CN105086629A - Preparation method and application of ultraviolet fluorescent powdered ink - Google Patents
Preparation method and application of ultraviolet fluorescent powdered ink Download PDFInfo
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- CN105086629A CN105086629A CN201510575289.4A CN201510575289A CN105086629A CN 105086629 A CN105086629 A CN 105086629A CN 201510575289 A CN201510575289 A CN 201510575289A CN 105086629 A CN105086629 A CN 105086629A
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Abstract
The invention provides a preparation method of ultraviolet fluorescent powdered ink. The method comprises the following steps: (1) preparing a polyester dispersion; (2) preparing an ultraviolet fluorescent pigment dispersion; (3) preparing a polyester dispersion containing a charge control agent; and (4) mixing the polyester dispersion in the step (1), the ultraviolet fluorescent pigment dispersion in the step (2), a wax emulsion and the polyester dispersion containing a charge control agent in the step (3) to obtain the powdered ink grains which have a proper granular diameter and a core-shell structure. The invention further provides the powdered ink granules prepared by the method and an application thereof.
Description
Technical field
The present invention relates to Ultraluminescence ink powder and preparation method thereof, belong to false proof Ultraluminescence ink powder field.
Background technology
Along with the development of office automation, the application of Laser Printing in work and life is increasingly extensive, and various ticket and trade mark and outsourcing etc. also instead of traditional printing process with Laser Printing.Being becoming increasingly rampant of fake and inferior commodities, the diversity of type of merchandize and the aesthetic property of printing are had higher requirement to antiforge material and technology.By Ultraluminescence ink powder (toner) for anti-counterfeit printing, there is the advantages such as enforcement is simple, cost is low, good concealment, bright in luster, inspection is convenient, thus also become study hotspot both domestic and external.Its false proof principle is in toner, add visible fluorescence (network) compound having ultraviolet and excite, and under UV-light (200 ~ 400nm) is irradiated, can send the extraordinary ink powder of visible ray (400 ~ 800nm).Coloured Ultraluminescence ink powder, colourless Ultraluminescence ink powder two kinds is divided into or without color according to printing toner.Coloured Ultraluminescence ink powder is that the compound with fluorescence is added in coloured ink powder, and the picture and text naked eyes of printing are visible; Colourless Ultraluminescence ink powder is that the compound with fluorescence is added in colourless ink powder, and the picture and text naked eyes of printing are invisible, demonstrates distinct fluorescence under ultraviolet light.
The using and report existing longer history of colourless fluoresent printing ink, because its preparation process is loaded down with trivial details, use a large amount of organic solvent, these shortcomings more and more denounce by everybody.Colourless Ultraluminescence ink powder prepares and use procedure is simple to operate, disposal of pollutants is few, has more wide prospect in Application in Anti-counterfeiting.The relevant colourless Ultraluminescence ink powder preparation method of current report mainly adopts physical method to prepare, the toner particle obtained like this has shape regularity and the shortcoming such as homogeneity of ingredients is poor, size-grade distribution is wide, and Physical preparation method process energy consumption is high besides, dust hazard is larger.This area is urgently developed new method and is solved the above-mentioned problems in the prior art.
Summary of the invention
One aspect of the present invention provides a kind of preparation method of Ultraluminescence ink powder, comprising:
1) polyester dispersion is prepared;
2) Ultraluminescence dispersible pigment dispersion is prepared;
3) preparation is containing the polyester dispersion of charge adjusting agent;
4) by step 1) polyester dispersion, step 2) Ultraluminescence dispersible pigment dispersion, wax emulsion and step 3) the polyester dispersion containing charge adjusting agent mix, obtain the toner particles of appropriate particle size.
According to the present invention, described dispersion liquid can be aqueous-based dispersions.Preferably, described dispersion liquid is made up of deionized water.
As required, described dispersion liquid can also comprise dispersion agent.
