CN113088132B - Optical color-changing ink and preparation method thereof - Google Patents
Optical color-changing ink and preparation method thereof Download PDFInfo
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- CN113088132B CN113088132B CN202110542921.0A CN202110542921A CN113088132B CN 113088132 B CN113088132 B CN 113088132B CN 202110542921 A CN202110542921 A CN 202110542921A CN 113088132 B CN113088132 B CN 113088132B
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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
- C09D11/50—Sympathetic, colour changing or similar inks
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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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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Abstract
The invention provides an optical color-changing ink and a preparation method thereof, and relates to the technical field of ink. The preparation method of the optical color-changing ink comprises the following steps: s1, heating and mixing an optically variable pigment, 1 fatty acid methyl ester sulfonate and a sulfonated polyphenyl ether solution to obtain a modified optically variable pigment; s2, mixing 30-50 parts by weight of resin, 20-50 parts by weight of monomer, 3-7 parts by weight of accelerator and 1-2 parts by weight of defoamer, and stirring at 70-90 ℃ to obtain a first mixture; s3, mixing the modified optically variable pigment, 0.5-2 parts by weight of wear-resistant agent and 1-2 parts by weight of stabilizer to obtain a second mixture; and S4, adding the second mixture, 4-8 parts by weight of photoinitiator, 0.5-1 part by weight of dispersant and 1-2 parts by weight of flatting agent into the first mixture, and stirring and mixing to obtain the optical modified ink. The optical modified ink has excellent quality and good adhesive force.
Description
Technical Field
The invention relates to the technical field of printing ink, and in particular relates to optical color-changing printing ink and a preparation method thereof.
Background
The optical color-changing ink is also called as optical color-changing ink or chameleon, and can enable a color block of a printed matter to present a pair of colors, such as red-green, green-blue, gold-silver and the like. The security paper is seen from front or side under white light, two different colors are presented along with the change of the visual angle of human eyes, the light variation characteristic is strong, the color difference change is large, the characteristic is obvious, and the security paper is applied to the anti-counterfeiting printing of valuable papers such as bank notes, checks, bonds and the like at the earliest. With the continuous development of science and technology, the optically variable ink is not only used for anti-counterfeiting printing of trademarks, but also used for surface decoration of special products.
The optically variable ink is obtained by adding optically variable pigment to the ink. However, in the existing optically variable ink, because the optically variable pigment is a solid component, the pigment is easily distributed unevenly in an ink system in the preparation process of the ink, the color distribution is uneven, and the anti-counterfeiting function is poor. In addition, the traditional optical modified ink is generally ester-soluble optical variable ink, so that the VOC content is high, the irritation is strong, and the environmental pollution is easily caused.
Disclosure of Invention
In order to solve the technical problems, the invention provides an optical color-changing ink and a preparation method thereof.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of optical color-changing printing ink, which comprises the following steps:
s1, heating and mixing 10-20 parts by weight of optically variable pigment, 1-2 parts by weight of fatty acid methyl ester sulfonate and 1-3 parts by weight of sulfonated polyphenyl ether solution to obtain modified optically variable pigment;
s2, mixing 30-50 parts by weight of resin, 20-50 parts by weight of monomer, 3-7 parts by weight of accelerator and 1-2 parts by weight of defoamer, and stirring at 70-90 ℃ to obtain a first mixture;
s3, mixing the modified optically variable pigment with 0.5-2 parts by weight of wear-resistant agent and 1-2 parts by weight of stabilizer to obtain a second mixture;
and S4, adding the second mixture, 4-8 parts by weight of photoinitiator, 0.5-1 part by weight of dispersant and 1-2 parts by weight of flatting agent into the first mixture, and stirring and mixing to obtain the optical modified ink.
Further, in a preferred embodiment of the present invention, the mass fraction of the sulfonated polyphenylene ether solution is 1 to 3%.
Further, in a preferred embodiment of the present invention, in step S2, the resin is selected from one or more of polyurethane acrylic resin, unsaturated polyester resin, polyether acrylic resin, polypropylene acrylate and epoxy acrylic resin.
Further, in a preferred embodiment of the present invention, in step S2, the monomer is selected from one or more of dipropylene glycol diacrylate, ethylene glycol diacrylate, ethoxyethoxyethyl acrylate, tripropylene glycol diacrylate and diethylene glycol diacrylate phthalate.
