CN113698815A - Fluorescent anti-counterfeiting printing ink, preparation method and printing method - Google Patents
Fluorescent anti-counterfeiting printing ink, preparation method and printing method Download PDFInfo
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- CN113698815A CN113698815A CN202110858205.3A CN202110858205A CN113698815A CN 113698815 A CN113698815 A CN 113698815A CN 202110858205 A CN202110858205 A CN 202110858205A CN 113698815 A CN113698815 A CN 113698815A
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- 238000007639 printing Methods 0.000 title claims abstract description 137
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 36
- 229910052693 Europium Inorganic materials 0.000 claims description 28
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 28
- 239000002518 antifoaming agent Substances 0.000 claims description 26
- 239000002562 thickening agent Substances 0.000 claims description 26
- 239000000080 wetting agent Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 22
- 239000013256 coordination polymer Substances 0.000 claims description 21
- 229920001795 coordination polymer Polymers 0.000 claims description 21
- 239000002244 precipitate Substances 0.000 claims description 21
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011324 bead Substances 0.000 claims description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 13
- 229920002635 polyurethane Polymers 0.000 claims description 8
- 239000004814 polyurethane Substances 0.000 claims description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 8
- 150000002910 rare earth metals Chemical class 0.000 claims description 8
- FEIQOMCWGDNMHM-UHFFFAOYSA-N 5-phenylpenta-2,4-dienoic acid Chemical compound OC(=O)C=CC=CC1=CC=CC=C1 FEIQOMCWGDNMHM-UHFFFAOYSA-N 0.000 claims description 7
- 229920001577 copolymer Polymers 0.000 claims description 7
- NZZIMKJIVMHWJC-UHFFFAOYSA-N dibenzoylmethane Chemical group C=1C=CC=CC=1C(=O)CC(=O)C1=CC=CC=C1 NZZIMKJIVMHWJC-UHFFFAOYSA-N 0.000 claims description 7
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 claims description 7
- 238000007646 gravure printing Methods 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- WBQTXTBONIWRGK-UHFFFAOYSA-N sodium;propan-2-olate Chemical compound [Na+].CC(C)[O-] WBQTXTBONIWRGK-UHFFFAOYSA-N 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 230000000694 effects Effects 0.000 abstract description 21
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000976 ink Substances 0.000 description 104
- 238000004519 manufacturing process Methods 0.000 description 7
- -1 polyoxyethylene Polymers 0.000 description 7
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 6
- 239000004721 Polyphenylene oxide Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000002390 adhesive tape Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 125000001165 hydrophobic group Chemical group 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000003921 oil Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002966 varnish Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M3/00—Printing processes to produce particular kinds of printed work, e.g. patterns
- B41M3/14—Security printing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M3/00—Printing processes to produce particular kinds of printed work, e.g. patterns
- B41M3/14—Security printing
- B41M3/144—Security printing using fluorescent, luminescent or iridescent effects
-
- 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 relates to the technical field of anti-counterfeiting printing ink, in particular to fluorescent anti-counterfeiting printing ink, a preparation method and a printing method, wherein the fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight: 1-3 parts of fluorescent powder, 4-8 parts of filler, 50-60 parts of connecting material, 1.3-1.6 parts of assistant and 34-37 parts of solvent. Compared with the existing fluorescent ink, the fluorescent anti-counterfeiting printing ink has good ductility, does not need to print a layer of virgule oil on the ground color, has lower requirements on paper than the existing fluorescent ink, can achieve and display good fluorescent anti-counterfeiting effect on general paper, does not need to adjust the ink by additionally adjusting an auxiliary agent, simplifies the use procedure, improves the printing efficiency, and has better economic benefit.
Description
Technical Field
The invention relates to the technical field of anti-counterfeiting printing ink, in particular to fluorescent anti-counterfeiting printing ink, a preparation method and a printing method.
Background
Along with the development of domestic economy, the varieties of commodities circulating in the market are more and more, and fake commodities are not faked; on the basis, the national strength for fighting against counterfeit commodities is also increasing. Therefore, the anti-counterfeiting printing technology has good development prospect on the basis of the market. The anti-fake ink is a special printing ink produced by adding anti-fake material with special performance into ink vehicle and through special technological process, and the identification of commodity is made by utilizing the characteristic performance of ink.