According to the present invention, above-mentioned one or more step can be carried out respectively by following methods:
1) vibrin is dissolved in organic solvent, the deionized water then added containing dispersion agent carries out emulsification, steams organic solvent, obtains polyester dispersion;
2) Ultraluminescence pigment, dispersion agent, deionized water are disperseed, obtain Ultraluminescence dispersible pigment dispersion;
3) vibrin, charge adjusting agent are dissolved in organic solvent, the deionized water then added containing dispersion agent carries out emulsification, steams organic solvent, obtains the polyester dispersion containing charge adjusting agent;
4) by step 1) polyester dispersion, step 2) Ultraluminescence dispersible pigment dispersion and wax emulsion mixing, adjust ph and temperature are to control particle diameter; Add the polyester dispersion containing charge adjusting agent again, adjust ph and temperature, obtain toner particles.
Preparation in accordance with the present invention, preferably,
Step 1) in:
Described organic solvent is hot organic solvent.The temperature of described hot organic solvent can be such as higher than the temperature of room temperature, is specifically as follows 30 ~ 50 DEG C.
Optionally, step 1) also comprise the step heating organic solvent.Exemplarily, can organic solvent be heated, then vibrin is dissolved in organic solvent; Or, vibrin is added organic solvent, then heats organic solvent with dissolved polyester resin.
Step 2) in:
Ultraluminescence pigment used in the present invention comprises can at wavelength 200 ~ 400nm, such as, inspire the colorless fluorescent compound of visible red or green glow or blue light under the UV-light of 365nm, or by the composite colorless fluorescent mixture that can inspire visible ray under ultraviolet light obtained.Described fluorescent chemicals can be mineral compound and/or organic compound.Such as, described mineral compound can be selected from following one or more: mineral dye, such as with yttrium oxide, sulfurated lime etc. for matrix, the pigment such as the Ultraluminescence red, green, blue being activator with rare earth element (such as europium), and pigment dyestuff, such as comprise the complex compound of rare earth element (such as europium) and organic ligand, carbocyclic ring or heterocyclic compound as compound and derivatives thereof such as toluylene, tonka bean camphor, pyrazoline, benzo oxygen nitrogen, Phthalimide.
The mass ratio of described Ultraluminescence pigment, dispersion agent, deionized water can be any suitable ratio.Such as, its quality can be 10 ~ 100:1 ~ 10:100 ~ 200 than scope, and such as 30 ~ 50:2 ~ 4:150 ~ 200, are specifically as follows 40:3:170 or 40:4:170.
Preferably, described Ultraluminescence dispersible pigment dispersion is prepared by ball milling.
According to the present invention, described vibrin: Ultraluminescence pigment: wax: the quality of charge adjusting agent can be 50 ~ 100:5 ~ 40:1 ~ 20:1 ~ 10 than scope, such as 70 ~ 85:10 ~ 20:5 ~ 10:1 ~ 5.
Described vibrin can be selected from crystalline resins and unformed resin one or more, such as, in optional autohemagglutination dimethyl terephthalate (DMT), poly bisphenol resin, polyethylene terephthalate, polybutylene terephthalate, poly-(ethene-succinate), copolymerization (propene-1-butene-ethylene glycol terephthalate) one or more; Exemplarily, described vibrin can be selected from such as poly terephthalic acid dimethyl ester, poly bisphenol resin or its mixture.
The example of organic solvent can comprise one or more the mixture in ketones solvent, alcoholic solvent and ether solvent.
Described alcoholic solvent can be C
1-20alcohol, be such as selected from one or more mixture following: ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol etc.
Described ketones solvent can be C
3-20ketone, be such as selected from one or more mixture following: acetone, butanone, methyl propyl ketone, methyl isopropyl Ketone, methyl iso-butyl ketone (MIBK) etc.
Described ether solvent can be C
2-
20ether, be such as selected from one or more mixture following: dibutyl ether, Isosorbide-5-Nitrae-dioxane, tetrahydrofuran (THF) etc.
The specific examples of organic solvent of the present invention is butanone, Virahol, acetone, or wherein one or more mixture.
