CN103804986A - Inorganic optical variable ink and fabrication method thereof - Google Patents
Inorganic optical variable ink and fabrication method thereof Download PDFInfo
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- CN103804986A CN103804986A CN201310703821.7A CN201310703821A CN103804986A CN 103804986 A CN103804986 A CN 103804986A CN 201310703821 A CN201310703821 A CN 201310703821A CN 103804986 A CN103804986 A CN 103804986A
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Abstract
The invention discloses an inorganic optical variable ink comprising a pigment, a binder and an assistant, wherein the pigment is a silver-doped lanthanum titanate compound, and can become into brick-red from white under ultraviolet light irradiation. The preparation method comprises the following steps: 1, mixing TiO2, La2O3 and AgNO3 powder/crystal, adding absolute ethyl alcohol to, grinding into a paste, heating and taking out, cooling, grinding into even and fine particles, naturally cooling to room temperature after roasting, carrying out ball-milling, and sieving after baking, so as to obtain La0.9Ag0.1TiO3 particles; 2, preparing a mixed solution from ethyl acetate, ethyecellulose and epoxy resin; 3, adding colloidal calcium, polyethylene glycol, an antidesiccant and a dispersing agent to the mixed solution prepared in the step 2, and evenly mixing; 4, putting the mixed solution evenly mixed in the step 3 into a light-tight ball-milling tank, putting the La0.9Ag0.1TiO3 particles into the ball-milling tank, and taking out after ball-milling.
Description
Technical field
The invention belongs to printed material technical field, relate to a kind of inorganic optical disclour printing ink, the preparation method of this color shifting ink.
Background technology
Fast-developing science and technology and printing packaging periphery product provide various convenient by way of the form take different as people live from multiple.But meanwhile, the product of high-tech content is popular has also expedited the emergence of continuing to bring out of various high emulation fakements, and various substandard products fakements have seriously damaged human consumer's rights and interests and the economic interests of businessman.Therefore, the angle of and life security healthy from Protection of consumer, false proof requirement and the demand degree of people to all kinds of commodity is all more and more higher.
In recent years, new and effective anti-counterfeiting technology and anti-forgery ink continue to bring out, common printing-ink and mode of printing can not meet the comprehensive special false proof demand of modern goods, use separately a kind of efficient anti-forging ink or combine the printing technology that uses multiple anti-forgery ink, in anti-counterfeit printing, being widely used.Anti-forgery ink is an extremely important part in the false proof field of modern society, and along with social progress and scientific and technological development, various anti-forgery inks are applied in printing.But the peculiar exclusivity of anti-counterfeiting technology requires anti-forgery ink to keep constantly renewal and the development of high speed, various anti-forgery ink also arises at the historic moment.
Also have in the prior art some photochromism anti-forging ink, but at present mainly take organic camouflage paint as main, its shortcoming is that the synthetic output capacity of pigment is low, variable color colour gamut is narrower, is difficult for check etc., and range of application is narrower.
Summary of the invention
The object of the invention is to provide a kind of inorganic optical disclour printing ink, and the synthetic output capacity of pigment that solves prior art existence is low, and variable color colour gamut is narrower, is difficult for the problem of check.
Technical scheme of the present invention is, inorganic optical disclour printing ink, comprises pigment, binder and auxiliary agent, and pigment is that under UV-irradiation, this pigment can be become from white brick-red with the lanthanium titanate compound of silver doping.
Feature of the present invention is also:
Pigment comprises that weight ratio is the lanthanium titanate oxide compound of the silver doping of 15% ﹣ 25%; Binder comprises that weight ratio is the ethyl acetate of 25%-40%, the ethyl cellulose of 15%-30% and the epoxy resin of 10%-20%; Auxiliary agent comprises that weight ratio is the colloid calcium of 10%-15%, the polyoxyethylene glycol of 1%-3%, 1% antidesiccant and the dispersion agent of 4%-10%.
Above-mentioned inorganic optical disclour printing ink is subject to UV-light or natural light irradiation 30s, and variable color can occur, and is become brick-redly from white, irradiates after 1min, and its maximum aberration is 13.96.
Above-mentioned inorganic optical disclour printing ink is being subject to after UV-irradiation generation variable color, and the baking oven of putting into 100 ℃ leaves standstill 20min, can be by the brick-red illumination white before that returns to.