At present, the anti-counterfeiting ink in China mainly takes spot color ink, magnetic ink and fluorescent ink as main materials. The fluorescent ink can be divided into three types according to the used fluorescent materials, wherein the organic fluorescent material is used as a luminescent material, and the inorganic fluorescent material is synthesized at high temperature; thirdly, a chemically synthesized rare earth organic complex is used. The three fluorescent inks have various advantages, but have defects, such as poor stability and easy oxidative decomposition of the organic fluorescent ink; inorganic fluorescent ink is difficult to disperse in an oil medium and has high synthesis difficulty. In addition, the requirements of the fluorescent ink in the production process are obviously higher than those of the common ink, and the problems that the requirements on the color of a paper surface are higher, some fluorescent ink with low quality cannot achieve a good hiding effect under natural light after being printed, the ink extensibility is poor and the like exist. Although the fluorescent ink has certain defects, the market occupation ratio of the fluorescent ink is still considerable, so in order to improve the defects of the fluorescent ink, some solutions are also proposed in the industry:
(1) in order to solve the problem of poor ductility of the fluorescent ink, when the fluorescent ink is used for printing a plate surface, a layer of the Vickers oil is printed on the ground color first, and then overprinting is carried out.
(2) In order to solve the problem that the fluorescent ink has high requirements on paper, the fluorescent ink needs to be selected according to the attributes of the paper, and the viscosity requirements of different paper on the fluorescent ink are different, so that additives such as varnish and the like need to be added for adjustment sometimes.
The above solutions are proposed to solve the defects of the fluorescent ink in the actual production process, but all enhance the printing effect of the fluorescent ink by adding processes, and have many production and printing processes and high cost.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the fluorescent anti-counterfeiting printing ink which has better ductility compared with the existing fluorescent ink, does not need to print a layer of vitamin oil on the ground color, has lower requirements on paper than the existing fluorescent ink, can achieve and display a good fluorescent anti-counterfeiting effect on general paper, does not need to adjust the ink by additionally adjusting an auxiliary agent, simplifies the use process, improves the printing efficiency and has better economic benefit.
The purpose of the invention is realized by the following technical scheme: the fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight:
preferably, the feed comprises the following raw materials in parts by weight:
preferably, the feed comprises the following raw materials in parts by weight:
most preferably, the feed comprises the following raw materials in parts by weight:
the fluorescent material is a europium coordination polymer NaEu (III) -DBM-PSAA, and is prepared by the following preparation method: 1) europium complex NaEu (DBM)4Preparation:adding anhydrous europium trichloride and isopropanol into a beaker, heating and refluxing, then gradually adding a mixed solution of sodium isopropoxide and HDBM to generate precipitates, removing a supernatant after no precipitate is generated, removing a solvent, and purifying to obtain a yellow solid rare earth europium complex NaEu (DBM)4(ii) a 2) And preparing a coordination polymer: adding a measured PSAA and reagent mixed solution into a beaker, heating in a constant-temperature water bath, and adding NaEu (DBM) while continuously stirring4And adjusting the pH value to 10.0, adding isopropanol for precipitation after reacting for a period of time, performing reduced pressure suction filtration on the precipitate, washing for multiple times, and drying in vacuum to obtain the europium coordination polymer NaEu (III) -DBM-PSAA.
The HDBM is dibenzoylmethane.
The PSAA is poly (styrene-acrylic acid) copolymer, and the reagent is isopropanol or glycerol.
The heating temperature of the constant-temperature water bath heating is 55-65 ℃, the reaction time in the step 2) is 24 hours, the vacuum drying temperature is 40 ℃, and the drying time is 4 hours.
The filler is a mixture of barium sulfate and wax powder in a weight ratio of 5: 1. By selecting the barium sulfate and the wax powder in a specific ratio, the wear resistance of the printed pattern layer can be enhanced on the premise of not influencing the fluorescent effect and the ductility of the ink, and the viscosity and the curing time of the ink are improved.