Dispersion agent used in the present invention is not particularly limited, such as can be selected from the compound with surface active properties, example is one or more in Sodium dodecylbenzene sulfonate, AKYPORLM100, sodium stearate, sodium dibutyl naphthalene sulfonate, sodium laurylsulfonate and sodium lauryl sulphate.
Preferably, the dispersion particle size of each step gained of the inventive method is no more than 800nm, such as be no more than 700nm, 600nm, 500nm, 400nm, 300nm or 200nm, such as 100-200nm, or 150-200nm, solid content is 5-50wt%, such as 10-40wt%, 15-35wt%, such as 20wt%.
Charge adjusting agent used in the present invention (CCA) is not particularly limited, and can be selected from charge control agent known in the art according to predetermined object.The example comprises following one or more: the metal-salt of triphenylmethane dye, molybdic acid inner complex pigment, rhodamine dyes, alkoxylamine, quaternary ammonium salt (comprising the quaternary ammonium salt of fluorine richness), alkylamide, phosphorus, phosphorus compound, tungsten, tungsten compound, fluorine-based active agents, salicylic metal-salt and salicyclic acid derivatives.Preferably, described charge adjusting agent can be that salicylic acid metal salt is as salumin, zinc salicylate or its mixture.
According to the present invention, described emulsification is realized by mulser, and rotating speed can be 5000rpm ~ 20000rpm, and emulsification times can be 10min ~ 40min.
Preferably, preparation method of the present invention also comprises step 5): add the compositions such as fluidity enhancers and mix with the Ultraluminescence ink powder obtaining being applicable to the false proof requirement of Laser Printing.
Described fluidity enhancers is preferably modified manometer silicon dioxide, and add-on is preferably 0.1% ~ 3% of toner mass.
The present invention provides the toner particles prepared by aforesaid method on the other hand.
According to the present invention, described ink powder is the particle with core-shell structure, and charge adjusting agent disperses in shell.Preferably, the particle diameter of described toner particles is 5-10 μm.
The present invention further provides described toner particles and prepare the purposes in ink.Preferably, described ink can be used for anti-counterfeiting printing and printing.
Preparation method of the present invention and the ink powder obtained have the following advantages:
1) gathering-fusion method of the present invention prepares Ultraluminescence ink powder, has that technique is simple, easy and simple to handle, the characteristic craft of environmental protection is simple, energy-conserving and environment-protective, production efficiency is high.
2) can provide the ink powder of enough charge carrier abilities, satisfactory thermal parameters, appropriate particle size and anti-counterfeiting performance, it is suitable for being applied in anti-counterfeiting printing and printing.
3) use method of the present invention can obtain coated even, high yield, the Ultraluminescence ink powder of high-quality Laser Printing and false proof requirement can be met.
4) toner using the inventive method to obtain prints specimen page in the sunlight for colourless or white, demonstrates distinct fluorescence under ultraviolet light.
Embodiment
Below by way of embodiment, foregoing of the present invention is described in further detail.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1:
The preparation of polyester dispersion: 100 grams of vibrin (poly terephthalic acid dimethyl ester) are added 400 grams of butanone solutions, is heated to 70 DEG C to dissolving as A bottle completely.Deionized water 400 grams containing 5 grams of Sodium dodecylbenzene sulfonatees is heated to 75 DEG C as B bottle.A bottle is added B bottle, mixed solution (15 minutes x2 time) is processed with high-speed emulsifying machine (being adjusted to 10000rpm), 80 DEG C steam butanone solvent recycling design, obtain the aqueous-based dispersions (particle diameter ~ 190nm, solid content 20wt.%) of vibrin (poly terephthalic acid dimethyl ester).
The preparation of Ultraluminescence dispersible pigment dispersion: in 500 milliliters of ball grinders that zirconium pearl is housed, adds 40 grams of Ultraluminescence pigment, deionized water 170 grams containing 3 grams of Sodium dodecylbenzene sulfonatees, stirs (500rpm) and mixes for 0.5 hour; With 6000rpm speed ball milling 3 hours, the aqueous-based dispersions (particle diameter ~ 450nm, solid content ~ 20wt.%) of Ultraluminescence pigment can be obtained.
