CN112708305A - Printing ink and preparation method and application thereof - Google Patents

Printing ink and preparation method and application thereof Download PDF

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Publication number
CN112708305A
CN112708305A CN202011496516.1A CN202011496516A CN112708305A CN 112708305 A CN112708305 A CN 112708305A CN 202011496516 A CN202011496516 A CN 202011496516A CN 112708305 A CN112708305 A CN 112708305A
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parts
weight
ink
solvent
prepolymer
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包亚群
谢国雄
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Guangzhou 1s Environmental Protection Technology Co ltd
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Guangzhou 1s Environmental Protection Technology Co ltd
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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
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
    • 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
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • 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
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

The invention provides ink and a preparation method and application thereof, wherein the ink comprises the following components in parts by weight: 40-60 parts of o-cresol epoxy acrylic resin prepolymer, 10-20 parts of polyurethane acrylate prepolymer, 4-8 parts of polyurethane resin, 5-10 parts of epoxy resin, 0.01-0.1 part of polymerization inhibitor, 3-6 parts of photopolymerization initiator, 1-2 parts of melamine and 10-15 parts of solvent. The ink has strong wetting ability, and no shrinkage cavity is generated on a dirty substrate; can resist strong corrosion acid soaking; the deinking time is short and no residue is left; deinking is easy to form flakes and not easy to hang.

Description

Printing ink and preparation method and application thereof
Technical Field
The invention belongs to the technical field of cover plate glass, relates to ink and a preparation method and application thereof, and particularly relates to protective ink for 3D cover plate glass and a preparation method thereof.
Background
In the existing cover plate glass processing technology, different pattern requirements can be generated through etching, one surface of glass is corroded by hydrogen fluoride, nitric acid or frosting liquid, and the like, so that patterns with different textures are carved, and visual effects such as patterns or frosting can be formed. But a protective film is required to cover the non-etching surface or the part which does not need to be etched so as to prevent the accidental etching and the appearance damage. The most common method is to print protective inks, which is suitable for large-scale production. The ink on the market at present is difficult to balance between protection and deinking, and in mass production, the rejection rate is high, the deinking speed is low, a large amount of production time and manpower can be consumed, and the productivity and the benefit can be reduced.
Therefore, in the art, it is desirable to develop a protective ink that has good protection and is easily deinked.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide ink and a preparation method and application thereof, and particularly provides protective ink for 3D cover glass and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides an ink, which comprises the following components in parts by weight:
40-60 parts of o-cresol epoxy acrylic resin prepolymer, 10-20 parts of polyurethane acrylate prepolymer, 4-8 parts of polyurethane resin, 5-10 parts of epoxy resin, 0.01-0.1 part of polymerization inhibitor, 3-6 parts of photopolymerization initiator, 1-2 parts of melamine and 10-15 parts of solvent.
According to the invention, the o-cresol epoxy acrylic resin prepolymer and the polyurethane acrylate prepolymer are matched for use, so that the chemical resistance, hardness and adhesive force of the ink can be well improved, and the polyurethane resin and the epoxy resin are matched, so that the UV-cured glass protective ink which is high in compactness, good in chemical resistance, good in adhesive force, good in wetting capacity, easy to strip and free of residue can be obtained.
In the invention, the deinking speed is improved by the urethane acrylate prepolymer, the o-cresol epoxy acrylic resin prepolymer can obtain a high-strength solvent-resistant and corrosion-resistant polymer after curing, the adhesion of the ink on glass is improved, and the ink is dispersed and falls off in a flake shape when an alkali solvent is removed from the film, so that the ink is not easy to remain on a substrate in a whole piece.
In the present invention, the o-cresol epoxy acryl resin prepolymer may be used in an amount of 42 parts by weight, 44 parts by weight, 46 parts by weight, 48 parts by weight, 50 parts by weight, 53 parts by weight, 55 parts by weight, 58 parts by weight, or 60 parts by weight.