The connecting material is waterborne polyurethane. The underwater polyurethane is used as a binder, so that a good carrier can be provided for pigment particles, the ink has necessary transfer performance, the printing adaptability of the ink is improved, and the dryness and the glossiness of a printed pattern layer are improved.
The auxiliary agent comprises a wetting agent, a thickening agent and a defoaming agent, and the mass ratio of the wetting agent to the thickening agent to the defoaming agent is 1.2-2:1: 1.
The solvent is a mixture of ethanol and n-butanol.
The wetting agent is alkylphenol polyoxyethylene wetting agent, the thickening agent is hydrophobic group modified nonionic association type thickening agent, and the defoaming agent is organic silicon polyether composite high-temperature defoaming agent. By selecting the specific auxiliary agent combination, the fineness, leveling property, viscosity, adhesion fastness, stability, surface tension and other properties of the printing ink are obviously improved, the printing effect of a printing pattern layer is better, the adaptability of paper is improved, and the requirement on the quality of the paper is lowered.
A preparation method of fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight: 1-3 parts of fluorescent powder, 4-8 parts of filler, 50-60 parts of binder, 1.3-1.6 parts of assistant, 34-37 parts of solvent and 0.1-0.2 part of glass beads for ink preparation, and comprises the following steps: adding fluorescent powder, filler, binder, auxiliary agent, solvent and glass beads for ink preparation into ink preparation equipment, oscillating and dispersing for 0.5-0.6h, and filtering to obtain the fluorescent anti-counterfeiting printing ink of the ink.
The filter screen adopted in the filtering procedure is a 300-mesh filter screen.
The printing method of the fluorescent anti-counterfeiting printing ink prepared by the preparation method adopts the gravure printing equipment, the printing environment temperature is 23-27 ℃, the printing environment humidity is 50-60%, the printing layer drying temperature is 65-75 ℃, the printing speed is 8200m/h, the plate roller pressure: 14-19X 105Pa。
In the anti-counterfeiting design of the package, the fluorescent anti-counterfeiting printing occupies a large proportion, and compared with other anti-counterfeiting technologies, the excellent fluorescent anti-counterfeiting printing can provide a simple and clear anti-counterfeiting effect. However, due to the limitation of fluorescent materials and filler components of the fluorescent ink currently used for fluorescent anti-counterfeiting printing, the fluorescent effect of the existing fluorescent ink in most cases has certain defects, such as insufficient fluorescent intensity, unobvious fluorescent effect and the like, and the anti-counterfeiting effect of the package is limited due to the problem. In order to avoid such problems, it is necessary to improve the composition ratio of the fluorescent ink and the applicability of the fluorescent material. Meanwhile, the complexity of the existing fluorescent ink in use is reduced, for example, how to reduce the problem that the paper adaptability adjustment of the fluorescent ink needs to be carried out by firstly printing a maintenance layer and additionally adding additives such as varnish and the like. However, considering the production cost and the convenience of use, the two considerations need to be combined for comprehensive consideration, so that the produced fluorescent ink not only meets the fluorescent effect required by anti-counterfeiting, but also has certain advantages in production cost compared with products on the market. The fluorescent powder is prepared through a specific production process, the fluorescent effect of the fluorescent powder is excellent, the applicability is strong, the requirement on the quality of paper is low, the fluorescent powder can be suitable for common fluorescent printing paper, a good hiding effect can be achieved under natural light, and a good fluorescent effect can be achieved.
Simultaneously, this application improves to the nature light hidden nature of anti-fake printing layer, anti-fake fluorescence effect, the wearability of printing ink, weatherability, pigment stability, ductility to optimize the drying nature and the glossiness of printing pattern layer, printing pattern layer has excellent wearability and stability simultaneously. This application is through producing specific phosphor powder, select specific filler, specific binder, specific injecting glue and specific solvent, and choose specific raw materials ratio for use, the anti-fake printing ink of fluorescence that obtains has excellent fluorescence effect, printing pattern layer wearability is good and stability is good, can keep still can normal use a year under the prerequisite of avoiding high temperature and burning sun to shine, printing ink ductility is good, paper adhesive force is good, paper adaptability is wide, adaptable in general fluorescence printing paper, printing ink need not add additive adjustment such as varnish before using, and need not to print one deck dimensional oil earlier, production and printing process have been reduced, it is more convenient to use, printing efficiency is for improving greatly.