Preparation containing the polyester dispersion of charge adjusting agent: 20 grams of CCA zinc salicylates, 80 grams of vibrin (poly terephthalic acid dimethyl ester) are added 300 grams of butanone solutions, is heated to 70 DEG C to dissolving as A bottle completely.Deionized water 300 grams containing 5 grams of Sodium dodecylbenzene sulfonatees is heated to 75 DEG C as B bottle.A bottle is added B bottle, mixed solution (15 minutes x2 time) is processed with high-speed emulsifying machine (being adjusted to 10000rpm), 80 DEG C steam butanone solvent recycling design, obtain vibrin (poly terephthalic acid dimethyl ester) aqueous-based dispersions (particle diameter ~ 198nm, CCA content 5wt.%) containing charge adjusting agent.
The preparation of Ultraluminescence ink powder: in the pressure reaction still of 500 milliliters, add polyester dispersion (150 grams, 20wt.%), Ultraluminescence dispersible pigment dispersion (25 grams, 20wt.%) and wax emulsion (15 grams, 20wt.%, commercial commodity), then add the deionized water 100 grams containing 1 gram of Sodium dodecylbenzene sulfonate, mixing and stirring; The pH value of regulation system is to about 1 and be heated to 50 – 60 DEG C, controls particle diameter to 2-5 μm; Add the polyester dispersion (30 grams containing charge adjusting agent zinc salicylate, CCA5wt.%), strong stirring (2000 – 5000rpm) 1 – 3 hours, after particle diameter reaches 5-10 μm, adjust ph is 7.5, and raised temperature to 95 DEG C stirs 3 – 5 hours; Cool, filter, wash, dry, obtain ink powder (powder is subsphaeroidal, particle diameter 5 – 10 μm), then add modified manometer silicon dioxide, fluidity enhancers etc. are outer adds composition, obtains the Ultraluminescence ink powder being applicable to the false proof requirement of Laser Printing.
Embodiment 2:
The preparation of polyester dispersion: 100 grams of vibrin (poly bisphenol resin) are dissolved in 400 grams of aqueous isopropanols, add 400 grams of deionized waters containing 5 grams of AKYPORLM100, mixed solution (15 minutes x2 time) is processed with high-speed emulsifying machine (being adjusted to 10000rpm), steam isopropanol solvent, obtain the aqueous-based dispersions (particle diameter ~ 180nm, solid content 20wt.%) of vibrin (poly bisphenol resin).
The preparation of Ultraluminescence dispersible pigment dispersion: in 500 milliliters of ball grinders that zirconium pearl is housed, adds the deionized water 170 grams of 40 grams of Ultraluminescence pigment, 2 grams of RLM100,2 grams of sodium dibutyl naphthalene sulfonates, stirs (500rpm) and mixes for 0.5 hour; With 6000rpm speed ball milling 3 hours, the aqueous-based dispersions (particle diameter ~ 500nm, solid content ~ 20wt.%) of Ultraluminescence pigment can be obtained.
Preparation containing the polyester dispersion of charge adjusting agent: 20 grams of CCA salumins, 80 grams of vibrin (poly bisphenol resin) are added 400 grams of aqueous isopropanols, is heated to 70 DEG C to dissolving as A bottle completely.Deionized water 300 grams containing 5 grams of Sodium dodecylbenzene sulfonatees is heated to 75 DEG C as B bottle.A bottle is added B bottle, mixed solution (15 minutes x2 time) is processed with high-speed emulsifying machine (being adjusted to 10000rpm), 80 DEG C steam isopropanol recovering solvent, obtain vibrin (poly bisphenol resin) aqueous-based dispersions (particle diameter ~ 198nm, CCA content 5wt.%) containing charge adjusting agent.
