KR20160139697A - The powder coating composition containing acrylate resin - Google Patents
The powder coating composition containing acrylate resin Download PDFInfo
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- KR20160139697A KR20160139697A KR1020150075042A KR20150075042A KR20160139697A KR 20160139697 A KR20160139697 A KR 20160139697A KR 1020150075042 A KR1020150075042 A KR 1020150075042A KR 20150075042 A KR20150075042 A KR 20150075042A KR 20160139697 A KR20160139697 A KR 20160139697A
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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
- C09D5/03—Powdery paints
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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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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Abstract
The present invention relates to an acrylic resin curing composition for powder coatings excellent in appearance (gloss), adhesion and water resistance.
The acrylic resin curing composition for powder coating of the present invention,
20-30 parts by weight of glycidyl acrylate or glycidyl methacrylate (content in the subject), 10-15 parts by weight of styrene monomer (content in the subject) and 40-50 parts by weight of acrylate monomer A subject synthesized in part (content in the subject); And
At least one of 4 to 12 parts by weight (in the hardening agent) of at least one of acrylic acid, methacrylic acid and maleic anhydride among the monomers containing a carboxyl group, 12 to 16 parts by weight of styrene monomer (content in the hardening agent) And a curing agent obtained by copolymerizing 45 to 50 parts by weight of a monomer (content in a curing agent).
Description
The present invention relates to an acrylic resin curing composition for powder coatings excellent in appearance (gloss), adhesion and water resistance.
More specifically, the present invention relates to an acrylic resin for a powder coating, which comprises a base made of an acrylic resin containing glycidyl acrylate or glycidyl methacrylate at the end of the synthesized polymer and an acrylic hardener containing a carboxyl group ≪ / RTI >
An automobile alloy wheel and a composition for protecting various platelets are obtained through the acrylic powder coating material obtained from the resin.
Commonly used paints are represented by solvent-based paints using organic solvents and water-based paints using water and non-solvent type powder paints.
As emissions standards for organic solvents have been strengthened globally and global environmental problems have arisen, studies on environmentally friendly coating systems are underway in the automotive paint industry, which is a typical example of organic solvent emissions. As a part of the above research, conversion of a solvent-type paint into an aqueous or powder has become a global trend, and research on this has been progressing gradually.
Since the 1970s, the development of powder coatings has been concentrated, and the use of powder coatings has increased dramatically worldwide due to its environmentally friendly properties and the development of resins, additives and equipment technology.
Particularly, powder coating materials are increasingly used in automobile bodies and automobile parts. Among them, transparent paints used for automobile alloy wheels are being converted from acrylic acrylic paints to acrylic powder paints.
Glycidyl methacrylate (GMA) based powder coatings based on powder coatings are often powder coating systems selected from other powder coating systems such as polyester, epoxy and their hybrids for use. GMA powder coatings have been used for over thirty years since the first filed patent (US Patent 3,752,870) published in 1973. GMA powder coatings generally have been generally acclaimed for their excellent smoothness, crystal transparency, chemical resistance, high gloss and excellent outdoor durability. Indeed, until recently, GMA powder coatings are powder coating systems that are selected for topcoat application of the entire vehicle body.
The above-mentioned automotive alloy wheels are highly likely to contact with water or calcium chloride due to their characteristics, and thus water resistance and corrosion resistance are recognized as important property items.
In the case of the transparent powder coating, the polyester type is not only poor in weatherability, but also has a considerably lower appearance compared to the solvent-type clear coating, and a new type of coating is required. A solution to this problem is the acrylic transparent powder coating. Acrylic transparent powder coatings are excellent in weatherability and chemical resistance due to the characteristics of acrylic resin itself, and acrylic powder resin suitable for conventional solvent type has been developed and applied to paints.
However, acrylic paint is superior in weatherability due to its structural characteristics, but water resistance and corrosion resistance are weak compared with epoxy paint. It is generally known that acrylic type is more susceptible to corrosion than polyester type.
As a solution to the above-mentioned problem, there exists a conventional curing method using DDDA (Dodecanedioic acid) as a powder coating material of GMA. However, since DDDA itself is a monomolecular substance, it is inevitably hardened There is a disadvantage in that a large molecular weight required for physical properties may not be obtained.
Therefore, in order to use GMA powder coatings for automobiles, it is necessary to improve and improve powder coatings.
