CN114702859B - Fluorescent ink with good transfer printing capability and preparation method thereof - Google Patents
Fluorescent ink with good transfer printing capability and preparation method thereof Download PDFInfo
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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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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- 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
- C09D11/30—Inkjet printing 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
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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Abstract
The invention discloses fluorescent ink with good transfer printing capability and a preparation method thereof, wherein the fluorescent ink is prepared from the following raw materials: p (St-co-AM) microspheres, a stabilizer, a fluorescent agent, carbon black, a binder, a sodium dodecyl sulfate solution, cobalt isooctanoate, polyethylene wax and a solvent; the P (St-co-AM) microspheres can be effectively combined with fluorescent dye, so that the fluorescent dye has stronger tinting strength, the branching effect of the stabilizer obviously improves the dispersibility of the ink, the ink can be better transferred to a printing stock during printing, the transfer printing transfer capability is good, the stability is improved, and the fluorescent effect is good; the preparation method comprises the steps of prepolymerization, microsphere coloring and ultrasonic dispersion, the prepared fluorescent ink toner is fine and young, and the cavitation of ultrasonic waves not only breaks the dyed microspheres into finer pigment particles, but also enables monomer beads to be suspended and dispersed into smaller droplets, so that the phenomenon of ink piling faults caused by accumulation of ink pigment particles is reduced.
Description
Technical Field
The invention relates to the technical field of fluorescent ink, in particular to fluorescent ink with good transfer printing capability and a preparation method thereof.
Background
The main component of the fluorescent ink is a fluorescent agent, which is also called fluorescent dye, absorbs energy of a certain form to excite photons, and releases the absorbed energy in a low visible light form, so that a fluorescence phenomenon is generated. How to effectively combine the fluorescent agent with the printing ink is the subject of the current research on fluorescent ink.
The high-quality fluorescent ink generally needs 65-75% of imported fluorescent ink essence to reach the standard, and the low-grade and low-cost fluorescent ink has the conditions of piling ink and excessive emulsification because no specially selected binder/auxiliary agent is adopted, even if the content of the fluorescent ink essence is increased to make the concentration higher, 1) 3-5 hundred printed pieces are printed in printing cannot be avoided; 2) The ink is not uniformly transferred to the substrate during printing because of the difficulty in dispersing the ink.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides fluorescent ink with good transfer printing capability and a preparation method thereof.
The technical scheme adopted for solving the technical problems is as follows:
a fluorescent ink with good transfer printing capability is prepared from the following raw materials in parts by weight: 1-5 parts of P (St-co-AM) microspheres, 0.3-0.5 part of stabilizer, 1-2 parts of fluorescent agent, 3-5 parts of carbon black, 10-20 parts of connecting material, 0.4-0.6 part of sodium dodecyl sulfate solution, 0.4-0.6 part of cobalt iso-octoate, 5-8 parts of polyethylene wax and 80-90 parts of solvent; the P (St-co-AM) microsphere is prepared from the following raw materials in parts by weight: 10-15 parts of styrene, 10-15 parts of acrylamide, 1-3 parts of ammonium persulfate, 3-5 parts of dibenzoyl peroxide and 60-70 parts of deionized water.
The preparation method of the P (St-co-AM) microsphere comprises the following steps:
(1) And adding the dibenzoyl peroxide, ammonium persulfate and deionized water in parts by weight into a high-temperature reaction kettle filled with nitrogen, and starting stirring at a stirring speed of 40-50r/min for 30min to obtain a mixed solution A.
(2) Dropwise adding the acrylamide in parts by weight into the mixed solution A through a flow liquid injector while stirring, wherein the stirring speed is 80-90r/min, and the stirring time and the dropwise adding time are 2-3min, so as to obtain the mixed solution B.
(3) Transferring the mixed solution B to a water bath kettle for heating, heating to 90-95 ℃, then dripping the styrene in parts by weight through a flow liquid injector for 2-3min, carrying out heat preservation reaction for 2-3 h after dripping, starting stirring after heat preservation, cooling to room temperature, and obtaining the mixed solution C at the stirring speed of 50-60 r/min.