Further, in a preferred embodiment of the present invention, in step S3, the anti-wear agent is obtained according to the following steps: dispersing boron nitride powder in a sodium hydroxide solution, heating and refluxing for 2-8 h, and then cleaning and drying to obtain activated boron nitride powder; adding 3-aminopropyltriethoxysilane into the activated boron nitride powder, stirring for 12-24 h at 90-110 ℃, separating and washing to obtain the wear-resistant agent.
Further, in a preferred embodiment of the present invention, in step S3, the stabilizer is obtained according to the following steps: adding sodium caseinate and ethylenediamine into deionized water, mixing to obtain a mixed solution, adding polyvinyl alcohol, heating and stirring for 1-5 h, adding an EDAC (electronic design automation) crosslinking agent, and reacting to obtain the stabilizer.
Further, in a preferred embodiment of the present invention, in step S4, the photoinitiator is selected from one or two of trimethylbenzoyldiphenylphosphine oxide and bisbenzoylphenylphosphine oxide.
Further, in a preferred embodiment of the present invention, in step S4, the leveling agent is a BYK-delayed aqueous rheological aid.
Further, in a preferred embodiment of the present invention, in step S4, the photoinitiator, the dispersant and the leveling agent of the second mixture are sequentially added while stirring at an oil bath temperature of 40 to 50 ℃, wherein the stirring speed is 30 to 50r/min.
The invention also provides an optical color-changing ink which is prepared according to the preparation method.
The optical color-changing ink and the preparation method thereof have the beneficial effects that:
in the preparation process of the optical color-changing printing ink, the optical color-changing pigment is modified in advance, and the fatty acid methyl ester sulfonate is used for introducing sulfonic acid groups, so that the hydrophilicity and the wettability of the pigment are improved, and the pigment can be well dispersed in the printing ink. The sulfonated polyphenylene oxide can form a stable conjugated pi-bond structure with the optically variable pigment, so that the color is more stable, the anti-counterfeiting performance is improved, and the service life is prolonged.
In addition, the optical color-changing ink can be cured through ultraviolet illumination, has excellent adhesive force on printing materials such as paper and plastics, is high in printing quality, does not have VOC (volatile organic compounds) emission, and can greatly expand the application of the optical color-changing ink in package anti-counterfeiting printing. And the mixing sequence of the raw materials is reasonably optimized, so that the raw materials are well dispersed and mixed, and the product quality is effectively improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The optically variable ink and the method of preparing the same according to the embodiments of the present invention will be described in detail below.
The preparation method of the optical color-changing ink provided by the embodiment of the invention comprises the following steps:
s1, heating and mixing 10-20 parts by weight of optically variable pigment, 1-2 parts by weight of fatty acid methyl ester sulfonate and 1-3 parts by weight of sulfonated polyphenyl ether solution to obtain the modified optically variable pigment.
Furthermore, in the sulfonated polyphenyl ether solution, the mass fraction of the sulfonated polyphenyl ether is 1-3%. The photochromic pigment is modified, and the hydrophilicity and the wettability of the pigment are improved by introducing a sulfonic acid group through fatty acid methyl ester sulfonate. Meanwhile, the sulfonated polyphenyl ether can form a stable conjugated pi-bond structure with the optically variable pigment, so that the color is more stable, the anti-counterfeiting performance of the product is improved, and the service life of the product is prolonged.
It is understood that optically variable pigments can be obtained from commercially available products.
S2, mixing 30-50 parts by weight of resin, 20-50 parts by weight of monomer, 3-7 parts by weight of accelerator and 1-2 parts by weight of defoamer, and stirring at 70-90 ℃ to obtain a first mixture.
Further, the resin is selected from one or more of polyurethane acrylic resin, unsaturated polyester resin, polyether acrylic resin, polypropylene acrylate and epoxy acrylic resin.
Further, the monomer is selected from one or more of dipropylene glycol diacrylate, ethylene glycol diacrylate, ethoxyethoxyethyl acrylate, tripropylene glycol diacrylate and diethylene glycol diacrylate phthalate.
Furthermore, the accelerator is selected from an active amine accelerator or a stannous chloride accelerator, and a small amount of accelerator is added, so that the curing rate can be improved, the wear resistance of the cured product can be improved, and the like.