Disclosure of the Invention The present invention has been made in view of the background as described above. It is an object of the present invention to provide an epoxy resin composition which has excellent mechanical properties such as appearance (gloss), adhesiveness, water resistance and corrosion resistance by suitably combining acrylic resin hardeners having epoxy groups and acrylic resin hardeners having carboxyl groups And an object thereof is to provide such an excellent powder coating composition.
In order to accomplish the above object, the present invention provides an acrylic resin curing composition for powder coating,
20-30 parts by weight of glycidyl acrylate or glycidyl methacrylate (content in the subject), 10-15 parts by weight of styrene monomer (content in the subject) and 40-50 parts by weight of acrylate monomer A subject synthesized in part (content in the subject); And
At least one of 4 to 12 parts by weight (in the hardening agent) of at least one of acrylic acid, methacrylic acid and maleic anhydride among the monomers containing a carboxyl group, 12 to 16 parts by weight of styrene monomer (content in the hardening agent) And a curing agent obtained by copolymerizing 45 to 50 parts by weight of a monomer (content in a curing agent).
As described above, the subject matter of the present invention includes 20 to 30% by weight of glycidyl acrylate or glycidyl methacrylate and 50 to 60% by weight of an acrylate monomer as raw materials, wherein glycidyl acrylate or glycidyl acrylate Although the sialyl methacrylate is a kind of acrylate monomer, it is distinguished from the meaning that it should be particularly included separately as described above.
Also, the curing agent simultaneously contains a monomer containing a carboxyl group and an acrylate monomer, and acrylic acid and methacrylic acid among the monomers including a carboxyl group are a kind of an acrylate monomer, but they are distinguished from each other It will be small.
Next, in the present invention, the glass transition temperature (Tg) of the curing agent in the case of using acrylic acid among the monomers containing a carboxyl group is in the range of 50 to 52 캜.
The glass transition temperature (Tg of maleic anhydride is excluded because the Tg of maleic anhydride is unknown, unlike other materials) of the curing agent in the case of using maleic anhydride in the monomer containing a carboxyl group is in the range of 70 to 75 ° C .
I will be more specific about the above configuration.
It is an object of the present invention to provide a topical and curing agent which is a powder coating composition excellent in appearance (gloss), adhesion, water resistance and corrosion resistance. For this purpose, a polymer cured product obtained through an acrylic polymerization process different from the dodecanedioic acid used in the prior art is used.
The composition of the present invention uses a monomer having a glycidyl group (epoxy group) in the synthesis of an acrylic polymer as a main component, wherein glycidyl acrylate or methacrylate is used as the monomer used.
As the curing agent, a polymer composition containing a carboxyl group is used.
The composition of the present invention is characterized by satisfying both rigidity and flexibility by polymerization of a monomer having an epoxy group and a monomer containing a carboxyl group as described above. That is, an acrylic resin containing an epoxy group exhibits an excellent effect of mechanical properties such as leveling, adhesion, water resistance and corrosion resistance by preparing a polymer cured product using acrylic acid and maleic anhydride, which are monomers containing a carboxyl group, at a certain ratio. In addition, even when an uncured portion occurs, the self-molecular weight is sufficiently larger than that of DDDA (dodecanedioic acid) and the number of functional groups is larger than that of DDDA (dodecanedioic acid).
The acrylate monomer used in the subject matter of the present invention and the curing agent may be selected from the group consisting of methyl acrylate, ethyl acrylate, butyl acrylate, isobutyl acrylate, It is preferable to use one or more selected from the group consisting of ethyl acrylate, hydroxyehtyl acrylate, methyl methacrylate, ethyl methacrylate, butyl methacrylate, isobutyl methacrylate, allyl methacrylate, ethylene glycol dimethacrylate, hydroxyethyl methacrylate, glycidyl methacrylate, hexanediol diacrylate, hexanediol Hexanediol dimethacrylate, trimethylpropane t-methacrylate, rimethacrylate, ethyl-3-ethoxy acrylate, triethylene glycol dimethacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate ( hydroxypropyl acrylate, hydroxypropyl methacrylate, hydroxybutyl acrylate, ethoxyethyl acrylate, ethoxyethyl methacrylate, ethylhexyl acrylate, ethylhexyl methacrylate ethylhexyl methacrylate, lauryl acrylate, lauryl methacrylate, ethylene diacrylate, ethyl-3-amino-3-ethoxy acrylate, tertbutyl acrylate, trimethylsilyl methacrylate, tripropylene glycol But are not limited to, tripropylene glycol diacrylate, hexafluoroisopropyl acrylate, hexafluoroisopropyl methacrylate, phenyl methacrylate, tetraethylene glycol diacrylate tetraethylene glycol diacrylate, polyehtylene glycol phenyl ether acrylate, 2-hydroxy-3-phenoxypropyl acrylate, ethylene glycol dicyclopentenyl ether acrylate, (Ethylene glycol dicyclopentenyl ether acrylate), ethylene glycol dicyclopentenyl ether methacrylate, sodium acrylate, sodium methacrylate, tridecyl methacrylate tridecyl methacrylate), hexyl acrylate ( hexyl acrylate, hexyl methacrylate, isodecyl acrylate, isodecyl methacrylate, cyclohexyl methacrylate, benzyl methacrylate, N-propyl acrylate, benzyl 2-ethyl acrylate, ethyl 2-N-propyl acrylate, zinc acrylate, butanediol Butanediol diacrylate, butanediol dimethacrylate, vinyl acrylate, and vinyl methacrylate. The term " a "
The composition of the present invention includes monomers containing a carboxyl group in addition to the acrylate monomers listed above. The composition may contain one, two or three or more substituted aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons, vinyl groups, A methacryl group or a phenyl group can be used. Among them, it is preferable that at least one of acrylic acid, methacrylic acid and maleic acid anhydride is essentially contained.