(4) And filtering and removing the large-particle polymer in the mixed solution C by using a filter to obtain filtrate, namely the P (St-co-AM) microspheres.
The connecting material is one of rosin modified phenolic resin, modified alkyd resin and asphalt resin.
The stabilizer is one of hydroxypropyl cellulose and polyethylene glycol.
The concentration of the sodium dodecyl sulfate solution is 0.08-0.14g/L.
The solvent consists of isopropanol and ethanol in a ratio of 1:1.
A method of preparing a fluorescent ink as described above, comprising the steps of:
(1) And (3) prepolymerizing: and (3) taking the P (St-co-AM) microspheres, the stabilizer and the solvent in parts by weight, putting the microspheres, the stabilizer and the solvent into a stirring kettle, starting stirring, heating to 60-65 ℃ while stirring, and stirring at the speed of 50-60r/min for 15-20 minutes to obtain the prepolymer.
(2) Coloring the microspheres: adding the fluorescent agent, carbon black, the connecting material, the sodium dodecyl sulfate solution, cobalt isooctanoate and polyethylene wax in parts by weight into the prepolymer solution, heating to 80-90 ℃ while stirring, and stirring at the stirring speed of 50-60r/min until the solution is uniform, thus obtaining the fluorescent solution.
(3) Ultrasonic dispersion: transferring the fluorescent solution obtained in the step (2) into an ultrasonic dispersing instrument, and performing ultrasonic dispersion for 10-15min to obtain the fluorescent ink.
The beneficial effects of the invention are as follows:
(1) The invention innovatively prepares the P (St-co-AM) microsphere by using a soap-free emulsion polymerization method, the microsphere can be effectively combined with fluorescent dye, has stronger tinting strength, the branching effect of the stabilizer obviously improves the dispersibility of the ink, so that the ink can be better transferred to a printing stock during printing, the transfer printing transfer capability is good, the stability is improved, and the fluorescent effect is good.
(2) The preparation method comprises the steps of prepolymerization, microsphere coloring and ultrasonic dispersion, the prepared fluorescent ink toner is fine and young, and the cavitation of ultrasonic waves not only breaks the dyed microspheres into finer pigment particles, but also enables monomer beads to be suspended and dispersed into smaller droplets, so that the phenomenon of ink piling faults caused by accumulation of ink pigment particles is reduced.
Detailed Description
In all the embodiments of the present invention, the temperature and the pressure are not particularly emphasized, and are normal temperature and normal pressure, and the use of the device is not particularly described, and the device can be used according to the conventional arrangement.
The present invention will be further described in detail with reference to the following embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be noted that, without conflict, the embodiments of the present invention and features in the embodiments may be combined with each other.
A fluorescent ink with good transfer printing capability is prepared from the following raw materials in parts by weight: 1-5 parts of P (St-co-AM) microsphere, 0.3-0.5 part of stabilizer, 1-2 parts of fluorescent agent, 3-5 parts of carbon black (purchased from Dongguan Brilliant chemical industry Co., ltd.), 10-20 parts of binder and sodium dodecyl sulfate solution (the molecular formula is CH) 3 (CH 2 ) 10 CH 2 OSO 3 Na) 0.4-0.6 part, cobalt iso-octoate (chemical formula is C) 16 H 30 CoO 4 ) 0.4-0.6 parts, polyethylene wax (purchased from Shanghai Kaijin chemical Co., ltd.) 5-8 parts and solvent 80-90 parts.
The P (St-co-AM) microsphere is prepared from the following raw materials in parts by weight: styrene (formula C) 8 H 8 ) 10-15 parts of acrylamide (chemical formula C 3 H 5 NO) 10-15 parts, ammonium persulfate (chemical formula (NH) 4 ) 2 S 2 O 8 ) 1-3 parts of dibenzoyl peroxide (purchased from Jinan Yu chemical Co., ltd.) 3-5 parts and deionized water 60-70 parts, styrene and acrylamide are difficult to polymerize under normal conditions, and the application utilizes a double initiator to prepare the P (St-co-AM) microsphere.