The preparation of Ultraluminescence ink powder: in the pressure reaction still of 500 milliliters, add polyester dispersion (160 grams, 20wt.%), Ultraluminescence dispersible pigment dispersion (28 grams, 20wt.%), wax emulsion (15 grams, 20wt.%, commercial commodity) add deionized water 100 grams containing 1 gram of Sodium dodecylbenzene sulfonate, mixing and stirring again; The pH value of regulation system is to about 1 and be heated to 50 – 60 DEG C, controls particle diameter to 2-5 μm; Add the polyester dispersion (40 grams, CCA5wt.%) of charge adjusting agent salumin, strong stirring (2000 – 5000rpm) 1 – 3 hours, after particle diameter reaches 5-10 μm, adjust ph is 7.5, raised temperature to 95
0c stirs 3 – 5 hours; Cool, filter, wash, dry, obtain ink powder (powder is subsphaeroidal, particle diameter 5 – 10 μm), then add as fluidity enhancers etc. adds composition outward, obtain the Ultraluminescence ink powder being applicable to the false proof requirement of Laser Printing.
The present invention is illustrated by above specific examples.It is pointed out that in spirit of the present invention and the scope stated, some changes and amendment can be made.Therefore, above-mentioned specific embodiment is non-for limiting the present invention.
Claims (10)
1. a preparation method for Ultraluminescence ink powder, comprising:
1) polyester dispersion is prepared;
2) Ultraluminescence dispersible pigment dispersion is prepared;
3) preparation is containing the polyester dispersion of charge adjusting agent;
4) by step 1) polyester dispersion, step 2) Ultraluminescence dispersible pigment dispersion, wax emulsion and step 3) the polyester dispersion containing charge adjusting agent mix, obtain the toner particles of appropriate particle size;
Wherein said dispersion liquid can be aqueous-based dispersions, and preferably, described dispersion liquid is made up of deionized water.
2. preparation method according to claim 1, wherein one or more steps can be carried out respectively by following methods:
1) vibrin is dissolved in organic solvent, the deionized water then added containing dispersion agent carries out emulsification, steams organic solvent, obtains polyester dispersion;
2) Ultraluminescence pigment, dispersion agent, deionized water are disperseed, obtain Ultraluminescence dispersible pigment dispersion;
3) vibrin, charge adjusting agent are dissolved in organic solvent, the deionized water then added containing dispersion agent carries out emulsification, steams organic solvent, obtains the polyester dispersion containing charge adjusting agent;
4) by step 1) polyester dispersion, step 2) Ultraluminescence dispersible pigment dispersion and wax emulsion mixing, adjust ph and temperature are to control particle diameter; Add the polyester dispersion containing charge adjusting agent again, adjust ph and temperature, obtain toner particles; And optionally,
5) add the compositions such as fluidity enhancers (modified manometer silicon dioxide as toner particles quality 0.1% ~ 3%) and mix with the Ultraluminescence ink powder obtaining being applicable to the false proof requirement of Laser Printing.
3. the preparation method described in claim 1 or 2, wherein said vibrin: Ultraluminescence pigment: wax: the quality of charge adjusting agent can be 50 ~ 100:5 ~ 40:1 ~ 20:1 ~ 10 than scope, such as 70 ~ 85:10 ~ 20:5 ~ 10:1 ~ 5.
4. the preparation method described in any one of claim 1-3, wherein said vibrin can be selected from crystalline resins and unformed resin one or more, such as, in optional autohemagglutination dimethyl terephthalate (DMT), poly bisphenol resin, polyethylene terephthalate, polybutylene terephthalate, poly-(ethene-succinate), copolymerization (propene-1-butene-ethylene glycol terephthalate) one or more; Exemplarily, described vibrin can be selected from such as poly terephthalic acid dimethyl ester, poly bisphenol resin or its mixture.
5. the method described in any one of claim 1-4, containing dispersion agent in wherein said dispersion liquid, described dispersion agent is preferably selected from the compound with surface active properties, and example is one or more in Sodium dodecylbenzene sulfonate, RLM100, sodium stearate, sodium dibutyl naphthalene sulfonate, sodium laurylsulfonate and sodium lauryl sulphate.
