CN111471335A - Novel crack-shaped crystalline material for vacuum coating technology and preparation method thereof - Google Patents

Novel crack-shaped crystalline material for vacuum coating technology and preparation method thereof Download PDF

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CN111471335A
CN111471335A CN202010375743.2A CN202010375743A CN111471335A CN 111471335 A CN111471335 A CN 111471335A CN 202010375743 A CN202010375743 A CN 202010375743A CN 111471335 A CN111471335 A CN 111471335A
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acrylic resin
crystalline material
novel
acrylate
crack
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程文
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Haili Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D4/00Coating 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
    • C09D4/06Organic 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C09D163/10Epoxy resins modified by unsaturated compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes
    • C09D175/14Polyurethanes having carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/28Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for wrinkle, crackle, orange-peel, or similar decorative effects

Abstract

The invention relates to the field of vacuum coating, in particular to a novel crack-shaped crystallization material for a vacuum coating technology and a preparation method thereof. The preparation raw materials of the novel crackle-shaped crystallization material comprise, by weight, 30-40 parts of acrylic resin, 5-12 parts of reactive diluent, 5-12 parts of initiator and 40-50 parts of solvent. The invention provides a novel crackle-shaped crystallization material which can be used for vacuum coating, solves the problem of coating adhesion durability by selecting specific modified acrylate, particularly avoids generating false adhesion when being used for an aluminum film, can solve the problem of poor dryness inside and outside the coating by controlling the using amount and proportion of the modified acrylate and an initiator, realizes cracking effect, and improves the stability of crackle patterns, thereby realizing good crackle-shaped crystallization effect.

Description

Novel crack-shaped crystalline material for vacuum coating technology and preparation method thereof
Technical Field
The invention relates to the field of vacuum coating, in particular to a novel crack-shaped crystallization material for a vacuum coating technology and a preparation method thereof.
Background
The vacuum coating technology is a new technology developed in the last decade, can coat a thin metal layer on the surface of a plated part to endow the surface of a base material such as plastic, metal, glass and the like with metallic luster, and is widely applied to the fields of 3C products, toys, automobiles, building materials and the like. With the improvement of living standard of people, the conventional UV electroplating product can not completely meet the pursuit of people for beauty, and the crack effect is proposed as a new concept product. Although many companies have been working on the development of coatings having a cracking effect, the requirements for pattern stability and durability of adhesion of a coating film cannot be satisfied at present.
Disclosure of Invention
In order to solve the problems, the invention provides a novel crackle-shaped crystallization material for vacuum coating technology, which comprises the following raw materials, by weight, 30-40 parts of acrylic resin, 5-12 parts of reactive diluent, 5-12 parts of initiator and 40-50 parts of solvent; the acrylic resin comprises modified acrylic resin, and the modified acrylic resin is selected from one or more of epoxy acrylic resin, polyurethane acrylic resin and amino acrylic resin.
In a preferred embodiment of the present invention, the urethane acrylic resin is an aliphatic urethane acrylic resin and/or a polycarbonate-modified urethane acrylic resin.
As a preferable technical scheme of the invention, the distributed viscosity of the polyurethane acrylic resin at 60 ℃ is 15000-75000 cps.
As a preferable technical scheme of the invention, the functionality of the polyurethane acrylic resin is 2-3.
As a preferable technical scheme of the invention, the weight percentage of the polyurethane acrylic resin in the total weight of the acrylic resin is 25-35 wt%.
As a preferable technical scheme of the invention, the epoxy acrylic resin accounts for 25-35 wt% of the total weight of the acrylic resin.
In a preferred embodiment of the present invention, the reactive diluent is selected from two or more of monofunctional acrylates, difunctional acrylates, and multifunctional acrylates.
In a preferred embodiment of the present invention, the multifunctional acrylate is one or more selected from trimethylolpropane triacrylate, ditrimethylolpropane tetraacrylate, pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, dipentaerythritol hexaacrylate, and pentaerythritol triacrylate.
In a preferred embodiment of the present invention, the monofunctional acrylate is one or more selected from the group consisting of isobornyl acrylate, isobornyl methacrylate, hydroxyethyl methacrylate and β -carboxyethyl acrylate.
The second aspect of the present invention provides a method for preparing the new crackle-shaped crystalline material for vacuum coating technology, comprising the following steps:
and mixing the acrylic resin, the reactive diluent, the initiator and the solvent at 300-500 r/min to obtain the novel crack-shaped crystalline material.