The invention has the beneficial effects that: the fluorescent anti-counterfeiting printing ink disclosed by the invention is good in ductility, good in fluorescent effect, excellent in wear resistance, good in weather resistance, adhesion, stability and glossiness, a layer of vitamin oil does not need to be printed on a ground color before printing, then overprinting is carried out, the requirement on paper is far lower than that of the existing similar fluorescent printing ink, the paper adaptability is good, the fluorescent anti-counterfeiting printing ink can be suitable for printing most of fluorescent paper, and the fluorescent anti-counterfeiting printing ink does not need to be adjusted by adding auxiliary agents such as varnish before printing. The fluorescent anti-counterfeiting printing ink can achieve an excellent fluorescent anti-counterfeiting effect, saves two processes before being used compared with the existing fluorescent printing ink, can remarkably improve the printing efficiency, and saves the printing cost.
The preparation method provided by the invention is simple in process and suitable for large-scale popularization.
According to the printing method, before the anti-counterfeiting pattern of the fluorescent anti-counterfeiting printing ink is formed, any process has an influence on the fluorescent anti-counterfeiting effect, the printing method has an important influence on the adsorption force and the wear-resistant strength of the printing pattern layer, and the adsorption force and the wear-resistant property of the printing pattern layer are ensured and the fluorescent anti-counterfeiting effect of the printing pattern layer is ensured by selecting specific process parameters which have important influences on the performance of the printing pattern layer.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
The fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight:
the fluorescent material is a europium coordination polymer NaEu (III) -DBM-PSAA, and is prepared by the following preparation method: 1) europium complex NaEu (DBM)4Preparation: adding anhydrous europium trichloride and isopropanol into a beaker, heating and refluxing, then gradually adding a mixed solution of sodium isopropoxide and HDBM to generate precipitates, removing a supernatant after no precipitate is generated, removing a solvent, and purifying to obtain a yellow solid rare earth europium complex NaEu (DBM)4(ii) a 2) And preparing a coordination polymer: adding a measured PSAA and reagent mixed solution into a beaker, heating in a constant-temperature water bath, and adding NaEu (DBM) while continuously stirring4And adjusting the pH value to 10.0, adding isopropanol for precipitation after reacting for a period of time, performing reduced pressure suction filtration on the precipitate, washing for multiple times, and drying in vacuum to obtain the europium coordination polymer NaEu (III) -DBM-PSAA.
The HDBM is dibenzoylmethane.
The PSAA is a poly (styrene-acrylic acid) copolymer and the reagent is isopropanol.
The heating temperature of the constant-temperature water bath heating is 55 ℃, the reaction time in the step 2) is 24 hours, the vacuum drying temperature is 40 ℃, and the drying time is 4 hours.
The filler is a mixture of barium sulfate and wax powder in a weight ratio of 5: 1.
The connecting material is waterborne polyurethane.
The auxiliary agent comprises a wetting agent, a thickening agent and a defoaming agent, and the mass ratio of the wetting agent to the thickening agent to the defoaming agent is 1.2:1: 1.
The solvent is a mixture of ethanol and n-butanol in a weight ratio of 1: 2.
The wetting agent is alkylphenol polyoxyethylene wetting agent, the thickening agent is hydrophobic group modified nonionic association type thickening agent, and the defoaming agent is organic silicon polyether composite high-temperature defoaming agent.
A preparation method of fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight: 1 part of fluorescent powder, 4 parts of filler, 50 parts of binder, 1.3 parts of assistant, 34 parts of solvent and 0.1 part of glass beads for ink preparation, and comprises the following steps: adding fluorescent powder, filler, binder, auxiliary agent, solvent and glass beads for ink preparation into ink preparation equipment, oscillating and dispersing for 0.5h, and filtering to obtain the fluorescent anti-counterfeiting printing ink of the ink.