Further, the defoaming agent is selected from one or more of silicone emulsion, polydimethylsiloxane and polyoxypropylene glycerol ether. The stability of the ink layer can be improved by adding the defoaming agent, and shrinkage cavities are avoided.
Further, in the step, after the raw materials are mixed, the stirring speed is 140-180 r/min, and the stirring time is 20-30 min. In this step, the resin and monomer are premixed at a relatively high agitation rate to produce a first blend of uniform quality. Avoids the problem that the optically variable raw materials are aggregated into a mass to influence the product quality due to uneven mixing in the process of adding the photoinitiator.
And S3, mixing the modified optically variable pigment obtained in the step S1 with 0.5-2 parts by weight of wear-resistant agent and 1-2 parts by weight of stabilizer to obtain a second mixture.
Further, in the present embodiment, the anti-wear agent is obtained according to the following steps: dispersing boron nitride powder in a sodium hydroxide solution, heating and refluxing for 2-8 h, and then cleaning and drying to obtain activated boron nitride powder; adding 3-aminopropyltriethoxysilane into the activated boron nitride powder, stirring for 12-24 h at 90-110 ℃, separating and washing to obtain the wear-resistant agent. Specifically, in one embodiment, 5g of boron nitride powder is dispersed in 5mol/L sodium hydroxide solution, heated and refluxed at 100-120 ℃ for 6h, and then washed and dried to obtain activated boron nitride powder. And (3) placing 5g of activated boron nitride powder into a three-neck flask filled with 50ml of toluene, adding 7ml of 3-aminopropyltriethoxysilane, stirring for 16 hours at the temperature of 90-110 ℃, and separating and washing to obtain the wear-resistant agent. Polyhydroxy and polyamino are modified to boron nitride to obtain amino-bonded boron nitride, hydroxyl and amino groups can form a cross-linked network structure with an ink matrix, so that the wear-resisting agent can be uniformly dispersed, and the active groups can improve the adhesion to printing media such as paper or plastics and the like and improve the wear resistance of the ink.
Further, in this example, the stabilizer was obtained according to the following steps: adding sodium caseinate and ethylenediamine into deionized water, mixing to obtain a mixed solution, adding polyvinyl alcohol, heating and stirring for 1-5 h, adding an EDAC (electronic design automation) crosslinking agent, and reacting to obtain the stabilizer. Specifically, the mass ratio of sodium caseinate to ethylenediamine to polyvinyl alcohol is 10-15: 3 to 6:5 to 10. The sodium caseinate has the effects of excellent bonding capacity and high temperature resistance, and can have good dispersing and leveling effects on the pigment. Sodium caseinate and polyvinyl alcohol are crosslinked to toughen, thicken and modify the sodium caseinate, so that a modified substance can form stable adsorption on a photochromic pigment, and aggregation can be effectively prevented.
And S4, adding the second mixture, 4-8 parts by weight of photoinitiator, 0.5-1 part by weight of dispersant and 1-2 parts by weight of flatting agent into the first mixture, and stirring and mixing to obtain the optical modified ink.
Further, in this step, the photoinitiator is selected from one or two of trimethylbenzoyldiphenylphosphine oxide and bisbenzoylphenylphosphine oxide.
Further, in this step, the dispersant is selected from the group consisting of polymeric dispersants D-265.
Further, in the step, the leveling agent is a BYK delayed type aqueous rheological aid.
Further, in the step, the second mixture, the photoinitiator, the dispersant and the leveling agent are sequentially added while stirring the first mixture at an oil bath temperature of 40-50 ℃, wherein the stirring speed is 30-50 r/min. And in the subsequent mixing process, reducing the stirring speed, and adding the second mixture and other auxiliary agents in sequence, so that the second mixture can be stably dispersed in the ink matrix.