Compared with the prior art, the invention has the following beneficial effects: the invention provides a novel crackle-shaped crystallization material which can be used for vacuum coating, solves the problem of coating adhesion durability by selecting specific modified acrylate, particularly avoids generating false adhesion when being used for an aluminum film, can solve the problem of poor dryness inside and outside the coating by controlling the using amount and proportion of the modified acrylate and an initiator, realizes cracking effect, and improves the stability of crackle patterns, thereby realizing good crackle-shaped crystallization effect.
Drawings
FIG. 1 is a picture of the new crazing crystal material provided in example 3 after spraying, curing and electroplating.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
The present invention is illustrated by the following specific embodiments, but is not limited to the specific examples given below.
The invention provides a novel crackle-shaped crystallization material for vacuum coating technology, which comprises, by weight, 30-40 parts of acrylic resin, 5-12 parts of reactive diluent, 5-12 parts of initiator and 40-50 parts of solvent.
In a preferred embodiment, the raw material for preparing the novel crazing crystalline material comprises, by weight, 35 parts of acrylic resin, 10 parts of reactive diluent, 10 parts of initiator and 45 parts of solvent.
[ acrylic resin ]
Acrylic resin (acrylic resin) is a generic name for polymers of acrylic acid, methacrylic acid and derivatives thereof. The acrylic resin coating is a thermoplastic or thermosetting resin coating prepared by using (methyl) acrylate and styrene as main components and acrylic resin obtained by copolymerizing the (methyl) acrylate and styrene with other acrylate, or an acrylic radiation coating. The acrylic resin of the present invention is not particularly limited and in one embodiment is commercially available from 8808B available from dongguan, a, supra.
In one embodiment, the acrylic resin of the present invention comprises a modified acrylic resin selected from one or more of epoxy acrylic resin, urethane acrylic resin, amino acrylic resin.
Preferably, the modified acrylic resin of the present invention includes an epoxy acrylic resin.
Epoxy acrylic resin
Epoxy Acrylate (EA), also known as vinyl ester resin, is prepared by esterification of epoxy resin and acrylic acid or methacrylic acid. The epoxy acrylate resin is a photocuring oligomer which is most widely applied and used at present, the photocuring speed of the epoxy acrylate resin is the fastest among various oligomers, a cured coating film has the characteristics of high hardness, good glossiness, excellent corrosion resistance, heat resistance, excellent electrochemistry and the like, and the epoxy acrylate resin is wide in raw material source, low in price and simple in synthesis process, so that the epoxy acrylate resin is one of the photosensitive resins which are most used in photocuring coating. The epoxy acrylate cured coating film has good adhesion, chemical resistance and strength, but has the disadvantages of insufficient flexibility and high brittleness. Therefore, to meet the needs of different fields, the (physical and/or chemical) modification of epoxy acrylates has become one of the research hotspots in this field. Structurally, they are classified into bisphenol a type epoxy acrylic resins, novolac epoxy acrylic resins, epoxy oil type acrylic resins, and modified epoxy acrylates.
More preferably, the epoxy acrylic resin is bisphenol A epoxy acrylic resin and modified epoxy acrylic resin, and the weight ratio is (2-3): (2-3); further, the epoxy acrylic resin is bisphenol A epoxy acrylic resin and modified epoxy acrylic resin, and the weight ratio of the bisphenol A epoxy acrylic resin to the modified epoxy acrylic resin is 1: 1.
in one embodiment, the bisphenol A type epoxy acrylic resin of the present invention has a Brookfield viscosity of 80000 to 100000cps at 25 ℃; further, the bisphenol A type epoxy acrylic resin of the present invention is available from 4213 (Brookfield viscosity at 25 ℃ of 80000 to 100000cps) of Zhongshan Ketian electronics materials Co.
Brookfield viscosity is measured by a Brookfield viscometer, cps being the unit of Brookfield viscosity.
More preferably, the modified epoxy acrylic resin has a Brookfield viscosity of 20000 to 35000cps at 25 ℃.
The modified epoxy acrylic resin is a modified product prepared by reacting epoxy groups or hydroxyl groups in epoxy acrylate with functional groups in other modified substances, and can be exemplified by polyol modified epoxy acrylic resins, acid and acid anhydride modified epoxy acrylic resins, polyurethane modified epoxy acrylic resins, and silicone modified epoxy acrylic resins. The present invention is not specifically limited to the modification method of the modified epoxy resin, and includes ETERCURE 6210G (distributed viscosity at 25 ℃ of 30000-35000 cps), ETERCURE6215-100 (distributed viscosity at 25 ℃ of 20000-35000 cps), and ETERCURE 623A-80.