Second technical scheme of the present invention is that the preparation method of above-mentioned color shifting ink, comprises the following steps:
Step 1, mixes TiO2, La2O3 and tri-kinds of powder of AgNO3/crystal, adds dehydrated alcohol to grind to form pasty state, heating, takes out the cooling even fine particle that grinds to form, and naturally cools to room temperature after roasting, carry out ball milling, after oven dry, sieve, obtain La0.9Ag0.1TiO3 particle;
Step 2, makes mixed solution by ethyl acetate, ethyl cellulose and epoxy resin;
Step 3, adds colloid calcium in step 2 in the mixed solution making, polyoxyethylene glycol, and antidesiccant and dispersion agent, mix;
Step 4, the mixed solution mixing that step 3 is made is put into lucifuge ball grinder, and La0.9Ag0.1TiO3 particle is put into ball grinder, after ball milling, takes out.
In step 1, under normal temperature, normal pressure, according to mole proportioning of TiO2:La2O3:AgNO3=1:4:2, three kinds of powder/crystal is mixed, add dehydrated alcohol to grind to form pasty state, put temperature and be 2h in the baking oven of 80 ℃, take out that room temperature is cooling grinds to form even fine particle, put into retort furnace roasting, 5 ℃/min to 900 ℃ of temperature rise rate, insulation roasting 6h; After roasting, naturally cool to room temperature, under turn/min of rotating speed 1200, carry out ball milling 3h with satellite-type ball mill, after taking out and drying, granules of pigments grinding is sifted out with 200 object screen clothes, obtain La0.9Ag0.1TiO3 particle.
Step 2, is under normal temperature, normal pressure, the ethyl acetate that is 25%-40% by mass ratio, and the ethyl cellulose of 15%-30%, the epoxy resin of 10%-20% is made mixed solution.
Step 3, is that the mixed solution of step 2 being made with dispersion machine is uniformly dispersed, and in dispersion process, to add weight ratio be the colloid calcium of 10%-15%, the polyoxyethylene glycol of 1%-3%, 1% antidesiccant, the dispersion agent of 4%-10%.
Step 4, is that finely dispersed mixed solution in step 3 is taken out and puts into lucifuge ball grinder, and the lanthanium titanate oxide compound of the silver that is 15%-25% by mass ratio doping is put into ball grinder, after ball milling 3h, takes out.
In step 1, when roasting pigment, temperature rise rate is 5 ℃/min.
In step 3, the jitter time of mixed solution in dispersion machine is 60-90min.
In step 4, drum's speed of rotation is turn/min of 950-1200.
The present invention has following beneficial effect:
1, the present invention is directed to single, the difficult check of current optical anti-counterfeiting ink type, the more high defect of cost, optical disclour printing ink for offset printing is proposed, it is false proof with photosensitive ink that this color shifting ink can be used for packages printing, have and implement the advantages such as simple, cost is low, hiding good, check is convenient, can replace traditional photosensitive anti-forgery ink.
2, color shifting ink of the present invention can be directly used in packing box, Valued Securities, daily necessities, the mark of commodity and the false proof some printings of packing such as clothes and CD goods, can increase the false proof point of above product, improve the business added value of the products such as packing box, for enterprise provides new profit growth.
3, color shifting ink of the present invention also can be used as light pollution indicator, is manufacturing for some specialty products, avoids the light pollution indicating label of illumination in storage and transportation.
4, preparation method of the present invention utilizes the photochromic property of ABO3 perovskite structure composite oxide, synthesizing inorganic optical disclour printing ink, and preparation method is simple, is easy to realize, and cost is low.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described further.
Embodiment 1, inorganic optical disclour printing ink, comprises pigment, binder and auxiliary agent.
The composition of pigment is the lanthanium titanate composite oxides La0.9Ag0.1TiO3 of silver doping, and its weight ratio is 20%.Binder comprises that weight ratio is 35% ethyl acetate, 15% ethyl cellulose and 10% epoxy resin.Auxiliary agent comprises that weight ratio is 12.51% colloid calcium, 1% polyoxyethylene glycol, 1% antidesiccant and 1% wilkinite.Antidesiccant is according to 2,6 di tert butyl 4 methyl phenol: a mole proportioning of No. six oil=5:95 mixes to be made.