The preparation process of the P (St-co-AM) microsphere comprises the following steps:
(1) And adding the dibenzoyl peroxide, ammonium persulfate and deionized water in parts by weight into a high-temperature reaction kettle filled with nitrogen, and starting stirring at the stirring speed of 80-85r/min for 30min to obtain a mixed solution A.
(2) Dropwise adding the acrylamide in parts by weight into the mixed solution A through a flow liquid injector while stirring, wherein the stirring speed is 80-90r/min, and the stirring time and the dropwise adding time are 2-3min, so as to obtain the mixed solution B.
(3) Transferring the mixed solution B to a water bath kettle for heating, heating to 90-95 ℃, then dripping the styrene in parts by weight through a flow liquid injector for 2-3min, carrying out heat preservation reaction for 2-3 h after dripping, starting stirring after heat preservation, cooling to room temperature, and obtaining the mixed solution C at a stirring speed of 85-90 r/min.
(4) And filtering and removing the large-particle polymer in the mixed solution C by using a filter to obtain filtrate, namely filtrate containing the P (St-co-AM) microspheres.
The reaction equation is as follows:
the invention adopts a soap-free emulsion polymerization method to innovatively prepare the P (St-co-AM) microsphere, wherein the soap-free emulsion refers to a polymerization mode without an emulsifier, and the method effectively avoids the influence of the emulsifier on a reaction system in the emulsion polymerization process, and the prepared polymer microsphere is clean and free of impurities. The hydrophilic group is introduced by adding the functional monomer Acrylamide (AM), so that the interaction between the microsphere surface and the water phase interface is enhanced, the surface energy of the microsphere surface is reduced, the stability of the microsphere is improved, and the polymerization reaction rate is also greatly improved.
However, soap-free emulsion polymerization also has the obvious disadvantage that the particles produced are large in size, typically in the hundreds of nanometers, and therefore an ultrasonic dispersion step must be added during the ink preparation process. The cavitation of the liquid medium is enhanced by the ultrasonic wave, so that the bubble expansion and compression are more intense, and the microspheres coated with the pigment are finer. It was found that the particle size of the dyed microspheres after ultrasonic dispersion was reduced to one third because cavitation of ultrasonic waves not only broken the dyed microspheres into finer pigment particles, but also suspended and dispersed the monomer droplets into smaller droplets, thus making it possible to compensate for the large particle size of the microspheres produced by soap-free emulsion polymerization by ultrasonic dispersion and making the final dyed microspheres smaller in size.
The P (St-co-AM) microsphere preparation process is affected by the stirring speed. The microsphere prepared by the soap-free emulsion polymerization has poor monodispersity, the faster the stirring speed is, the worse the monodispersity is, and through analysis and research, when the stirring speed is 80-90r/min, the shearing speed in a system is relatively moderate, and the particle size of the prepared microsphere is relatively uniform.
The stabilizer is hydroxypropyl cellulose (molecular formula C 36 H 70 O 19 ) Polyethylene-basedPyrrolidone (chemical formula (C) 6 H 9 NO) n ) And polyethylene glycol (chemical formula is HO (CH) 2 CH 2 O) n H) One of them. The stabilizer plays a vital role in the preparation of the fluorescent ink, the used stabilizers are amphiphilic compounds, can be grafted to microsphere molecular chains and positioned on the surfaces of the microspheres, so that the steric stabilization effect is achieved, the microspheres cannot be clustered together, and the dispersibility is good.
The fluorescent agent is preferably a fluorescent whitening agent produced by Jinan Huijian commercial company, and the model is CBS-127.
The carbon black is black powder obtained by partial combustion or thermal cracking decomposition of hydrocarbon, has low cost, strong coloring capability and good stability, and can be effectively combined with the P (St-co-AM) microspheres.
The connecting material is one of rosin modified phenolic resin, modified alkyd resin and asphalt resin. Preferably, the rosin modified phenolic resin can be better combined with the colored microspheres effectively, so that the colored microspheres can be well dispersed and transferred to the surface of a printing stock through a printing machine.