The monomer of the above-mentioned subject includes 10 to 15 parts by weight (content in the subject) of styrene monomer, 40 to 50 parts by weight (content in the subject) of acrylate monomer, and epoxy group By weight of a monomer (glycidyl acrylate or glycidyl methacrylate) (content in the subject). The monomers thus prepared are mixed with an oil-soluble initiator and an organic solvent. The monomer may be composed of 75 to 85 parts by weight of monomers, 3 to 4 parts by weight of an oil-soluble initiator, and a residual organic solvent. The oil-soluble initiator and the organic solvent to be administered at this time are already known components, which can be administered by a person skilled in the art as needed, and are not characteristics of the present invention.
In the case of an acrylic curing agent composition containing a carboxyl group, the monomer is preferably 4 to 12 parts by weight (content in the curing agent) of at least one of acrylic acid, methacrylic acid or maleic anhydride among the monomers containing a carboxyl group; 12 to 16 parts by weight of styrene monomer (content in the curing agent); 45 to 50 parts by weight (content in the curing agent) of an acrylate monomer. The monomers as described above are mixed with an oil-soluble initiator and an organic solvent, and numerically they can be composed of 65 to 75 parts by weight of monomer, 5 to 9 parts by weight of an oil-soluble initiator, and residual organic solvent. The oil-soluble initiator and the organic solvent to be administered at this time are already known components, which can be administered by a person skilled in the art as needed, and are not characteristics of the present invention. The solvent is removed from the prepared reaction mixture to obtain an acrylic polymer.
The powder coating composition of the present invention obtained by mixing the acrylic resin having epoxy groups and the acrylic resin curing agent having carboxyl groups at a certain ratio has excellent mechanical properties such as leveling, adhesion, water resistance and corrosion resistance.
Hereinafter, the structure and operation of the present invention will be described in more detail with reference to preferred embodiments of the present invention. It is to be understood, however, that the same is by way of illustration and example only and is not to be construed in a limiting sense. Even if the contents are not described in detail herein, those skilled in the art will be able to deduce technically enough that detailed description thereof will be omitted.
[Manufacturing Example 1] An acrylic composition (subject) containing an epoxy group,
In a four-necked flask, an impeller for stirring is installed, and a cooling condenser is mounted. 18 parts by weight of xylene as an organic solvent is metered in and introduced. The temperature of the reaction part is raised to 140 degrees. The stirring speed is 140 rpm. In another container, 12.7 parts by weight of styrene, 27.1 parts by weight of methylmethacrylate, 18.0 parts by weight of n-butyl methacrylate, 22.2 parts by weight of glycidyl methacrylate, Parts by weight, and the mixture is stirred uniformly. 3.75 parts by weight of AIBN (n, n-Azobisburylonitrile) to be used as a initiator is uniformly mixed until completely dissolved. The mixture thus prepared is dropped into the reaction part at a uniform rate for 4 hours. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. 0.2 parts by weight of AIBN (n, n-Azobisburylonitrile) as an initiator and 2 parts by weight of xylene as an organic solvent are homogeneously mixed and dripped into the reaction part at a uniform rate for 1 hour. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. The acrylic composition thus obtained had a nonvolatile content of 80% and a viscosity of from Z to Z3 and a glass transition temperature (Tg) of 65 degrees with a Gardner viscometer. The solvent is removed from the prepared reaction mixture to obtain an acrylic polymer.