Further preferably, the weight percentage of the epoxy acrylic resin in the total weight of the acrylic resin is 25-35 wt%; further, the weight percentage of the epoxy acrylic resin in the invention to the total weight of the acrylic resin is 29 wt%.
In one embodiment, the modified acrylic resin of the present invention comprises a urethane acrylic resin.
Polyurethane acrylic resin
The molecule of the polyurethane acrylic resin contains acrylic acid functional group and urethane bond, and the cured adhesive has high wear resistance, adhesion, flexibility, high peel strength, excellent low temperature resistance of polyurethane and excellent optical performance and weather resistance of polyacrylate, and is a radiation curing material with excellent comprehensive performance.
In one embodiment, the polyurethane acrylic resin of the present invention is an aliphatic polyurethane acrylic resin and/or a polycarbonate-modified polyurethane acrylic resin.
The aliphatic polyurethane acrylic resin is a polymer obtained by reacting aliphatic polyurethane with acrylate, and can be exemplified by aliphatic polyurethane acrylic resin with bifunctional degree, such as W2525B (distributed viscosity at 30 ℃ is 8000-18000 cps), W2544, W266J-75, W1080T, W300 (distributed viscosity at 60 ℃ is 50000-75000 cps), W300-Q, W300-P (distributed viscosity at 60 ℃ is 30000-55000 cps), W100 (distributed viscosity at 60 ℃ is 16000-35000 cps); trifunctional aliphatic polyurethane acrylic resins, such as W2513 and W6009 (having a Brookfield viscosity of 16000-32000 cps at 60 ℃).
Preferably, the distributed viscosity of the polyurethane acrylic resin at 60 ℃ is 15000-75000 cps; further, the polyurethane acrylate comprises A type polyurethane acrylic resin and B type polyurethane acrylate, wherein the distributed viscosity of the A type polyurethane acrylic resin at 60 ℃ is 15000-35000 cps, and the distributed viscosity of the B type polyurethane acrylic resin at 60 ℃ is 50000-75000 cps.
More preferably, the weight ratio of the A type polyurethane acrylic resin to the B type polyurethane acrylate is (2-3): (2-3); further, the weight ratio of the A type polyurethane acrylic resin to the B type polyurethane acrylate is 1: 1.
further preferably, the functionality of the polyurethane acrylic resin is 2-3; further, the functionality of the polyurethane acrylic resin of the present invention is 2.
The functionality is the number of functional groups that can participate in the reaction in one molecule.
Still more preferably, the weight percentage of the polyurethane acrylic resin in the invention is 25-35 wt% of the total weight of the acrylic resin; further, the weight percentage of the polyurethane acrylic resin in the invention to the total weight of the acrylic resin is 29 wt%.
Reactive diluent
In one embodiment, the reactive diluent of the present invention is selected from two or more of monofunctional acrylates, difunctional acrylates, multifunctional acrylates.
Examples of monofunctional acrylates include, but are not limited to, isobornyl acrylate, isobornyl methacrylate, hydroxyethyl methacrylate, β -carboxyethyl acrylate.
Examples of difunctional acrylates include, but are not limited to, 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate, diethylene glycol diacrylate, neopentyl glycol diacrylate.
Examples of the multifunctional acrylate include, but are not limited to, trimethylolpropane triacrylate, ditrimethylolpropane tetraacrylate, pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, dipentaerythritol hexaacrylate, pentaerythritol triacrylate.
Preferably, the acrylate of the present invention comprises monofunctional acrylate and multifunctional acrylate, and the weight ratio of the monofunctional acrylate to the multifunctional acrylate is 1: (1-2); further, the weight ratio of the monofunctional acrylate to the multifunctional acrylate is 1: 1.
more preferably, the functionality of the multifunctional acrylate is 3-4; further, the multifunctional acrylate of the present invention has a functionality of 3.
Initiator
In one embodiment, the initiator of the present invention is selected from one or more of benzoin type initiators, benzil type initiators, alkyl phenone type initiators, acyl phosphine oxide type initiators, benzophenone type initiators, and thioxanthone type initiators.
Examples of benzoin-based initiators include, but are not limited to, benzoin dimethyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin butyl ether; in one embodiment, the benzoin-based initiator is benzoin butyl ether.
Examples of the benzil initiator include, but are not limited to, diphenylethanone, α -dimethoxy- α -phenylacetophenone.