6. the method described in any one of claim 1-5, wherein said charge adjusting agent is selected from charge control agent known in the art, such as, comprise following one or more: the metal-salt of triphenylmethane dye, molybdic acid inner complex pigment, rhodamine dyes, alkoxylamine, quaternary ammonium salt (comprising the quaternary ammonium salt of fluorine richness), alkylamide, phosphorus, phosphorus compound, tungsten, tungsten compound, fluorine-based active agents, salicylic metal-salt and salicyclic acid derivatives; Preferably, described charge adjusting agent can be that salicylic acid metal salt is as salumin, zinc salicylate or its mixture.
7. the preparation method described in any one of claim 1-6, wherein step 1) also comprise the step heating organic solvent.
8. the toner particles that described in any one of claim 1-7, preparation method prepares.
9. toner particles according to claim 8, it is the particle with core-shell structure, and charge adjusting agent disperses in shell; Preferably, the particle diameter of described toner particles is 5-10 μm.
10. toner particles according to claim 8 is in preparation Laser Printing ink powder, especially for the purposes in anti-counterfeiting printing and printing.
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| CN201510575289.4A CN105086629A (en) | 2015-09-10 | 2015-09-10 | Preparation method and application of ultraviolet fluorescent powdered ink |
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| CN201510575289.4A CN105086629A (en) | 2015-09-10 | 2015-09-10 | Preparation method and application of ultraviolet fluorescent powdered ink |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107329381A (en) * | 2017-08-29 | 2017-11-07 | 邯郸汉光办公自动化耗材有限公司 | Color toner and preparation method thereof and the method for digital thermal transfer printing |
| CN107880768A (en) * | 2017-11-29 | 2018-04-06 | 张家港宝视特影视器材有限公司 | A kind of coating material for plastics curtain and preparation method thereof |
| CN108034358A (en) * | 2017-11-29 | 2018-05-15 | 张家港宝视特影视器材有限公司 | A kind of projection screen fluoresent coating material and preparation method thereof |
| CN110068992A (en) * | 2018-01-24 | 2019-07-30 | 施乐公司 | Safe ink powder and its application method |
| CN113087834A (en) * | 2021-04-15 | 2021-07-09 | 联想万像(深圳)科技有限公司 | Fluorescent ink powder and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103869644A (en) * | 2014-02-28 | 2014-06-18 | 湖北鼎龙化学股份有限公司 | Polyester type color powdered ink and preparation method thereof |
-
2015
- 2015-09-10 CN CN201510575289.4A patent/CN105086629A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103869644A (en) * | 2014-02-28 | 2014-06-18 | 湖北鼎龙化学股份有限公司 | Polyester type color powdered ink and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107329381A (en) * | 2017-08-29 | 2017-11-07 | 邯郸汉光办公自动化耗材有限公司 | Color toner and preparation method thereof and the method for digital thermal transfer printing |
| CN107880768A (en) * | 2017-11-29 | 2018-04-06 | 张家港宝视特影视器材有限公司 | A kind of coating material for plastics curtain and preparation method thereof |
| CN108034358A (en) * | 2017-11-29 | 2018-05-15 | 张家港宝视特影视器材有限公司 | A kind of projection screen fluoresent coating material and preparation method thereof |
| CN110068992A (en) * | 2018-01-24 | 2019-07-30 | 施乐公司 | Safe ink powder and its application method |
| CN113087834A (en) * | 2021-04-15 | 2021-07-09 | 联想万像(深圳)科技有限公司 | Fluorescent ink powder and application thereof |
| CN113087834B (en) * | 2021-04-15 | 2022-10-04 | 联想万像(深圳)科技有限公司 | Fluorescent ink powder and application thereof |
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Inventor after: Fan Xinheng Inventor after: Zhang Lipeng Inventor after: Yang Lianming Inventor before: Fan Xinheng Inventor before: Zhang Lipeng Inventor before: Xu Shoumin Inventor before: Yang Lianming |
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