In the present invention, the urethane acrylate prepolymer may be used in an amount of 10 parts by weight, 12 parts by weight, 14 parts by weight, 16 parts by weight, 18 parts by weight, 20 parts by weight.
In the present invention, the polyurethane resin may be used in an amount of 4 parts by weight, 4.5 parts by weight, 5 parts by weight, 5.5 parts by weight, 6 parts by weight, 6.5 parts by weight, 7 parts by weight, 7.5 parts by weight, or 8 parts by weight.
In the present invention, the epoxy resin may be used in an amount of 5 parts by weight, 5.5 parts by weight, 6 parts by weight, 7 parts by weight, 8 parts by weight, 9 parts by weight, or 10 parts by weight.
In the present invention, the polymerization inhibitor may be used in an amount of 0.01 parts by weight, 0.03 parts by weight, 0.05 parts by weight, 0.08 parts by weight, or 0.1 parts by weight.
In the present invention, the photopolymerization initiator may be used in an amount of 3 parts by weight, 3.5 parts by weight, 4 parts by weight, 4.5 parts by weight, 5 parts by weight, 5.5 parts by weight, or 6 parts by weight.
In the present invention, the photo solvent may be used in an amount of 10 parts by weight, 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, or 15 parts by weight.
Preferably, the acid value of the o-cresol epoxy acrylic resin prepolymer is 45-70mgKOH/g, such as 45mgKOH/g, 48mgKOH/g, 50mgKOH/g, 55mgKOH/g, 58mgKOH/g, 60mgKOH/g, 65mgKOH/g, 68mgKOH/g or 70 mgKOH/g.
Preferably, the acid value of the urethane acrylate prepolymer is 160-180mgKOH/g, such as 160mgKOH/g, 165mgKOH/g, 168mgKOH/g, 170mgKOH/g, 175mgKOH/g, 178mgKOH/g, or 180 mgKOH/g.
Preferably, the polyurethane resin is a high-functional polyurethane acrylate, the functionality is 4-6 (such as 4, 5, 6), the weight-average molecular weight is 1000-5000 (such as 1000, 1500, 2000, 2500, 3000, 3500, 4000, 4500 or 5000, etc.), the reactivity can be improved, and the resistance to chemical reaction, hardness and abrasion of the system can be improved after curing.
Preferably, the epoxy resin is a south Asia NPCN-704, NPES-904 or NPEL-128 epoxy resin.
Preferably, the inhibitor is tris (N-nitroso-N-phenylhydroxylamine) aluminium salt, for example may be a commercially available e.g. 510UV inhibitor.
Preferably, the photopolymerization initiator is any one or a combination of at least two of 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1-hydroxycyclohexyl benzophenone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -1-butanone, 2,4, 6-trimethylbenzoylethoxyphenylphosphinic oxide, 2,4, 6-trimethylbenzoyldiphenylphosphinic oxide, isopropylthioxanthene, or 2, 4-diethylthioxanthone.
Preferably, the ink further comprises a diluent in an amount of 10 to 15 parts by weight, such as 10 parts by weight, 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, or 15 parts by weight.
Preferably, the diluent is any one or a combination of at least two of ethyl acetate, propylene glycol methyl ether ester, dipropylene glycol methyl ether ester, butanone, cyclohexanone or isophorone.
Preferably, the ink further comprises a leveling agent in an amount of 0.2 to 0.5 parts by weight, for example 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight or 0.5 parts by weight.
Preferably, the leveling agent is polyether modified siloxane copolymer, preferably Bike BYK-333 and/or Glide 435 and the like.
Preferably, the ink further comprises an oil-repellent agent in an amount of 0.1 to 0.4 parts by weight, for example, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight.
Preferably, the oil repellent is an active silicone oil repellent so that no cratering may occur on the soiled surface, preferably an oil repellent of 47V500 and/or 47V1000, and the like.
Preferably, the ink further comprises a matting agent in an amount of 2 to 5 parts by weight, for example 2 parts by weight, 3 parts by weight, 4 parts by weight or 5 parts by weight.
Preferably, the matting agent is precipitated or fumed silica, and may be Japanese Tosoh E-1011 or Gray ED-30.