Examples of alkylphenone initiators include, but are not limited to, α -diethoxyacetophenone, α -hydroxyalkylphenone, α -aminoalkylphenone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1-hydroxycyclohexylphenylketone, and in one embodiment, 2-hydroxy-2-methyl-1-phenyl-1-propanone or 1-hydroxycyclohexylphenylketone.
Examples of acylphosphine oxide initiators include, but are not limited to, aroylphosphine oxide, bis-benzoylphenylphosphine oxide.
Examples of benzophenone-based initiators include, but are not limited to, benzophenone, 2, 4-dihydroxybenzophenone, Michler's ketone; in one embodiment, the benzophenone-type initiator is benzophenone.
Examples of thioxanthone initiators include, but are not limited to, thiopropoxythioxanthone, isopropyl thioxanthone.
Preferably, the initiator of the present invention comprises a benzophenone-based initiator.
More preferably, the initiator of the present invention further comprises a benzoin-type initiator or an alkyl benzophenone-type initiator.
Further preferably, the initiator provided by the invention is a benzophenone initiator and a benzoin initiator, and the weight ratio is (3-5): 1; further, the weight ratio of the benzophenone initiator to the benzoin initiator is 4: 1.
more preferably, the initiator provided by the invention is a benzophenone initiator and an alkylbenzene ketone initiator, and the weight ratio of the benzophenone initiator to the alkylbenzene ketone initiator is (3-5): 1; further, the weight ratio of the benzophenone initiator to the alkylbenzene initiator is 4: 1.
the applicant finds that the adhesion of vacuum coating can be promoted by selecting proper acrylic resin, such as unmodified acrylic resin, and the combined action of epoxy acrylic resin and polyurethane acrylic resin, and particularly, the acrylic resin with different viscosities is adopted to promote the stability of crack patterns while obtaining good adhesion, and particularly has good effect on aluminum films; and the curing speed of different types of acrylic resin can be controlled by controlling the functionality and viscosity of the acrylic resin and the functionality of the reactive diluent, for example, the low-viscosity polyurethane acrylic resin is slow to cure and has high flexibility, the high-viscosity polyurethane acrylic resin is slow to cure and has high hardness, and the drying property of the surface layer of the paint film can be promoted and the crack effect can be promoted by the combined action of the high-viscosity polyurethane acrylic resin and different initiators. The applicant finds that the phenomenon of false adhesion is easy to occur when the acrylic resin is selected improperly, or the problem of poor drying property inside and outside the coating film is caused when the initiator is selected improperly, such as no benzophenone initiator or no benzoin initiator or alkyl benzophenone initiator or other initiators.
Solvent(s)
The solvent is not specifically limited in the present invention, and is a solvent well known in the art, including, but not limited to, ester solvents such as ethyl acetate, butyl acetate, ethylene glycol monoethyl ether acetate; ketone solvents such as methyl isobutyl ketone, cyclohexanone; alcohol solvents such as ethanol, propanol; benzene-based solvents such as xylene and toluene; ether solvents such as ethylene glycol n-butyl ether, diethyl ether.
In one embodiment, the raw material for preparing the novel crackle-shaped crystalline material further comprises an auxiliary agent.
Auxiliary agent
The invention is not particularly limited to the auxiliaries, and examples thereof include leveling agents, defoaming agents and dispersing agents. The type and amount of these adjuvants are well known to those skilled in the art.
The type and amount of the leveling agent according to the invention are known to the person skilled in the art, for example EFKA3883, EFKA3886, EFKA3600 from loeka, netherlands, BYK306, BYK333, BYK307 from BYK, DEGO410, DEGO2110 from germany. The content of the leveling agent is 0-2 wt%, preferably 0-1.5 wt% based on the total weight of the new crackle crystalline material.
The type and amount of the defoaming agent of the present invention are known to those skilled in the art, for example, EFKA2022, EFKA2527, EFKA2040, ByK352, BYK354, BYK357, from Effka of the Netherlands. The content of the defoaming agent is 0-2 wt%, preferably 0-1.5 wt% based on the total weight of the novel crack-shaped crystalline material.
The dispersant of the present invention is any substance capable of improving the dispersion state of the host resin in a solvent, such as Kerper-602, Kerper-605, Kerper630 of Kerperd of the United states, CFC-500HP, CFC-510, CFC-637, CFC-604S of CFC of France. The content of the dispersant is 0-2 wt%, preferably 0-1.5 wt%, based on the total weight of the new material.