[Example 1] An acrylic composition containing a carboxyl group (curing agent 1)
In a four-necked flask, an impeller for stirring is installed, and a cooling condenser is mounted. 26 parts by weight of xylene as an organic solvent is metered in and introduced. The temperature of the reaction part is raised to 125 degrees. The stirring speed is 140 rpm. In another container, 12 parts by weight of styrene, 22 parts by weight of methylmethacrylate, 16.0 parts by weight of n-butyl methacrylate, n-butyl acrylate, 9.22 parts by weight, and acrylic acid (10.78 parts by weight), and the mixture was stirred uniformly. 7.0 parts by weight of Chemex-BO (t-butyl peroxy-2-ethylhexanoate) to be used as a initiator is uniformly mixed until it is completely mixed. The mixture thus prepared is dropped into the reaction part at a uniform rate for 4 hours. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. 0.2 parts by weight of chemex-BO (t-butyl peroxy-2-ethylhexanoate) as an initiator and 2 parts by weight of xylene as an organic solvent are uniformly mixed and dripped into the reaction part at a uniform rate for 1 hour. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. The acrylic composition thus obtained had a nonvolatile content of 70%, a viscosity of from Z to Z3 and a Tg of 52 degrees with a Gardner viscometer, an acid value of 120, and an off-white color. The solvent is removed from the prepared reaction mixture to obtain an acrylic polymer.
[Example 2] An acrylic composition containing a carboxyl group (curing agent 2)
In a four-necked flask, an impeller for stirring is installed, and a cooling condenser is mounted. 26 parts by weight of xylene as an organic solvent is metered in and introduced. The temperature of the reaction part is raised to 125 degrees. The stirring speed is 140 rpm. In another container, 12.6 parts by weight of styrene, 23.2 parts by weight of methylmethacrylate, 16.0 parts by weight of n-butyl methacrylate, 16.0 parts by weight of n-butyl acrylate, 9.22 parts by weight, and acrylic acid (8.98 parts by weight), and the mixture was stirred uniformly. 7.0 parts by weight of Chemex-BO (t-butyl peroxy-2-ethylhexanoate) to be used as a initiator is uniformly mixed until it is completely mixed. The mixture thus prepared is dropped into the reaction part at a uniform rate for 4 hours. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. 0.2 parts by weight of chemex-BO (t-butyl peroxy-2-ethylhexanoate) as an initiator and 2 parts by weight of xylene as an organic solvent are uniformly mixed and dripped into the reaction part at a uniform rate for 1 hour. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. The acrylic composition thus obtained had a nonvolatile content of 70%, a viscosity of from Z to Z3 and a Tg of 52 degrees with a Gardner viscometer, an acid value of 100, and an off-white color. The solvent is removed from the prepared reaction mixture to obtain an acrylic polymer.
[Example 3] An acrylic composition containing a carboxyl group (curing agent 3)
In a four-necked flask, an impeller for stirring is installed, and a cooling condenser is mounted. 26 parts by weight of xylene as an organic solvent is metered in and introduced. The temperature of the reaction part is raised to 125 degrees. The stirring speed is 140 rpm. In another container, 13.27 parts by weight of styrene, 24.31 parts by weight of methylmethacrylate, 16.0 parts by weight of n-butyl methacrylate, 16.0 parts by weight of n-butyl acrylate, 9.22 parts by weight, and acrylic acid (7.2 parts by weight), and the mixture was uniformly stirred. 7.0 parts by weight of Chemex-BO (t-butyl peroxy-2-ethylhexanoate) to be used as a initiator is uniformly mixed until it is completely mixed. The mixture thus prepared is dropped into the reaction part at a uniform rate for 4 hours. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. 0.2 parts by weight of chemex-BO (t-butyl peroxy-2-ethylhexanoate) as an initiator and 2 parts by weight of xylene as an organic solvent are uniformly mixed and dripped into the reaction part at a uniform rate for 1 hour. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. The acrylic composition thus obtained had a nonvolatile content of 70%, a viscosity of from Z to Z3 and a Tg of 52 degrees with a Gardner viscometer, an acid value of 80, and an off-white color. The solvent is removed from the prepared reaction mixture to obtain an acrylic polymer.