The sodium dodecyl sulfate solution is used as an emulsifier in a system, the concentration of the sodium dodecyl sulfate solution is 0.08-0.14g/L, the concentration of the sodium dodecyl sulfate solution used in the invention is far less than the critical micelle concentration (about 2.3 g/L) of the sodium dodecyl sulfate solution, no micelle is formed by the emulsifier in the polymerization process, and when the oligomer with hydrophilic groups at the chain ends reaches the critical micelle concentration, oligomer micelles are formed close to each other, a monomer is solubilized, a reaction nucleus is formed, and therefore, the colored microsphere with good monodispersity can be obtained.
The cobalt iso-octoate is an oxidation type drying agent, has extremely strong drying capacity, and particularly promotes surface drying. The cobalt iso-octoate adopted by the invention plays a role in accelerating the drying of the oxidation conjunctiva of the ink, also called a drier, and is one of the most important auxiliary agents. Common driers are metal driers such as manganese driers, but the driers have poor drying effect and are not generally used for printing ink.
The polyethylene wax is used as an antifriction aid, and can be added into the ink to enable the polyethylene wax to float on an ink film after being printed on a printing stock so as to increase the antifriction property. The amount of polyethylene wax used is critical to the performance of the ink, directly affecting the ink flow, transfer and gloss.
The applicant has also investigated the effect of temperature on the condition of staining of microspheres. Research shows that in the temperature range of 80-90 ℃, dye molecules are easier to enter the microsphere at higher temperature, dye molecules are more difficult to diffuse at lower temperature, and dye is gathered on the surface of the microsphere or in a shallower layer, so that the color development effect of the prepared fluorescent ink is poor.
The invention uses a heating copolymerization method to color P (St-co-AM) microspheres, and the principle is that a fluorescent agent is inlaid on the expanded microspheres in a heating mode, the microspheres are expanded by heating, and carbon black is diffused into the microspheres, so that the microspheres are colored.
A method of preparing a fluorescent ink as described above, comprising the steps of:
(1) And (3) prepolymerizing: and (3) taking the P (St-co-AM) microspheres, the stabilizer and the solvent in parts by weight, putting the microspheres, the stabilizer and the solvent into a stirring kettle, starting stirring, heating to 60-65 ℃ while stirring, and stirring at the speed of 50-60r/min for 15-20 minutes to obtain the prepolymer.
(2) Coloring the microspheres: adding the fluorescent agent, carbon black, the connecting material, the sodium dodecyl sulfate solution, cobalt isooctanoate and polyethylene wax in parts by weight into the prepolymer solution, heating to 80-90 ℃ while stirring, and stirring at the stirring speed of 50-60r/min until the solution is uniform, thus obtaining the fluorescent solution.
(3) Ultrasonic dispersion: transferring the fluorescent solution obtained in the step (2) into an ultrasonic dispersing instrument, and performing ultrasonic dispersion for 10-15min to obtain the fluorescent ink.
Example 1: 3 parts of P (St-co-AM) microsphere, 0.4 part of stabilizer, 1.5 parts of fluorescent agent, 4 parts of carbon black, 15 parts of connecting material, 0.5 part of sodium dodecyl sulfate solution, 0.5 part of cobalt iso-octoate, 6 parts of polyethylene wax and 85 parts of solvent.
The preparation procedure of example 1 is as follows:
(1) And (3) prepolymerizing: and (3) taking the P (St-co-AM) microspheres, the stabilizer and the solvent in parts by weight, putting the microspheres, the stabilizer and the solvent into a stirring kettle, starting stirring, heating to 60 ℃ while stirring, and obtaining the prepolymer liquid at the stirring speed of 50r/min for 15 minutes.
(2) Coloring the microspheres: adding the fluorescent agent, carbon black, the connecting material, the sodium dodecyl sulfate solution, cobalt isooctanoate and polyethylene wax in parts by weight into the prepolymer solution, heating to 90 ℃ while stirring, and stirring at the speed of 50r/min until the solution is uniform, thus obtaining the fluorescent solution.