The second aspect of the present invention provides a method for preparing a new crackle-shaped crystalline material for vacuum coating technology, comprising the following steps:
and mixing the acrylic resin, the reactive diluent, the initiator and the solvent at 300-500 r/min to obtain the novel crack-shaped crystalline material.
In one embodiment, the method for preparing a novel crackle-shaped crystalline material for vacuum coating technology comprises the following steps:
and mixing the acrylic resin, the reactive diluent, the initiator and the solvent for 1-2 hours at a speed of 300-500 r/min, and adding an auxiliary agent for mixing to obtain the novel crack-shaped crystalline material.
Examples
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
A1: acrylic resin
The acrylic resin is purchased from 8808B of chemical industry of Dongguan well.
A2: acrylic resin
The acrylic resin is epoxy acrylic resin, and is purchased from 4213 of Zhongshan Ketian electronic materials Co.
A3: acrylic resin
The acrylic resin is modified epoxy acrylic resin, and is purchased from ETERCURE6215-100 of Changxing chemical.
A4: acrylic resin
The acrylic resin is aliphatic polyurethane acrylic resin and is purchased from W100 of New materials, Inc. of Wuxing, Guangzhou.
A5: acrylic resin
The acrylic resin is aliphatic polyurethane acrylic resin which is purchased from W2525B of New five elements materials, Inc. of Guangzhou.
A6: acrylic resin
The acrylic resin is aliphatic polyurethane acrylic resin which is purchased from W300 of New five-element materials, Inc. of Guangzhou.
A7: acrylic resin
The acrylic resin is aliphatic polyurethane acrylic resin and is purchased from W6009 of New five-element materials, Inc. of Guangzhou.
B1: reactive diluent
The active diluent is trimethylolpropane triacrylate.
B2: reactive diluent
The reactive diluent is hydroxyethyl methacrylate.
B3: reactive diluent
The reactive diluent is dipentaerythritol hexaacrylate.
C1: initiator
The initiator is benzophenone and is purchased from Tianjin durable new materials.
C2: initiator
The initiator is benzoin butyl ether and is purchased from Tianjin durable new materials.
C3: initiator
The initiator is 2-hydroxy-2-methyl-1-phenyl-1-acetone, and is purchased from Tianjin new materials for a long time.
C4: initiator
The initiator is 1-hydroxycyclohexyl phenyl ketone, and is purchased from Tianjin new materials for a long time.
D1: solvent(s)
The solvent is ethyl acetate.
D2: solvent(s)
The solvent is butyl acetate.
D3: solvent(s)
The solvent is methyl isobutyl ketone.
D4: solvent(s)
The solvent is ethylene glycol monoethyl ether acetate.
E1: auxiliary agent
The auxiliary agent is BYK 306.
E2: auxiliary agent
The aid is DEGO 2110.
TABLE 1
Figure BDA0002479819320000101
Figure BDA0002479819320000111
Examples 1 to 9 provide novel crack-like crystalline materials, the raw materials for preparing the novel crack-like crystalline materials being shown in table 1 in parts by weight.
Embodiments 1 to 9 further provide a method for preparing the new crack-shaped crystalline material, which includes the following steps:
and mixing the acrylic resin, the reactive diluent, the initiator and the solvent for 1-2 hours at a speed of 300-500 r/min, and adding an auxiliary agent for mixing to obtain the novel crack-shaped crystalline material.
Evaluation of Performance
The new crack-shaped crystalline material for vacuum coating technology provided in the example was sprayed onto a plated article, baked at 60 ℃ for 10min, cured by uv light for 5min, vacuum plated, and used as a sample for the following experiments.
1. Adhesion force: the adhesion was evaluated according to the number of electroplated layers stuck up by the tape and the percentage of the craters, as provided in the examples, with 0B: the peeling area of the representative paint layer is more than 65%; 1B: some squares are partially or completely peeled off, and the peeling area is more than 35 percent and less than or equal to 65 percent; 2B; the peeling of a part or a large area of the paint layer is represented along the edge of the cut, even some grid parts are peeled off integrally, the area is more than 15 percent and less than or equal to 35 percent; 3B: the area of the edge of the cut and the intersection which is peeled off is more than 5 percent and less than or equal to 15 percent; 4B: representing that a small piece of paint layer peels off at the intersection of the cuts, and the actual damage in the grid-scribed area is less than or equal to 5 percent; 5B: it is indicated that the edges of the grid did not peel off and the edges of the cuts were completely smooth. The results are shown in Table 2.