[Example 4] An acrylic composition containing a carboxyl group (curing agent 4)
In a four-necked flask, an impeller for stirring is installed, and a cooling condenser is mounted. 13 parts by weight of xylene as an organic solvent is metered in and introduced. The temperature of the reaction part is raised to 125 degrees. The stirring speed is 140 rpm. In another container, 13.74 parts by weight of styrene, 29.4 parts by weight of methylmethacrylate, and 19.51 parts by weight of n-butyl methacrylate were added in this order, followed by uniform stirring. 9 parts by weight of xylene and 10.78 parts by weight of maleic anhydride, which are solvents, are completely dissolved in another container. After confirming that the maleic anhydride is completely dissolved in the solvent, the above monomer mixture is added and uniformly mixed. 6.0 parts by weight of Chemex-BO (t-butyl peroxy-2-ethylhexanoate) to be used as a initiator is uniformly mixed in 3 parts by weight of Xylene as a solvent until it is completely mixed. The monomer mixture thus prepared is added dropwise to the reaction section at a uniform rate for 4 hours and the initiator for 4 hours and 30 minutes, respectively. The reaction temperature is gradually raised according to the refluxing rate of the solvent. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. After cooling the temperature of the reaction part to 65 degrees or less, 0.01 part by weight of lithium hydroxide is completely dissolved together with 7.5 parts by weight of methanol, and then slowly dropped into the reaction part. The reaction temperature is raised to 75 to 80 ° C. and maintained for 5 hours. The acid value is measured and the reaction is completed when the target is reached. The acrylic composition thus obtained had a nonvolatile content of 70%, a viscosity of from Z to Z3 and a Tg of 72.7 degrees with a Gardner viscometer, an acid value of 120 and an off-white color. The solvent is removed from the prepared reaction mixture to obtain an acrylic polymer.
[Example 5] An acrylic composition containing a carboxyl group (curing agent 5)
In a four-necked flask, an impeller for stirring is installed, and a cooling condenser is mounted. 13 parts by weight of xylene as an organic solvent is metered in and introduced. The temperature of the reaction part is raised to 125 degrees. The stirring speed is 140 rpm. In another container, 14.01 parts by weight of styrene, 29.96 parts by weight of methylmethacrylate and 19.9 parts by weight of n-butyl methacrylate were added in this order, followed by uniform stirring. 9 parts by weight of xylene and 6.13 parts by weight of maleic anhydride, which are solvents, are completely dissolved in another container. After confirming that the maleic anhydride is completely dissolved in the solvent, the above monomer mixture is added and uniformly mixed. 6.0 parts by weight of Chemex-BO (t-butyl peroxy-2-ethylhexanoate) to be used as a initiator is uniformly mixed in 3 parts by weight of Xylene as a solvent until it is completely mixed. The monomer mixture thus prepared is added dropwise to the reaction section at a uniform rate for 4 hours and the initiator for 4 hours and 30 minutes, respectively. The reaction temperature is gradually raised according to the refluxing rate of the solvent. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. After cooling the temperature of the reaction part to 65 degrees or less, 0.01 part by weight of lithium hydroxide is completely dissolved together with 7.5 parts by weight of methanol, and then slowly dropped into the reaction part. The reaction temperature is raised to 75 to 80 ° C. and maintained for 5 hours. The acid value is measured and the reaction is completed when the target is reached. The acrylic composition thus obtained had a nonvolatile content of 70%, a viscosity of from Z to Z3 and a Tg of 72.7 degrees with a Gardner viscometer, an acid value of 100, and an off-white color. The solvent is removed from the prepared reaction mixture to obtain an acrylic polymer.
[Example 6] An acrylic composition containing a carboxyl group (curing agent 6)
In a four-necked flask, an impeller for stirring is installed, and a cooling condenser is mounted. 13 parts by weight of xylene as an organic solvent is metered in and introduced. The temperature of the reaction part is raised to 125 degrees. The stirring speed is 140 rpm. In another container, 14.28 parts by weight of styrene, 30.54 parts by weight of methylmethacrylate, and 20.29 parts by weight of n-butyl methacrylate were added in this order, followed by uniform stirring. 9 parts by weight of xylene and 4.89 parts by weight of maleic anhydride, which are solvents, are completely dissolved in another container. After confirming that the maleic anhydride is completely dissolved in the solvent, the above monomer mixture is added and uniformly mixed. 6.0 parts by weight of Chemex-BO (t-butyl peroxy-2-ethylhexanoate) to be used as a initiator is uniformly mixed in 3 parts by weight of Xylene as a solvent until it is completely mixed. The monomer mixture thus prepared is added dropwise to the reaction section at a uniform rate for 4 hours and the initiator for 4 hours and 30 minutes, respectively. The reaction temperature is gradually raised according to the refluxing rate of the solvent. After completion of the dropwise addition, the reaction is maintained at the same temperature for 1 hour. After cooling the temperature of the reaction part to 65 degrees or less, 0.01 part by weight of lithium hydroxide is completely dissolved together with 7.5 parts by weight of methanol, and then slowly dropped into the reaction part. The reaction temperature is raised to 75 to 80 ° C. and maintained for 5 hours. The acid value is measured and the reaction is completed when the target is reached. The acrylic composition thus obtained had a nonvolatile content of 70%, a viscosity of from Z to Z3 and a Tg of 72.7 degrees with a Gardner viscometer, an acid value of 80, and an off-white color. The solvent is removed from the prepared reaction mixture to obtain an acrylic polymer.