The preparation method of this inorganic optical disclour printing ink is as follows:
Step 1, under normal temperature, normal pressure, according to mole proportioning of TiO2:La2O3:AgNO3=1:4:2, three kinds of powder/crystal is mixed, add dehydrated alcohol to grind to form pasty state, put temperature and be 2h in the baking oven of 80 ℃, take out that room temperature is cooling grinds to form even fine particle, put into retort furnace roasting, 5 ℃/min to 900 ℃ of temperature rise rate, insulation roasting 6h.The pigment sample fired is taken out, naturally cool to room temperature, under turn/min of rotating speed 1200, carry out ball milling 3h with satellite-type ball mill, after taking out and drying, granules of pigments grinding is sifted out with 200 object screen clothes, obtain camouflage paint particle.When roasting pigment, temperature rise rate is 5 ℃/min.
Step 2, under normal temperature, normal pressure, the ethyl acetate that is 35% by mass ratio, 15% ethyl cellulose, 10% epoxy resin is made mixed solution.
Step 3, is uniformly dispersed mixed solution made in step 2 with dispersion machine, and in dispersion process, to add weight ratio be 15% colloid calcium, 1% polyoxyethylene glycol, 1% antidesiccant and 1% dispersion agent.The jitter time of mixed solution in dispersion machine is controlled at 90min.
Dispersion agent is common dispersants DC, and effective constituent is sodium polyacrylate.
Step 4, takes out finely dispersed mixed solution in step 3 to put into lucifuge ball grinder, and the silver-colored La0.9Ag0.1TiO3 that is 20% by mass ratio puts into ball grinder, after ball milling 3h, takes out.Drum's speed of rotation is controlled at 1200 turn/min.
Embodiment 2, inorganic optical disclour printing ink, comprises pigment, binder and auxiliary agent.
The composition of pigment is the lanthanium titanate composite oxides La0.9Ag0.1TiO3 of silver doping, and its weight ratio is 25%.
Binder comprises that weight ratio is 40% ethyl acetate, 25% ethyl cellulose and 15% epoxy resin;
Auxiliary agent comprises: the colloid calcium that weight ratio is 15%, 3% polyoxyethylene glycol, 1% antidesiccant and 3% wilkinite.Antidesiccant is according to 2,6 di tert butyl 4 methyl phenol: a mole proportioning of No. six oil=5:95 mixes to be made.
The making method of this inorganic optical disclour printing ink:
Step 1, under normal temperature, normal pressure, according to mole proportioning of TiO2:La2O3:AgNO3=1:4:2, three kinds of powder/crystal is mixed, add dehydrated alcohol to grind to form pasty state, put temperature and be 2h in the baking oven of 80 ℃, take out that room temperature is cooling grinds to form even fine particle, put into retort furnace roasting, 5 ℃/min to 900 ℃ of temperature rise rate, insulation roasting 6h.The pigment sample fired is taken out, naturally cool to room temperature, under turn/min of rotating speed 1200, carry out ball milling 3h with satellite-type ball mill, after taking out and drying, granules of pigments grinding is sifted out with 200 object screen clothes, obtain camouflage paint particle.When roasting pigment, temperature rise rate is 5 ℃/min.
Step 2, under normal temperature, normal pressure, the ethyl acetate that is 40% by mass ratio, 25% ethyl cellulose, 15% epoxy resin is made mixed solution.
Step 3, is uniformly dispersed mixed solution made in S2 with dispersion machine, and in dispersion process, to add weight ratio be 15% colloid calcium, 1% polyoxyethylene glycol, 1% antidesiccant, 1% dispersion agent.The jitter time of mixed solution in dispersion machine should be controlled at 90min.
Dispersion agent is common dispersants DC, and effective constituent is sodium polyacrylate.
Step 4, takes out finely dispersed mixed solution in S3 step to put into lucifuge ball grinder, and the silver-colored La0.9Ag0.1TiO3 that is 25% by mass ratio puts into ball grinder, after ball milling 3h, takes out.
Drum's speed of rotation is controlled at 1200 turn/min.
, being subject to UV-light or natural light irradiation 30s, can there is variable color in inorganic optical disclour printing ink prepared by the present invention, become brick-redly from white, irradiates after 1min, and its maximum aberration is 13.96.Be subject to after UV-irradiation generation variable color, the baking oven of putting into 100 ℃ leaves standstill 20min, can be by the brick-red illumination white before that returns to.
Claims (10)
1. inorganic optical disclour printing ink, is characterized in that, comprises pigment, binder and auxiliary agent, and described pigment is that under UV-irradiation, this pigment can be become from white brick-red with the lanthanium titanate compound of silver doping.
