hydroxymethyl acrylamide, first
20 parts of base methyl acrylate, 30 parts of butyl acrylate, 14 parts of styrene, the initiator include：0.2 part of azodiisobutyronitrile,
The solvent includes：Isopropanol, ethylene glycol ethyl ether, butyl glycol ether, ethyl acetate, butyl acetate, ethyl cellosolve acetate
One or more of；
The neutralizer is acetic acid；
The environment-friendly type catalyst is that isooctyl acid bismuth and aphthenic acids yttrium press 1:2 compound；
The coalescents include：Ethylene glycol ethyl ether, propylene-glycol ethyl ether, butyl glycol ether, propandiol butyl ether, isopropanol,
One or more of sec-butyl alcohol.
Preparation method includes the following steps：
S1, in 250 milliliters of four-hole boiling flasks equipped with blender, thermometer, reflux condensing tube and constant pressure funnel, first
Appropriate cosolvent ethyl acetate and butyl glycol ether is added, is heated to 75 DEG C；
S2, into the cosolvent obtained by step S1, add above-mentioned monomer and initiator in constant pressure funnel, stirring
It mixes down and maintains the temperature at 75~85 DEG C, monomer and initiator is made to be dripped in 3h or so；
S3, on the basis of step S2, add 3 parts of ethyl acetate and 0.02 part of azodiisobutyronitrile leaked in constant pressure addition
It is slowly added dropwise in bucket, is added dropwise to complete in 10~20min or so；
S4, the mixture obtained by step S3 is kept the temperature into 1.5h, waits for that reaction conversion ratio reaches requirement and starts to cool down, system drop
Temperature is to 40 DEG C or so；
S5,0.3 part of acetic acid is added into the reactant obtained by step S4, catalyst compounded 0.1 part, stirring waits for that resin is complete
Fully dissolved obtains lurid self-crosslinking acrylic resin；
S6, suitable deionized water and aqueous color paste are added into the self-crosslinking acrylic resin obtained by step S5, are made into
Acrylic acid cathodic electrophoretic emulsion；
S7, by the acrylic acid cathodic electrophoretic emulsion obtained by step S6 in solid content in 12~13%, electrophoretic voltage 120V, electricity
Swim time 80s, and 160 DEG C, hardening time 30min of solidification temperature obtains flat appearance, good luster, 20 μm of film thickness, the paint of hardness 5H
Film.
A kind of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection proposed by the present invention carries out synthetic schemes
Process optimization, meanwhile, high glaze is prepared, hardness and film thickness can reach the cathode electrodip painting of user demand；It can effectively drop
VOC in prepared paint alleviates load of the coating to environment, and improves the health of the mankind；High catalytic efficiency, it is nontoxic；
Self-cross linking type environmental protection acrylic cathodic electrophoretic emulsion, can be mating with the Water-borne modification mill base of existing market, has toning side
Just, the advantages that construction is simple, operating aspect；The invention also provides a kind of high-performance self-crosslinking acrylic resin environment-friendly type cathodes
The preparation method of electrophoretic paint, easy to operate, required material is simple and easy to get, is worthy to be popularized.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of formula of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection, which is characterized in that including following heavy
Measure the raw material of part：15~25 parts of acrylic resin, 0.3~1 part of neutralizer, 0.1~0.2 part of environment-friendly type catalyst, coalescents
0.1~0.5 part, 1~2 part of mill base, 60~70 parts of deionized water；
The synthesis material of the acrylic resin includes：Monomer, initiator and solvent, the monomer include the original of following parts by weight
Material：13~18 parts of Dimethylaminoethyl Methacrylate, 13~18 parts of hydroxy propyl methacrylate, N hydroxymethyl acrylamide 4
~8 parts, 20~25 parts of methyl methacrylate, 20~30 parts of butyl acrylate, 10~15 parts of styrene, the initiator packet
It includes：1~3 part of azodiisobutyronitrile, the solvent include：Isopropanol, ethylene glycol ethyl ether, butyl glycol ether, ethyl acetate, acetic acid
One or more of butyl ester, ethyl cellosolve acetate；
The neutralizer includes：One kind in formic acid, acetic acid, lactic acid；
The environment-friendly type catalyst includes：One or two kinds of compounding in isooctyl acid bismuth, aphthenic acids yttrium；
The coalescents include：Ethylene glycol ethyl ether, propylene-glycol ethyl ether, butyl glycol ether, propandiol butyl ether, isopropanol, Zhong Ding
One or more of alcohol.
2. a kind of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection according to claim 1, feature exist
In the monomer includes the raw material of following parts by weight：15 parts of Dimethylaminoethyl Methacrylate, hydroxy propyl methacrylate 16
Part, 5 parts of N hydroxymethyl acrylamide, 20 parts of methyl methacrylate, 30 parts of butyl acrylate, 14 parts of styrene.
3. a kind of preparation method of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection, which is characterized in that including with
Lower step：
S1, in 250 milliliters of four-hole boiling flasks equipped with blender, thermometer, reflux condensing tube and constant pressure funnel, be first added
Appropriate cosolvent ethyl acetate and butyl glycol ether, are heated to 75 DEG C；
S2, into the cosolvent obtained by step S1, add above-mentioned monomer and initiator in constant pressure funnel, under stiring
75~85 DEG C are maintained the temperature at, monomer and initiator is made to be dripped in 3h or so；
S3, on the basis of step S2, add appropriate solvent and initiator be slowly added dropwise in constant pressure funnel, 10~
20min or so is added dropwise to complete；
S4, the mixture obtained by step S3 is kept the temperature into 1.5h, waits for that reaction conversion ratio reaches requirement and starts to cool down, system cools to
40 DEG C or so；
S5, appropriate neutralizer and environment-friendly type catalyst are added into the reactant obtained by step S4, stir, waits for that resin is completely molten
Solution, obtains lurid self-crosslinking acrylic resin；
S6, suitable deionized water and aqueous color paste are added into the self-crosslinking acrylic resin obtained by step S5, are made into propylene
Sour cathodic electrophoretic emulsion；
S7, by the acrylic acid cathodic electrophoretic emulsion obtained by step S6 in solid content 12~13%, electrophoretic voltage 120V, when electrophoresis
Between 80s, 160 DEG C of solidification temperature, hardening time 30min obtains paint film.
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| CN201810266209.0A CN108424680A (en) | 2018-03-28 | 2018-03-28 | A kind of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection and preparation method |
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| CN201810266209.0A CN108424680A (en) | 2018-03-28 | 2018-03-28 | A kind of high-performance self-crosslinking acrylic resin Cathode Electrophoretic Paint of Environment Protection and preparation method |
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Cited By (2)
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| CN110117339A (en) * | 2019-06-13 | 2019-08-13 | 深圳市志邦科技有限公司 | A kind of ability cathode electrophoresis coating resins of high salt spray resistance and preparation method thereof |
| CN115536775A (en) * | 2022-10-28 | 2022-12-30 | 江西高杰新材料有限公司 | Acrylic resin copolymer, environment-friendly cathode electrophoretic coating and preparation method |
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Cited By (2)
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|---|---|---|---|---|
| CN110117339A (en) * | 2019-06-13 | 2019-08-13 | 深圳市志邦科技有限公司 | A kind of ability cathode electrophoresis coating resins of high salt spray resistance and preparation method thereof |
| CN115536775A (en) * | 2022-10-28 | 2022-12-30 | 江西高杰新材料有限公司 | Acrylic resin copolymer, environment-friendly cathode electrophoretic coating and preparation method |
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