[Examples 7 to 12 and Comparative Examples]
The mixture shown in Table 1 was homogeneously dispersed for 4 minutes in a mixer and uniformly melted and mixed in a temperature range of 100 ° C using a melt kneader such as a kneader or extruder. The mixture was pulverized using a turbo mill or a pin disc type pulverizer, and then passed through a 200 mesh sieve to obtain a powder coating material having an average particle size of 10 to 40 μm.
Precipitator: prism 15
Melting disperser: ZSK 27 (Werner & Pleider)
Grinder: HosoKawa alpine 100UPZ (HosoKaWa Micron)
Test items and test methods of coating are as follows.
The powder coating obtained after mixing with the composition shown in Table 1 was electrostatically coated on an aluminum plate pretreated with chromium and cured under the conditions of 160 ° C × 20 minutes (based on the surface of the substrate) to prepare a coating film having a coating film thickness of 80 μm Respectively. The results of the physical properties test of the prepared coating film samples are shown in Table 2 below.
1. Appearance (gloss)
60 degree reflectance measurement using a Potable Gloss-Meter manufactured by BW Co.
(Indicated as "good" when the reflectance is 100 or higher)
2. Initial adhesion (MS600-35 6.8.1)
Measure the degree of peeling by dividing into 100 cells by a grid at 2mm intervals.
(100/100 best ~ 0/100 worst adhesion)
3. Water resistance (MS600-35 7.1)
Adhesion test after immersion at 40 ± 2 ° C for 120 hours
(100/100 best ~ 0/100 worst adhesion)
4. Moisture resistance (MS600-35 7.1)
40 ± 2 ℃ 120 hours Adhesion test after constant temperature and humidity
(100/100 best ~ 0/100 worst adhesion)
5. CASS (GMW14458)
After the X-cut, the coating was sprayed with 35 ± 1 ℃, NaCl 5% + Cupric chloride (CuCl2H2O) 1 ± 0.1 g / gallon + glacial acetic acid 5.5 ml / gallon (pH 3.1 ~ 3.3) × 168 hours, creep back )
(One side mm, the smaller the corrosion area, the better)
6. Salt water silent (MS600-35 7.11)
After immersing in 0.5% sodium chloride solution at 35 ± 2 ℃ for 1200 hours, confirm
The corrosion site should be within 0.5mm of one side from the cross-cut point.
(If it is less than 0.5mm on one side, it is marked as "good")
As shown in Table 2, the powder coating materials using the acrylic hardening agent compositions for powders of Examples 7 to 12 according to the present invention had an acid value of 80 to 100, confirming excellent appearance, adhesion, water resistance, moisture resistance and corrosion resistance I could. Especially, in the case of water resistance and corrosion resistance, compared with the case of using DDDA (dodecanedioic acid), which is a conventional hardening agent, in Comparative Examples, better results were obtained.
Claims (3)
At least one of 4 to 12 parts by weight (in the hardening agent) of at least one of acrylic acid, methacrylic acid and maleic anhydride among the monomers containing a carboxyl group, 12 to 16 parts by weight of styrene monomer (content in the hardening agent) And a curing agent obtained by copolymerizing 45 to 50 parts by weight of a monomer (content in a curing agent).
Acrylic resin curing composition for powder coating.
And the glass transition temperature (Tg) of the curing agent in the case of using acrylic acid among the monomers containing a carboxyl group is in the range of 50 to 52 占 폚.
Acrylic resin curing composition for powder coating.
And the glass transition temperature of the curing agent in the case of using maleic anhydride in the monomer containing a carboxyl group is in the range of 70 to 75 占 폚.
Acrylic resin curing composition for powder coating.
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| KR101768314B1 (en) | 2017-08-14 |
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