2. inorganic optical disclour printing ink as claimed in claim 1, is characterized in that, described pigment comprises that weight ratio is the lanthanium titanate oxide compound of the silver doping of 15% ﹣ 25%; Described binder comprises that weight ratio is the ethyl acetate of 25%-40%, the ethyl cellulose of 15%-30% and the epoxy resin of 10%-20%; Described auxiliary agent comprises that weight ratio is the colloid calcium of 10%-15%, the polyoxyethylene glycol of 1%-3%, 1% antidesiccant and the dispersion agent of 4%-10%.
3. inorganic optical disclour printing ink as claimed in claim 1 or 2, is characterized in that, is subject to UV-light or natural light irradiation 30s, and variable color can occur, and is become brick-redly from white, irradiates after 1min, and its maximum aberration is 13.96.
4. inorganic optical disclour printing ink as claimed in claim 3, is characterized in that, is being subject to after UV-irradiation generation variable color, and the baking oven of putting into 100 ℃ leaves standstill 20min, can be by the brick-red illumination white before that returns to.
5. the preparation method of the inorganic optical disclour printing ink as described in claim 1-4 any one, comprises the following steps:
Step 1, mixes TiO2, La2O3 and tri-kinds of powder of AgNO3/crystal, adds dehydrated alcohol to grind to form pasty state, heating, takes out the cooling even fine particle that grinds to form, and naturally cools to room temperature after roasting, carry out ball milling, after oven dry, sieve, obtain La0.9Ag0.1TiO3 particle;
Step 2, makes mixed solution by ethyl acetate, ethyl cellulose and epoxy resin;
Step 3, adds colloid calcium in step 2 in the mixed solution making, polyoxyethylene glycol, and antidesiccant and dispersion agent, mix;
Step 4, the mixed solution mixing that step 3 is made is put into lucifuge ball grinder, and La0.9Ag0.1TiO3 particle is put into ball grinder, after ball milling, takes out.
6. the preparation method of inorganic optical disclour printing ink as claimed in claim 5, it is characterized in that: in step 1, under normal temperature, normal pressure, according to mole proportioning of TiO2:La2O3:AgNO3=1:4:2, three kinds of powder/crystal are mixed, add dehydrated alcohol to grind to form pasty state, put temperature and be 2h in the baking oven of 80 ℃, take out that room temperature is cooling grinds to form even fine particle, put into retort furnace roasting, 5 ℃/min to 900 ℃ of temperature rise rate, insulation roasting 6h; After roasting, naturally cool to room temperature, under turn/min of rotating speed 1200, carry out ball milling 3h with satellite-type ball mill, after taking out and drying, granules of pigments grinding is sifted out with 200 object screen clothes, obtain La0.9Ag0.1TiO3 particle.
7. the preparation method of inorganic optical disclour printing ink as claimed in claim 5, is characterized in that: step 2 is under normal temperature, normal pressure, the ethyl acetate that is 25%-40% by mass ratio, and the ethyl cellulose of 15%-30%, the epoxy resin of 10%-20% is made mixed solution.
8. the preparation method of inorganic optical disclour printing ink as claimed in claim 5, it is characterized in that: step 3, that the mixed solution of step 2 being made with dispersion machine is uniformly dispersed, and in dispersion process, to add weight ratio be the colloid calcium of 10%-15%, the polyoxyethylene glycol of 1%-3%, 1% antidesiccant, the dispersion agent of 4%-10%.
9. the preparation method of inorganic optical disclour printing ink as claimed in claim 5, it is characterized in that: step 4, be that finely dispersed mixed solution in step 3 is taken out and puts into lucifuge ball grinder, the lanthanium titanate oxide compound of the silver that is 15%-25% by mass ratio doping is put into ball grinder, after ball milling 3h, takes out.
10. the preparation method of the inorganic optical disclour printing ink as described in claim 5-9 any one, is characterized in that:
In step 1, when roasting pigment, temperature rise rate is 5 ℃/min;
In step 3, the jitter time of mixed solution in dispersion machine is 60-90min;
In step 4, drum's speed of rotation is turn/min of 950-1200.
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| CN201310703821.7A CN103804986B (en) | 2013-12-19 | 2013-12-19 | Inorganic optical color shifting ink and manufacture method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154290A (en) * | 2020-01-15 | 2020-05-15 | 吉安市中意陶瓷化工有限公司 | Preparation method of silver red ceramic pigment |
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| CN111154290A (en) * | 2020-01-15 | 2020-05-15 | 吉安市中意陶瓷化工有限公司 | Preparation method of silver red ceramic pigment |
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