Preferably, the ink further comprises a filler in an amount of 35 to 45 parts by weight, such as 35 parts by weight, 37 parts by weight, 40 parts by weight, 42 parts by weight, 44 parts by weight, or 45 parts by weight.
Preferably, the filler is one or a combination of at least two of barium sulfate, calcium carbonate, magnesium carbonate, titanium dioxide, alumina or talc.
Preferably, the solvent is an ester solvent or a ketone solvent.
Preferably, the solvent is any one or a combination of at least two of ethyl acetate, propylene glycol methyl ether ester, dipropylene glycol methyl ether ester, butanone, cyclohexanone or isophorone.
In the invention, the melamine is selected as electronic grade melamine, and is crosslinked into a three-dimensional network structure through a chemical reaction by reacting with functional groups of molecules of a film forming material, so that the hardness and the adhesive force of a formed film can be improved.
In another aspect, the present invention provides a method of preparing an ink as described above, the method comprising the steps of:
stirring and mixing the o-cresol epoxy acrylic resin prepolymer, the polyurethane acrylate prepolymer, the polyurethane resin, the epoxy resin and the solvent, then adding the polymerization inhibitor, the photopolymerization initiator and the melamine, and stirring and dispersing uniformly to obtain the ink.
In another aspect, the present invention provides the use of an ink as described above as a 3D cover glass protective ink.
Compared with the prior art, the invention has the following beneficial effects:
the ink has strong wetting ability, and no shrinkage cavity is generated on a dirty substrate; can resist strong corrosion acid soaking; the deinking time is short (below 12 min), and no residue is left; deinking is easy to form flakes and hang, the adhesive force can reach 0 grade, and the hardness after abrasion is good.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
In this embodiment, an ink is provided, which includes the following components in parts by weight:
Figure BDA0002842328750000051
Figure BDA0002842328750000061
weighing and feeding an o-cresol formaldehyde epoxy acrylate prepolymer, polyurethane resin, a polyurethane acrylate prepolymer, epoxy resin and a solvent. And (3) after stirring uniformly, adding 510 polymerization inhibitor, DETX, IRGACURE 369, titanium dioxide, barium sulfate, talcum powder and melamine while stirring, grinding by using a three-roll grinder until the fineness is less than 10 micrometers, adding the leveling agent, the oil-resistant agent and the matting powder while stirring, and dispersing uniformly to obtain the ink.
Example 2
In this embodiment, an ink is provided, which includes the following components in parts by weight:
Figure BDA0002842328750000062
Figure BDA0002842328750000071
weighing and feeding an o-cresol formaldehyde epoxy acrylate prepolymer, polyurethane resin, a polyurethane acrylate prepolymer, epoxy resin and a solvent. And (3) after stirring uniformly, adding 510 polymerization inhibitor, DETX, IRGACURE 369, titanium dioxide, barium sulfate, talcum powder and melamine while stirring, grinding by using a three-roll grinder until the fineness is less than 10 micrometers, adding the leveling agent, the oil-resistant agent and the matting powder while stirring, and dispersing uniformly to obtain the ink.
Example 3
In this embodiment, an ink is provided, which includes the following components in parts by weight:
Figure BDA0002842328750000072
Figure BDA0002842328750000081
weighing and feeding an o-cresol formaldehyde epoxy acrylate prepolymer, polyurethane resin, a polyurethane acrylate prepolymer, epoxy resin and a solvent. And (3) after stirring uniformly, adding 510 polymerization inhibitor, DETX, IRGACURE 369, titanium dioxide, barium sulfate, talcum powder and melamine while stirring, grinding by using a three-roll grinder until the fineness is less than 10 micrometers, adding the leveling agent, the oil-resistant agent and the matting powder while stirring, and dispersing uniformly to obtain the ink.