(3) Ultrasonic dispersion: transferring the fluorescent solution obtained in the step (2) into an ultrasonic dispersing instrument, and performing ultrasonic dispersion for 10min to obtain the example 1.
Example 2: 3 parts of polystyrene microsphere (purchased from Dongguan, michaelia new materials Co., ltd.), 0.4 part of stabilizer, 1.5 parts of fluorescent agent, 4 parts of carbon black, 15 parts of connecting material, 0.5 part of sodium dodecyl sulfate solution, 0.5 part of cobalt iso-octoate, 6 parts of polyethylene wax and 85 parts of solvent.
The procedure for the preparation of example 2 is as follows:
(1) And (3) prepolymerizing: and (3) taking the polystyrene microspheres, the stabilizer and the solvent in parts by weight, putting the polystyrene microspheres, the stabilizer and the solvent into a stirring kettle, starting stirring, heating to 60 ℃ while stirring, and obtaining the prepolymer liquid at the stirring speed of 50r/min for 15 minutes.
(2) Coloring the microspheres: adding the fluorescent agent, carbon black, the connecting material, the sodium dodecyl sulfate solution, cobalt isooctanoate and polyethylene wax in parts by weight into the prepolymer solution, heating to 90 ℃ while stirring, and stirring at the speed of 50r/min until the solution is uniform, thus obtaining the fluorescent solution.
(3) Ultrasonic dispersion: transferring the fluorescent solution obtained in the step (2) into an ultrasonic dispersing instrument, and performing ultrasonic dispersion for 10min to obtain the example 2.
Example 3: 3 parts of P (St-co-AM) microsphere, 1.5 parts of fluorescent agent, 4 parts of carbon black, 15 parts of connecting material, 0.5 part of sodium dodecyl sulfate solution, 0.5 part of cobalt iso-octoate, 6 parts of polyethylene wax and 85 parts of solvent.
The procedure for the preparation of example 3 is as follows:
(1) And (3) prepolymerizing: and (3) taking the P (St-co-AM) microspheres and the solvent in parts by weight, putting the microspheres and the solvent into a stirring kettle, starting stirring, heating to 60 ℃ while stirring, and obtaining the prepolymer liquid at the stirring speed of 50r/min and the stirring time of 15 minutes.
(2) Coloring the microspheres: adding the fluorescent agent, carbon black, the connecting material, the sodium dodecyl sulfate solution, cobalt isooctanoate and polyethylene wax in parts by weight into the prepolymer solution, heating to 90 ℃ while stirring, and stirring at the speed of 50r/min until the solution is uniform, thus obtaining the fluorescent solution.
(3) Ultrasonic dispersion: transferring the fluorescent solution obtained in the step (2) into an ultrasonic dispersing instrument, and performing ultrasonic dispersion for 10min to obtain the example 3.
Example 4: 3 parts of P (St-co-AM) microsphere, 0.4 part of stabilizer, 1.5 parts of fluorescent agent, 4 parts of carbon black, 15 parts of connecting material, 0.5 part of sodium dodecyl sulfate solution, 0.5 part of cobalt iso-octoate, 6 parts of polyethylene wax and 85 parts of solvent.
The procedure for the preparation of example 4 is as follows:
(1) And (3) prepolymerizing: and (3) taking the P (St-co-AM) microspheres and the solvent in parts by weight, putting the microspheres and the solvent into a stirring kettle, starting stirring, heating to 60 ℃ while stirring, and obtaining the prepolymer liquid at the stirring speed of 50r/min and the stirring time of 15 minutes.
(2) Coloring the microspheres: and adding the fluorescent agent, carbon black, a connecting material, a sodium dodecyl sulfate solution, cobalt isooctanoate and polyethylene wax in parts by weight into the prepolymer solution, heating to 90 ℃ while stirring, and stirring at a speed of 50r/min until the solution is uniform to obtain the example 4.
Example 5: 3 parts of P (St-co-AM) microsphere, 0.4 part of stabilizer, 1.5 parts of fluorescent agent, 4 parts of carbon black, 15 parts of connecting material, 0.5 part of sodium dodecyl sulfate solution, 0.5 part of cobalt iso-octoate, 6 parts of polyethylene wax and 85 parts of solvent.