The filter screen adopted in the filtering procedure is a 300-mesh filter screen.
The printing method of the fluorescent anti-counterfeiting printing ink prepared by the preparation method adopts the gravure printing machine as the printing equipment, the printing environment temperature is 23 ℃, the printing environment humidity is 50%, the printing layer drying temperature is 65 ℃, the printing speed is 8200m/h, the plate roller pressure: 14X 105Pa。
Example 2
The fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight:
the fluorescent material is a europium coordination polymer NaEu (III) -DBM-PSAA, and is prepared by the following preparation method: 1) europium complex NaEu (DBM)4Preparation: adding anhydrous europium trichloride and isopropanol into a beaker, heating and refluxing, then gradually adding a mixed solution of sodium isopropoxide and HDBM to generate precipitates, removing a supernatant after no precipitate is generated, removing a solvent, and purifying to obtain a yellow solid rare earth europium complex NaEu (DBM)4(ii) a 2) And preparing a coordination polymer: adding a measured PSAA and reagent mixed solution into a beaker, heating in a constant-temperature water bath, and adding NaEu (DBM) while continuously stirring4And adjusting the pH value to 10.0, adding isopropanol for precipitation after reacting for a period of time, performing reduced pressure suction filtration on the precipitate, washing for multiple times, and drying in vacuum to obtain the europium coordination polymer NaEu (III) -DBM-PSAA.
The HDBM is dibenzoylmethane.
The PSAA is a poly (styrene-acrylic acid) copolymer, and the reagent is glycerol.
The heating temperature of the constant-temperature water bath heating is 58 ℃, the reaction time in the step 2) is 24 hours, the vacuum drying temperature is 40 ℃, and the drying time is 4 hours.
The filler is a mixture of barium sulfate and wax powder in a weight ratio of 5: 1.
The connecting material is waterborne polyurethane.
The auxiliary agent comprises a wetting agent, a thickening agent and a defoaming agent, and the mass ratio of the wetting agent to the thickening agent to the defoaming agent is 1.5:1: 1.
The solvent is a mixture of ethanol and n-butanol in a mass ratio of 1: 1.
The wetting agent is alkylphenol polyoxyethylene wetting agent, the thickening agent is hydrophobic group modified nonionic association type thickening agent, and the defoaming agent is organic silicon polyether composite high-temperature defoaming agent.
A preparation method of fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight: 1.5 parts of fluorescent powder, 4.5 parts of filler, 53 parts of binder, 1.4 parts of assistant, 35 parts of solvent and 0.12 part of glass beads for ink preparation, and the method comprises the following steps: adding fluorescent powder, filler, binder, auxiliary agent, solvent and glass beads for ink preparation into ink preparation equipment, oscillating and dispersing for 0.5h, and filtering to obtain the fluorescent anti-counterfeiting printing ink of the ink.
The filter screen adopted in the filtering procedure is a 300-mesh filter screen.
The printing method of the fluorescent anti-counterfeiting printing ink prepared by the preparation method adopts the gravure printing machine as the printing equipment, the printing environment temperature is 24 ℃, the printing environment humidity is 52%, the printing layer drying temperature is 68 ℃, the printing speed is 8200m/h, and the plate roller pressure is as follows: 15X 105Pa。
Example 3
The fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight:
the fluorescent material is a europium coordination polymer NaEu (III) -DBM-PSAA, and is prepared by the following preparation method: 1) europium complex NaEu (DBM)4Preparation: adding anhydrous europium trichloride and isopropanol into a beaker, heating and refluxing, then gradually adding a mixed solution of sodium isopropoxide and HDBM to generate precipitates, removing a supernatant after no precipitate is generated, removing a solvent, and purifying to obtain a yellow solid rare earth europium complex NaEu (DBM)4(ii) a 2) And preparing a coordination polymer: adding a measured PSAA and reagent mixed solution into a beaker, heating in a constant-temperature water bath, and adding NaEu (DBM) while continuously stirring4And adjusting the pH value to 10.0, adding isopropanol for precipitation after reacting for a period of time, performing reduced pressure suction filtration on the precipitate, washing for multiple times, and drying in vacuum to obtain the europium coordination polymer NaEu (III) -DBM-PSAA.