Example 4
In this embodiment, an ink is provided, which includes the following components in parts by weight:
Figure BDA0002842328750000082
Figure BDA0002842328750000091
weighing and feeding an o-cresol formaldehyde epoxy acrylate prepolymer, polyurethane resin, a polyurethane acrylate prepolymer, epoxy resin and a solvent. And (3) after stirring uniformly, adding 510 polymerization inhibitor, DETX, IRGACURE 369, titanium dioxide, barium sulfate, talcum powder and melamine while stirring, grinding by using a three-roll grinder until the fineness is less than 10 micrometers, adding the leveling agent, the oil-resistant agent and the matting powder while stirring, and dispersing uniformly to obtain the ink.
Example 5
In this embodiment, an ink is provided, which includes the following components in parts by weight:
Figure BDA0002842328750000092
Figure BDA0002842328750000101
weighing and feeding an o-cresol formaldehyde epoxy acrylate prepolymer, polyurethane resin, a polyurethane acrylate prepolymer, epoxy resin and a solvent. And (3) after stirring uniformly, adding 510 polymerization inhibitor, DETX, IRGACURE 369, titanium dioxide, barium sulfate, talcum powder and melamine while stirring, grinding by using a three-roll grinder until the fineness is less than 10 micrometers, adding the leveling agent, the oil-resistant agent and the matting powder while stirring, and dispersing uniformly to obtain the ink.
Comparative example 1
This comparative example differs from example 1 only in that no o-cresol novolac epoxy acrylate prepolymer was included in the ink and the urethane acrylate prepolymer was used in an amount of 55 parts by weight.
Comparative example 2
This comparative example differs from example 1 only in that the ink does not include a urethane acrylate prepolymer and the amount of o-cresol novolac epoxy acrylate prepolymer is 55 parts by weight.
Comparative example 3
This comparative example differs from example 1 only in that the ink does not include a polyurethane resin.
Comparative example 4
This comparative example differs from example 1 only in that no epoxy resin is included in the ink.
The performance of the inks of the examples and comparative examples was tested as follows:
(1) adhesion force:
the adhesion of the inks to the glass surface was tested according to GB/T9286-1998 test Cross cut for paint and varnish films, according to the test methods described therein, and was rated according to the area of ink release as 0, 1, 2, 3, 4, 5.
(2) Hardness after corrosion: the scratch resistance was tested on the ink surface using hard metal.
(3) Nitric acid corrosion resistance: printing ink on a glass substrate, pre-baking at 80-100 ℃ for 8-10 minutes, irradiating with ultraviolet parallel light with the wavelength of 365nm and the energy of 1000-2And the final baking temperature is 160-180 ℃ for 30-60 minutes. The ink cured under the above conditions was immersed in a 50% nitric acid solution at 25 ℃ for 30 minutes. The discoloration of the ink upon permeation of nitric acid into the ink was observed.
(4) Deinking time: and (3) soaking the glass covered with the cured printing ink in a 5% sodium hydroxide solution, removing the film at 80-85 ℃, and recording the time.
The results are shown in Table 1.
TABLE 1
Figure BDA0002842328750000111
Figure BDA0002842328750000121
The applicant states that the present invention is illustrated by the above examples to the ink of the present invention and the preparation method and application thereof, but the present invention is not limited to the above examples, that is, it does not mean that the present invention must be implemented by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. The printing ink is characterized by comprising the following components in parts by weight:
40-60 parts of o-cresol epoxy acrylic resin prepolymer, 10-20 parts of polyurethane acrylate prepolymer, 4-8 parts of polyurethane resin, 5-10 parts of epoxy resin, 0.01-0.1 part of polymerization inhibitor, 3-6 parts of photopolymerization initiator, 1-2 parts of melamine and 10-15 parts of solvent.
2. The ink according to claim 1, wherein the o-cresol epoxy acrylic resin prepolymer has an acid value of 45 to 70 mgKOH/g;
preferably, the acid value of the polyurethane acrylate prepolymer is 160-180 mgKOH/g;
preferably, the polyurethane resin is a high functional polyurethane acrylate, the functionality should be 4-6, and the weight average molecular weight is 1000-5000.