(1) And (3) prepolymerizing: and (3) taking the P (St-co-AM) microspheres, the stabilizer and the solvent in parts by weight, putting the microspheres, the stabilizer and the solvent into a stirring kettle, starting stirring, heating to 60 ℃ while stirring, and obtaining the prepolymer liquid at the stirring speed of 50r/min for 15 minutes.
(2) Coloring the microspheres: adding the fluorescent agent, carbon black, the connecting material, the sodium dodecyl sulfate solution, cobalt isooctanoate and polyethylene wax in parts by weight into the prepolymer solution, heating to 80 ℃ while stirring, and stirring at the stirring speed of 50r/min until the solution is uniform, thus obtaining the fluorescent solution.
(3) Ultrasonic dispersion: transferring the fluorescent solution obtained in the step (2) into an ultrasonic dispersing instrument, and performing ultrasonic dispersion for 10min to obtain the example 5.
The applicant tested the printing effect of examples 1-4, wherein the printing rate was 6000 to 10000 sheets/hour, and the test results showed that:
example 1 the print was smooth, full dots, free from run-off, plate-pasting and piling during printing, and good print adhesion.
Example 2 the printed product had smooth lines and full dots, and the phenomenon of flying ink occurred in the late stage of printing, and the overall print was well attached.
Example 3 the prints were smooth, full dots, no mottle, plate burning and piling during printing, and good print adhesion.
Example 4 the print was smooth, full dots, and the print was printed with ink fly, paste, and pile, with a general print adhesion.
Example 5 the print was smooth, full dots, free from run-off, plate-stick and piling during printing, and the print was generally attached.
The Applicant has carried out measurements of fineness, viscosity, tack-free, tinting strength, adhesion fastness and dye-uptake of examples 1 to 5, wherein:
the fineness is detected according to the standard of GB/T13217.1-91, and the unit is mu m;
the viscosity is measured according to the GB/T13217.1-91 standard, and the unit is (25 ℃ +/-1) S;
the tinting strength was measured according to the standard of GB/T13217.1-91 in (%);
the attachment fastness is detected according to the GB/T13217.1-91 standard, and the unit is (%);
dye uptake is according to Beer-Lambert law, which is essentially that the absorbance of a dilute solution is proportional to its concentration when other conditions are set. And obtaining the dye uptake according to the ratio of the absorbance of the P (St-co-AM) microsphere at the lambda max in the tetrahydrofuran solution to the absorbance of the undyed mixed solution with the same concentration at the lambda max in the tetrahydrofuran solution.
The measurement results are as follows:
| material | Fineness of | Viscosity of the mixture | Tinting strength | Attachment fastness | Dye uptake/% | Luminous intensity/cd |
| Example 1 | 6 | 43 | 102 | 99 | 94.5 | 2.97 |
| Example 2 | 8 | 41 | 97 | 99 | 79.3 | 2.1 |
| Example 3 | 6 | 40 | 100 | 95 | 85.6 | 1.73 |
| Example 4 | 20 | 41 | 101 | 98 | 91.2 | 2.43 |
| Example 5 | 7 | 42 | 99 | 98 | 89.1 | 2.68 |
From the data surface, compared with the prior polystyrene microsphere, the P (St-co-AM) microsphere has stronger coating property and more stability; the P (St-co-AM) microspheres after ultrasonic dispersion are finer, and the coloring capability and the attachment fastness are better; the P (St-co-AM) microsphere and the stabilizer can generate excellent synergistic effect, so that the dye-uptake of the microsphere is increased, and the luminous intensity is good.