The HDBM is dibenzoylmethane.
The PSAA is a poly (styrene-acrylic acid) copolymer and the reagent is isopropanol.
The heating temperature of the constant-temperature water bath heating is 60 ℃, the reaction time in the step 2) is 24 hours, the vacuum drying temperature is 40 ℃, and the drying time is 4 hours.
The filler is a mixture of barium sulfate and wax powder in a weight ratio of 5: 1.
The connecting material is waterborne polyurethane.
The auxiliary agent comprises a wetting agent, a thickening agent and a defoaming agent, and the mass ratio of the wetting agent to the thickening agent to the defoaming agent is 1.6:1: 1.
The solvent is a mixture of ethanol and n-butanol in a weight ratio of 2: 1.
The wetting agent is alkylphenol polyoxyethylene wetting agent, the thickening agent is hydrophobic group modified nonionic association type thickening agent, and the defoaming agent is organic silicon polyether composite high-temperature defoaming agent.
A preparation method of fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight: 2 parts of fluorescent powder, 6 parts of filler, 55 parts of connecting material, 1.5 parts of auxiliary agent, 36 parts of solvent and 0.15 part of glass beads for ink making, and the method comprises the following steps: adding fluorescent powder, filler, binder, auxiliary agent, solvent and glass beads for ink preparation into ink preparation equipment, oscillating and dispersing for 0.5h, and filtering to obtain the fluorescent anti-counterfeiting printing ink of the ink.
The filter screen adopted in the filtering procedure is a 300-mesh filter screen.
The printing method of the fluorescent anti-counterfeiting printing ink prepared by the preparation method adopts the gravure printing machine as printing equipment, the printing environment temperature is 25 ℃, the printing environment humidity is 55%, the printing layer drying temperature is 70 ℃, the printing speed is 8200m/h, and the plate roller pressure: 16X 105Pa。
Example 4
The fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight:
the fluorescent material is a europium coordination polymer NaEu (III) -DBM-PSAA, and is prepared by the following preparation method: 1) europium complex NaEu (DBM)4Preparation: adding anhydrous europium trichloride and isopropanol into a beaker, heating and refluxing, then gradually adding a mixed solution of sodium isopropoxide and HDBM to generate precipitates, removing a supernatant after no precipitate is generated, removing a solvent, and purifying to obtain a yellow solid rare earth europium complex NaEu (DBM)4(ii) a 2) And preparing a coordination polymer: adding a measured PSAA and reagent mixed solution into a beaker, heating in a constant-temperature water bath, and adding NaEu (DBM) while continuously stirring4And adjusting the pH value to 10.0, adding isopropanol for precipitation after reacting for a period of time, performing reduced pressure suction filtration on the precipitate, washing for multiple times, and drying in vacuum to obtain the europium coordination polymer NaEu (III) -DBM-PSAA.
The HDBM is dibenzoylmethane.
The PSAA is a poly (styrene-acrylic acid) copolymer, and the reagent is glycerol.
The heating temperature of the constant-temperature water bath heating is 62 ℃, the reaction time in the step 2) is 24 hours, the vacuum drying temperature is 40 ℃, and the drying time is 4 hours.
The filler is a mixture of barium sulfate and wax powder in a weight ratio of 5: 1.
The connecting material is waterborne polyurethane.
The auxiliary agent comprises a wetting agent, a thickening agent and a defoaming agent, and the mass ratio of the wetting agent to the thickening agent to the defoaming agent is 1.8:1: 1.
The solvent is a mixture of ethanol and n-butanol in a weight ratio of 2: 1.
The wetting agent is alkylphenol polyoxyethylene wetting agent, the thickening agent is hydrophobic group modified nonionic association type thickening agent, and the defoaming agent is organic silicon polyether composite high-temperature defoaming agent.