The embodiment of the invention also provides the optical color-changing ink which is prepared according to the preparation method.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The present embodiment provides an optical color-changing ink, which is obtained according to the following steps:
(1) Preparing 13 parts of optically variable pigment, 1.5 parts of fatty acid methyl ester sulfonate, 1.5 parts of 2wt% sulfonated polyphenyl ether solution, 45 parts of polyurethane acrylic resin, 25 parts of dipropylene glycol diacrylate, 4 parts of active amine accelerator, 1 part of defoaming agent (emulsified silicone oil), 1 part of wear-resisting agent, 1 part of stabilizing agent, 5 parts of photoinitiator (trimethyl benzoyl diphenyl phosphine oxide), 0.5 part of dispersing agent (D-265) and 1.5 parts of flatting agent (BYK delayed type aqueous hyper-rheological additive);
wherein the preparation process of the wear-resisting agent comprises the following steps: dispersing 5g of boron nitride powder in 5mol/L sodium hydroxide solution, heating and refluxing for 6h at 100 ℃, and then cleaning and drying to obtain activated boron nitride powder. 5g of activated boron nitride powder is put into a three-neck flask filled with 50ml of toluene, 7ml of 3-aminopropyltriethoxysilane is added, stirring is carried out for 16h at 90 ℃, and the anti-wear agent is obtained through separation and washing.
Wherein, the preparation process of the stabilizer comprises the following steps: adding 10-15 wt% of sodium caseinate solution and 3-6 wt% of ethylenediamine into deionized water, mixing to obtain a mixed solution, adding 5-10 wt% of polyvinyl alcohol, heating and stirring for 2 hours, adding 0.2wt% of EDAC crosslinking agent, and reacting to obtain the stabilizer.
(2) Heating and mixing the optically variable pigment, the fatty acid methyl ester sulfonate and the sulfonated polyphenyl ether solution to obtain a modified optically variable pigment;
(3) Mixing polyurethane acrylic resin, dipropylene glycol diacrylate, an accelerant and a defoaming agent, and stirring at 85 ℃ for 30min at a speed of 150r/min to obtain a material A;
(4) Mixing the modified optically variable pigment obtained in the step (2) with the wear-resisting agent and the stabilizing agent in the step (1) to obtain a material B;
(5) And stirring the material A at the oil bath temperature of 45 ℃ at the speed of 45r/min, sequentially adding the material B, the photoinitiator, the dispersant and the flatting agent, and stirring and mixing to obtain the optically modified ink.
Example 2
The present embodiment provides an optical color-changing ink, which is obtained according to the following steps:
(1) Preparing 10 parts of optically variable pigment, 2 parts of fatty acid methyl ester sulfonate, 1 part of 2wt% sulfonated polyphenyl ether solution, 40 parts of epoxy acrylic resin, 33 parts of ethylene glycol diacrylate, 3 parts of active amine accelerator, 2 parts of defoaming agent (emulsified silicone oil), 0.5 part of wear-resisting agent (same as example 1), 2 parts of stabilizing agent (same as example 1), 4 parts of photoinitiator (trimethylbenzoyl diphenyl phosphine oxide), 1 part of dispersing agent (D-265) and 1.5 parts of flatting agent (BYK delayed type aqueous hyper-rheological additive) according to parts by weight;
(2) Heating and mixing the optically variable pigment, the fatty acid methyl ester sulfonate and the sulfonated polyphenyl ether solution to obtain a modified optically variable pigment;
(3) Mixing epoxy acrylic resin, ethylene glycol diacrylate, an accelerator and a defoaming agent, and stirring at 85 ℃ at the speed of 150r/min for 30min to obtain a material A;
(4) Mixing the modified optically variable pigment obtained in the step (2) with the wear-resistant agent and the stabilizing agent in the step (1) to obtain a material B;
(5) And (3) stirring the material A at the oil bath temperature of 45 ℃ at the speed of 45r/min, sequentially adding the material B, the photoinitiator, the dispersant and the flatting agent, and stirring and mixing to obtain the optical modified ink.
Example 3
The present embodiment provides an optical color-changing ink, which is obtained according to the following steps:
(1) Preparing 16 parts of optically variable pigment, 2 parts of fatty acid methyl ester sulfonate, 1 part of 2wt% sulfonated polyphenyl ether solution, 40 parts of epoxy acrylic resin, 20 parts of ethylene glycol diacrylate, 7 parts of active amine accelerator, 1 part of defoaming agent (emulsified silicone oil), 1.5 parts of wear-resisting agent (same as example 1), 1 part of stabilizing agent (same as example 1), 8 parts of photoinitiator (trimethylbenzoyl diphenylphosphine oxide), 0.5 part of dispersing agent (D-265) and 2 parts of flatting agent (BYK delayed type aqueous hyper-rheological additive) by weight;
(2) Heating and mixing the optically variable pigment, the fatty acid methyl ester sulfonate and the sulfonated polyphenyl ether solution to obtain a modified optically variable pigment;
(3) Mixing epoxy acrylic resin, ethylene glycol diacrylate, an accelerator and a defoaming agent, and stirring at 85 ℃ at the speed of 150r/min for 30min to obtain a material A;
(4) Mixing the modified optically variable pigment obtained in the step (2) with the wear-resisting agent and the stabilizing agent in the step (1) to obtain a material B;
(5) And (3) stirring the material A at the oil bath temperature of 45 ℃ at the speed of 45r/min, sequentially adding the material B, the photoinitiator, the dispersant and the flatting agent, and stirring and mixing to obtain the optical modified ink.