2. Pattern stability: coating and spraying the novel crackle-shaped crystal material for the vacuum coating technology provided by the embodiment on 15 plated parts, baking the plated parts at 60 ℃ for 5 minutes, then carrying out ultraviolet curing and vacuum plating to obtain samples, observing the crack conditions of the 15 samples, and evaluating the samples, wherein the 1-grade cracks of the 15 samples are similar; the 2-level sample has similar cracks of 14-13 samples; the 3-grade sample has similar cracks of 12-11 samples; the 4-grade sample has similar cracks of 9-10 samples; no more than 9 specimens with similar cracks on grade 5. The results are shown in Table 2. Wherein FIG. 1 is a picture of a sample provided in example 3, clear crack lines, metallic feeling and luster can be found.
Table 2 characterization test of properties
Examples Adhesion force Stability of pattern
1 4B Level 1
2 5B Stage 2
3 5B Level 1
4 3B 4 stage
5 4B Grade 3
6 3B Grade 3
7 4B Grade 3
8 4B Grade 3
9 4B Stage 2
The test results in table 2 show that the novel crackle-shaped crystalline material provided by the invention can be used in vacuum coating technology, the adhesion of the substrate such as a crackle-shaped paint layer and a plated part and electroplated metal is good, and the applicant can ensure the cracking effect and the pattern stability by regulating and controlling the preparation raw material of the novel crackle-shaped crystalline material, and is suitable for large-scale production.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.

Claims (10)

1. A novel crackle-shaped crystallization material for a vacuum coating technology is characterized in that raw materials for preparing the novel crackle-shaped crystallization material comprise, by weight, 30-40 parts of acrylic resin, 5-12 parts of an active diluent, 5-12 parts of an initiator and 40-50 parts of a solvent; the acrylic resin comprises modified acrylic resin, and the modified acrylic resin is selected from one or more of epoxy acrylic resin, polyurethane acrylic resin and amino acrylic resin.
2. The new crack-shaped crystalline material for vacuum deposition technology as claimed in claim 1, wherein the polyurethane acrylic resin is aliphatic polyurethane acrylic resin and/or polycarbonate-modified polyurethane acrylic resin.
3. The novel crack-shaped crystalline material for vacuum deposition according to claim 2, wherein the urethane acrylic resin has a Brookfield viscosity of 15000 to 75000cps at 60 ℃.
4. The novel crack-shaped crystalline material for vacuum deposition as claimed in claim 2, wherein the polyurethane acrylic resin has a functionality of 2 to 3.
5. The novel crack-shaped crystalline material for vacuum deposition as claimed in claim 1, wherein the polyurethane acrylic resin is 25-35 wt% based on the total weight of the acrylic resin.
6. The novel crack-shaped crystalline material for vacuum deposition as claimed in claim 1, wherein the epoxy acrylic resin is present in an amount of 25-35 wt% based on the total weight of the acrylic resin.
7. The novel crack-shaped crystalline material for vacuum deposition as claimed in any one of claims 1 to 6, wherein the reactive diluent is selected from two or more of monofunctional acrylate, difunctional acrylate and polyfunctional acrylate.
8. The new craze crystalline material for vacuum deposition technique as claimed in claim 7, wherein the multifunctional acrylate is selected from one or more of trimethylolpropane triacrylate, ditrimethylolpropane tetraacrylate, pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, dipentaerythritol hexaacrylate, and pentaerythritol triacrylate.
9. The new crack-shaped crystalline material for vacuum deposition technology as claimed in claim 7, wherein the monofunctional acrylate is selected from one or more of isobornyl acrylate, isobornyl methacrylate, hydroxyethyl methacrylate, β -carboxyethyl acrylate.
10. The method for preparing the novel crackle-shaped crystalline material for the vacuum coating technology according to any one of claims 1 to 9, comprising the following steps:
and mixing the acrylic resin, the reactive diluent, the initiator and the solvent at 300-500 r/min to obtain the novel crack-shaped crystalline material.
CN202010375743.2A 2020-05-07 2020-05-07 Novel crack-shaped crystalline material for vacuum coating technology and preparation method thereof Withdrawn CN111471335A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114806269A (en) * 2022-05-07 2022-07-29 佛山市西伦化工有限公司 High-brightness liquid photosensitive solder mask ink and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114806269A (en) * 2022-05-07 2022-07-29 佛山市西伦化工有限公司 High-brightness liquid photosensitive solder mask ink and preparation method thereof

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