3. The ink of claim 1 or 2, wherein the epoxy resin is a south asian NPCN-704, NPES-904, NPES-907, or NPEL-128 epoxy resin;
preferably, the polymerization inhibitor is tris (N-nitroso-N-phenylhydroxylamine) aluminum salt;
preferably, the photopolymerization initiator is any one or a combination of at least two of 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1-hydroxycyclohexyl benzophenone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -1-butanone, 2,4, 6-trimethylbenzoylethoxyphenylphosphinic oxide, 2,4, 6-trimethylbenzoyldiphenylphosphinic oxide, isopropylthioxanthene, or 2, 4-diethylthioxanthone.
4. The ink according to any one of claims 1 to 3, characterized in that it further comprises a diluent in an amount of 10 to 15 parts by weight;
preferably, the diluent is any one or a combination of at least two of ethyl acetate, propylene glycol methyl ether ester, dipropylene glycol methyl ether ester, butanone, cyclohexanone or isophorone.
5. The ink according to any one of claims 1 to 4, further comprising a leveling agent in an amount of 0.2 to 0.5 parts by weight;
preferably, the leveling agent is a polyether modified siloxane copolymer, preferably bick BYK-333 and/or Glide 435.
6. The ink according to any one of claims 1 to 5, characterized in that the ink further comprises an oil-repellent agent, the content of the oil-repellent agent being 0.1 to 0.4 parts by weight;
preferably, the oil-repellent agent is an active silicone oil-repellent agent, preferably a 47V500 and/or 47V1000 oil-repellent agent.
7. The ink according to any one of claims 1 to 6, characterized in that it further comprises a matting agent in an amount of 2 to 5 parts by weight;
preferably, the matting agent is precipitated or fumed silica, preferably Japanese Tosoh E-1011 or Gray ED-30.
8. The ink according to any one of claims 1 to 7, further comprising a filler, wherein the filler is contained in an amount of 35 to 45 parts by weight;
preferably, the filler is one or a combination of at least two of barium sulfate, calcium carbonate, magnesium carbonate, titanium dioxide, alumina or talcum powder;
preferably, the solvent is an ester solvent or a ketone solvent;
preferably, the solvent is any one or a combination of at least two of ethyl acetate, propylene glycol methyl ether ester, dipropylene glycol methyl ether ester, butanone, cyclohexanone or isophorone.
9. Method for preparing an ink according to any one of claims 1 to 8, characterized in that it comprises the following steps:
stirring and mixing the o-cresol epoxy acrylic resin prepolymer, the polyurethane acrylate prepolymer, the polyurethane resin, the epoxy resin and the solvent, then adding the polymerization inhibitor, the photopolymerization initiator and the melamine, and stirring and dispersing uniformly to obtain the ink.
10. Use of the ink according to any one of claims 1 to 8 as a protective ink for 3D cover glass.
CN202011496516.1A 2020-12-17 2020-12-17 Printing ink and preparation method and application thereof Pending CN112708305A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104808436A (en) * 2014-01-27 2015-07-29 太阳油墨（苏州）有限公司 Alkali-developable photosensitive resin composition, dry film, cured product and printed circuit board
CN111100499A (en) * 2019-12-23 2020-05-05 无锡德贝尔光电材料有限公司 High-resolution solder resist ink
CN111647304A (en) * 2020-05-11 2020-09-11 Oppo广东移动通信有限公司 Yellow ink, shell of electronic device and manufacturing method of shell

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104808436A (en) * 2014-01-27 2015-07-29 太阳油墨（苏州）有限公司 Alkali-developable photosensitive resin composition, dry film, cured product and printed circuit board
CN111100499A (en) * 2019-12-23 2020-05-05 无锡德贝尔光电材料有限公司 High-resolution solder resist ink
CN111647304A (en) * 2020-05-11 2020-09-11 Oppo广东移动通信有限公司 Yellow ink, shell of electronic device and manufacturing method of shell

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
曾晓鹰等: "《电子束固化涂料及应用》", 31 December 2014, 天津大学出版社 *

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Application publication date: 20210427