Comparative example 1
The present comparative example provides an optically variable ink obtained according to the following steps:
(1) According to parts by weight, 13 parts of optically variable pigment, 1.5 parts of fatty acid methyl ester sulfonate, 1.5 parts of 2wt% sulfonated polyphenyl ether solution, 45 parts of polyurethane acrylic resin, 25 parts of dipropylene glycol diacrylate, 4 parts of active amine accelerator, 1 part of defoaming agent (emulsified silicone oil), 1 part of wear-resisting agent (same as example 1), 1 part of stabilizer (same as example 1), 5 parts of photoinitiator (trimethylbenzoyl diphenyl phosphine oxide), 0.5 part of dispersant (D-265) and 1.5 parts of flatting agent (BYK delayed type aqueous hyper-rheological additive) are prepared;
(2) Heating and mixing the optically variable pigment, the fatty acid methyl ester sulfonate and the sulfonated polyphenyl ether solution to obtain a modified optically variable pigment;
(3) And (3) mixing the modified optically variable pigment obtained in the step (2) with polyurethane acrylic resin, dipropylene glycol diacrylate, an accelerator, a defoaming agent, an anti-wear agent, a stabilizer, a photoinitiator, a dispersing agent and a flatting agent, and stirring at the oil bath temperature of 45 ℃ at the speed of 100r/min for 60min to obtain the optically variable ink.
Comparative example 2
The present comparative example provides an optically variable ink obtained according to the following steps:
(1) According to parts by weight, 13 parts of optically variable pigment, 45 parts of polyurethane acrylic resin, 25 parts of dipropylene glycol diacrylate, 4 parts of active amine accelerator, 1 part of defoaming agent (emulsified silicone oil), 5 parts of photoinitiator (trimethylbenzoyl diphenyl phosphine oxide), 0.5 part of dispersant (D-265) and 1.5 parts of flatting agent (BYK delayed type aqueous hyper-rheological additive) are prepared;
(3) Mixing polyurethane acrylic resin, dipropylene glycol diacrylate, an accelerator and a defoaming agent, and stirring at 85 ℃ at a speed of 150r/min for 30min to obtain a material A;
(5) And (3) stirring the material A at the oil bath temperature of 45 ℃ at the speed of 45r/min, sequentially adding the optically variable pigment, the photoinitiator, the dispersant and the flatting agent, and stirring and mixing to obtain the optically modified ink.
Test example 1
The optically variable inks of examples 1 to 3 and comparative examples 1 to 2 were filtered through a screen and then applied uniformly to PVC. Then, the sample is placed into an ultraviolet irradiation box, and is taken out after being irradiated for 15min, so that samples 1-5 are obtained respectively. The above samples were tested and the results are shown in table 1:
and (3) testing the photocuring performance: touch detection was performed on a sample taken out from an ultraviolet light irradiation chamber, and the ratio of grade 1: no tack, touch ink, no sticky feel. Level 2: the thumb twist is tack-free, with approximately 5kg downward pressure, and the thumb is used to make a rotational twist on the ink film without breaking the ink film. Level 3: no scratch and solidification, no crack when scratching the ink film with fingernails.
And (3) stability test: the inks obtained in examples 1 to 3 and comparative examples 1 to 2 were allowed to stand at ordinary temperature for 15 days, and the results were observed. Level 1: a large amount of flocculation occurs; level 2: a small amount of flocculation occurs; level 3: and does not settle.
And (3) testing the adhesive force: the ink film is scribed with a needle point in a X shape, then pasted on the nick with cellophane adhesive tape and pulled to see whether the ink film is pulled off. Level 0: the scored ink film can be basically pulled off; level 1: a small amount of ink film is pulled off; level 2: only a slight amount of the ink film is pulled off; and (3) level: no ink film is pulled off.