A preparation method of fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight: 2.5 parts of fluorescent powder, 7 parts of filler, 58 parts of binder, 1.55 parts of assistant, 36.5 parts of solvent and 0.18 part of glass beads for ink preparation, and the method comprises the following steps: adding fluorescent powder, filler, binder, auxiliary agent, solvent and glass beads for ink preparation into ink preparation equipment, oscillating and dispersing for 0.6h, and filtering to obtain the fluorescent anti-counterfeiting printing ink of the ink.
The filter screen adopted in the filtering procedure is a 300-mesh filter screen.
The printing method of the fluorescent anti-counterfeiting printing ink prepared by the preparation method adopts the gravure printing machine as the printing equipment, the printing environment temperature is 26 ℃, the printing environment humidity is 58%, the printing layer drying temperature is 72 ℃, the printing speed is 8200m/h, and the plate roller pressure is as follows: 17X 105Pa。
Example 5
The fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight:
the fluorescent material is a europium coordination polymer NaEu (III) -DBM-PSAA, and is prepared by the following preparation method: 1) europium complex NaEu (DBM)4Preparation: adding anhydrous europium trichloride and isopropanol into a beaker, heating and refluxing, then gradually adding a mixed solution of sodium isopropoxide and HDBM to generate precipitates, removing a supernatant after no precipitate is generated, removing a solvent, and purifying to obtain a yellow solid rare earth europium complex NaEu (DBM)4(ii) a 2) And preparing a coordination polymer: adding a measured PSAA and reagent mixed solution into a beaker, heating in a constant-temperature water bath, and adding NaEu (DBM) while continuously stirring4And adjusting the pH value to 10.0, adding isopropanol for precipitation after reacting for a period of time, performing reduced pressure suction filtration on the precipitate, washing for multiple times, and drying in vacuum to obtain the europium coordination polymer NaEu (III) -DBM-PSAA.
The HDBM is dibenzoylmethane.
The PSAA is a poly (styrene-acrylic acid) copolymer, and the reagent is glycerol.
The heating temperature of the constant-temperature water bath heating is 65 ℃, the reaction time in the step 2) is 24 hours, the vacuum drying temperature is 40 ℃, and the drying time is 4 hours.
The filler is a mixture of barium sulfate and wax powder in a weight ratio of 5: 1.
The connecting material is waterborne polyurethane.
The auxiliary agent comprises a wetting agent, a thickening agent and a defoaming agent, and the mass ratio of the wetting agent to the thickening agent to the defoaming agent is 2:1: 1.
The solvent is a mixture of ethanol and n-butanol in a weight ratio of 1: 1.
The wetting agent is alkylphenol polyoxyethylene wetting agent, the thickening agent is hydrophobic group modified nonionic association type thickening agent, and the defoaming agent is organic silicon polyether composite high-temperature defoaming agent.
A preparation method of fluorescent anti-counterfeiting printing ink comprises the following raw materials in parts by weight: 3 parts of fluorescent powder, 8 parts of filler, 60 parts of binder, 1.6 parts of assistant, 37 parts of solvent and 0.2 part of glass beads for ink making, and the method comprises the following steps: adding fluorescent powder, filler, binder, auxiliary agent, solvent and glass beads for ink preparation into ink preparation equipment, oscillating and dispersing for 0.6h, and filtering to obtain the fluorescent anti-counterfeiting printing ink of the ink.
The filter screen adopted in the filtering procedure is a 300-mesh filter screen.
The printing method of the fluorescent anti-counterfeiting printing ink prepared by the preparation method adopts the gravure printing machine as the printing equipment, the printing environment temperature is 27 ℃, the printing environment humidity is 60%, the printing layer drying temperature is 75 ℃, the printing speed is 8200m/h, the plate roller pressure: 19X 105Pa。
The following table is a table of inspection parameters for the printed pattern layer of the fluorescent security printing inks of examples 1 to 5 of the present application:
and (3) wear resistance test: a special eraser (the type of the eraser is a round eraser at the head of a Chinese-brand pencil) is used for applying a load of 2kgf, the printing pattern layer is rubbed at the speed of 20 times/minute, the rubbing stroke is about 20mm, the rubbing is performed for 30 times, and the single character falls off and fades without influencing the recognition as qualified.