And (3) testing the wear resistance:
and (3) placing the sample for 24h, then carrying out wear resistance test, and testing by adopting an ink friction resistance tester, wherein a 500g weight is selected and rubbed for 50 times. Level 0: a large amount of ink is wiped off; level 1: a small amount of ink is wiped off; level 2: only a slight amount of ink was wiped off; and (3) level: no ink film ink was wiped off.
TABLE 1 test results table
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Claims (5)
1. The preparation method of the optical color-changing ink is characterized by comprising the following steps:
s1, heating and mixing 10-20 parts by weight of optically variable pigment, 1-2 parts by weight of fatty acid methyl ester sulfonate and 1-3 parts by weight of sulfonated polyphenyl ether solution to obtain modified optically variable pigment;
s2, mixing 30-50 parts by weight of resin, 20-50 parts by weight of monomer, 3-7 parts by weight of accelerator and 1-2 parts by weight of defoamer, and stirring at 70-90 ℃ to obtain a first mixture; wherein the stirring speed is 140-180 r/min, the stirring time is 20-30 min, the resin is selected from one or more of polyurethane acrylic resin, unsaturated polyester resin, polyether acrylic resin, polypropylene acrylate and epoxy acrylic resin, and the monomer is selected from one or more of dipropylene glycol diacrylate, ethylene glycol diacrylate, ethoxy ethyl acrylate, tripropylene glycol diacrylate and phthalic acid diethylene glycol diacrylate;
s3, mixing the modified optically variable pigment with 0.5-2 parts by weight of wear-resistant agent and 1-2 parts by weight of stabilizer to obtain a second mixture; wherein the stabilizer is obtained according to the following steps: adding sodium caseinate and ethylenediamine into deionized water, mixing to obtain a mixed solution, adding polyvinyl alcohol, heating and stirring for 1-5 h, adding an EDAC (electronic design automation) crosslinking agent, and reacting to obtain the stabilizer, wherein the mass ratio of the sodium caseinate to the ethylenediamine to the polyvinyl alcohol is 10-15: 3 to 6:5 to 10; the anti-wear agent is obtained according to the following steps: dispersing boron nitride powder in a sodium hydroxide solution, heating and refluxing for 2-8 h, and then cleaning and drying to obtain activated boron nitride powder; adding 3-aminopropyltriethoxysilane into the activated boron nitride powder, stirring for 12-24 h at 90-110 ℃, separating and washing to obtain the wear-resisting agent;
s4, adding the second mixture, 4-8 parts by weight of photoinitiator, 0.5-1 part by weight of dispersant and 1-2 parts by weight of flatting agent into the first mixture, and stirring and mixing to obtain optical modified ink; the stirring and mixing process comprises the following steps: and at the oil bath temperature of 40-50 ℃, the second mixture, the photoinitiator, the dispersant and the flatting agent are added in sequence while the first mixture is stirred, wherein the stirring speed is 30-50 r/min.
2. The method for preparing an optically variable ink according to claim 1, wherein the mass fraction of the sulfonated polyphenylene ether solution is 1 to 3%.
3. The method for preparing an optically variable ink according to claim 1, wherein in step S4, the photoinitiator is selected from one or both of trimethylbenzoyldiphenylphosphine oxide and bisbenzoylphenylphosphine oxide.
4. The method of claim 1, wherein in step S4, the leveling agent is a BYK-delayed aqueous rheological aid.
5. An optically variable ink, characterized by being produced by the production method according to any one of claims 1 to 4.
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| CN102464919A (en) * | 2010-11-12 | 2012-05-23 | 惠州市华阳光学技术有限公司 | Optical color-changing flexo printing ink |
| CN106010181B (en) * | 2016-06-20 | 2018-04-06 | 上海理工大学 | The preparation method of metal conditioner and its corrosion-resistant finishes containing nm-class boron nitride |
| CN107236367B (en) * | 2017-06-30 | 2020-11-24 | 厦门理工学院 | Temperature-sensing reversible color-changing UV (ultraviolet) ink for PVC (polyvinyl chloride), and preparation method and use method thereof |
| CN110527354A (en) * | 2019-07-29 | 2019-12-03 | 北京金辰西维科安全印务有限公司 | Cold light source solidifies optically variable security ink and preparation method thereof and printing process |
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