And (3) testing the adhesive force: tightly pasting a 3M600 adhesive tape on a test part (the pasting of the adhesive tape is more than or equal to 25mm and can be adjusted according to the size of a box surface), wiping the pasted adhesive tape with an eraser by 10N-15N force for three times to increase the contact area and force between the adhesive tape and a tested area, extruding bubbles and standing for 1min, grasping one end of the adhesive tape by a hand, tearing off the adhesive tape in the direction of 45-60 degrees within 0.5-1S, testing for one time, observing the falling condition of the printed pictures and texts under the specified test condition, so that the printed pictures and texts do not fade and are full, the printed contents can be clearly identified, and the fluorescent effect is qualified without obvious change.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A fluorescent anti-counterfeiting printing ink is characterized in that: the feed comprises the following raw materials in parts by weight:
2. the fluorescent security printing ink as claimed in claim 1, wherein:
3. the fluorescent security printing ink as claimed in claim 1, wherein:
4. the fluorescent security printing ink as claimed in claim 1, wherein: the fluorescent material is a europium coordination polymer NaEu (III) -DBM-PSAA, and is prepared by the following preparation method: 1) europium complex NaEu (DBM)4Preparation: adding anhydrous europium trichloride and isopropanol into a beaker, heating and refluxing, then gradually adding a mixed solution of sodium isopropoxide and HDBM to generate precipitates, removing a supernatant after no precipitate is generated, removing a solvent, and purifying to obtain a yellow solid rare earth europium complex NaEu (DBM)4(ii) a 2) And preparing a coordination polymer: adding a measured PSAA and reagent mixed solution into a beaker, heating in a constant-temperature water bath, and adding NaEu (DBM) while continuously stirring4And adjusting the pH value to 10.0, adding isopropanol for precipitation after reacting for a period of time, performing reduced pressure suction filtration on the precipitate, washing for multiple times, and drying in vacuum to obtain the europium coordination polymer NaEu (III) -DBM-PSAA.
5. The fluorescent security printing ink as claimed in claim 4, wherein: the HDBM is dibenzoylmethane.
6. The fluorescent security printing ink as claimed in claim 4, wherein: the PSAA is poly (styrene-acrylic acid) copolymer, and the reagent is isopropanol or glycerol.
7. The fluorescent security printing ink as claimed in claim 4, wherein: the heating temperature of the constant-temperature water bath heating is 55-65 ℃, the reaction time in the step 2) is 24 hours, the vacuum drying temperature is 40 ℃, and the drying time is 4 hours.
8. The fluorescent security printing ink as claimed in claim 1, wherein: the filler is a mixture of barium sulfate and wax powder in a weight ratio of 5:1, the binder is waterborne polyurethane, the auxiliary agent comprises a wetting agent, a thickening agent and a defoaming agent, the mass ratio of the wetting agent to the thickening agent to the defoaming agent is 1.2-2:1:1, and the solvent is a mixture of ethanol and n-butyl alcohol.
9. A preparation method of fluorescent anti-counterfeiting printing ink is characterized by comprising the following steps: the feed comprises the following raw materials in parts by weight: 1-3 parts of fluorescent powder, 4-8 parts of filler, 50-60 parts of binder, 1.3-1.6 parts of assistant, 34-37 parts of solvent and 0.1-0.2 part of glass beads for ink preparation, and comprises the following steps: adding fluorescent powder, filler, binder, auxiliary agent, solvent and glass beads for ink preparation into ink preparation equipment, oscillating and dispersing for 0.5-0.6h, and filtering to obtain the fluorescent anti-counterfeiting printing ink of the ink.
10. A printing method of fluorescent anti-counterfeiting printing ink is characterized by comprising the following steps: the fluorescent anti-counterfeiting printing ink prepared by the preparation method of claim 9, wherein the adopted printing equipment is a gravure printing machine, the printing environment temperature is 23-27 ℃, the printing environment humidity is 50-60%, the printing layer drying temperature is 65-75 ℃, the printing speed is 8200m/h, the plate roller pressure is: 14-19X 105Pa。
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