The applicant also researches the influence of the types and the proportions of the solvents on the microspheres, but does not form detailed and complete experimental data, and according to the existing experimental data, the types and the proportions of the solvents have great influence on the dye-uptake of the microspheres by combining with preliminary analysis, and the fluorescent effect of the ink is directly influenced. In theory, the solvent used in the invention is composed of isopropanol and ethanol, and the ratio of 1:1 is not the optimal combination.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (5)
1. A method for preparing fluorescent ink with good transfer printing capability is prepared from the following raw materials in parts by weight: 1-5 parts of P (St-co-AM) microspheres, 0.3-0.5 part of stabilizer, 1-2 parts of fluorescent agent, 3-5 parts of carbon black, 10-20 parts of connecting material, 0.4-0.6 part of sodium dodecyl sulfate solution, 0.4-0.6 part of cobalt iso-octoate, 5-8 parts of polyethylene wax and 80-90 parts of solvent;
the method is characterized in that:
the P (St-co-AM) microsphere is prepared from the following raw materials in parts by weight: 10-15 parts of styrene, 10-15 parts of acrylamide, 1-3 parts of ammonium persulfate, 3-5 parts of dibenzoyl peroxide and 60-70 parts of deionized water;
the preparation method of the P (St-co-AM) microsphere comprises the following steps:
(1) Adding the dibenzoyl peroxide, ammonium persulfate and deionized water in parts by weight into a high-temperature reaction kettle filled with nitrogen, and starting stirring at a stirring speed of 40-50r/min for 30min to obtain a mixed solution A;
(2) Dropwise adding the acrylamide in parts by weight into the mixed solution A through a flow liquid injector while stirring, wherein the stirring speed is 80-90r/min, and the stirring time and the dropwise adding time are 2-3min to obtain mixed solution B;
(3) Transferring the mixed solution B to a water bath kettle for heating, heating to 90-95 ℃, then dripping the styrene in parts by weight through a flow liquid injector for 2-3min, carrying out heat preservation reaction for 2-3 h after dripping, starting stirring after heat preservation, cooling to room temperature, and obtaining a mixed solution C at a stirring speed of 50-60 r/min;
(4) Filtering out and removing the large-particle polymer in the mixed solution C by using a filter to obtain filtrate, namely P (St-co-AM) microspheres;
the preparation method of the fluorescent ink comprises the following steps:
(1) And (3) prepolymerizing: taking the P (St-co-AM) microspheres, the stabilizer and the solvent in parts by weight, and stirring in a stirring kettle, heating to 60-65 ℃ while stirring, wherein the stirring speed is 50-60r/min, and the stirring time is 15-20 minutes to obtain a prepolymer liquid;
(2) Coloring the microspheres: adding the fluorescent agent, carbon black, the connecting material, the sodium dodecyl sulfate solution, cobalt isooctanoate and polyethylene wax in parts by weight into the prepolymer solution, heating to 80-90 ℃ while stirring, and stirring at the stirring speed of 50-60r/min until the solution is uniform to obtain a fluorescent solution;
(3) Ultrasonic dispersion: transferring the fluorescent solution obtained in the step (2) into an ultrasonic dispersing instrument, and performing ultrasonic dispersion for 10-15min to obtain the fluorescent ink.
2. The method for preparing fluorescent ink with good transfer printing capability according to claim 1, wherein the binder is one of rosin modified phenolic resin, modified alkyd resin and asphalt resin.
3. The method for preparing fluorescent ink with good transfer ability according to claim 1, wherein the stabilizer is one of hydroxypropyl cellulose and polyethylene glycol.
4. The method for preparing a fluorescent ink with good transfer ability according to claim 1, wherein the concentration of the sodium dodecyl sulfate solution is 0.08-0.14g/L.
5. The method for preparing fluorescent ink with good transfer ability according to claim 1, wherein the solvent consists of isopropanol and ethanol in a ratio of 1:1.
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| CN202210450507.1A CN114702859B (en) | 2022-04-26 | 2022-04-26 | Fluorescent ink with good transfer printing capability and preparation method thereof |
| PCT/CN2022/126749 WO2023206990A1 (en) | 2022-04-26 | 2022-10-21 | Fluorescent ink with good printing capability, and preparation method therefor |
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| CN115839945B (en) * | 2023-02-13 | 2023-06-13 | 上海索昕生物科技有限公司 | Photosensitive microsphere for photoexcitation chemiluminescence detection |
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| JP4692506B2 (en) * | 1994-10-31 | 2011-06-01 | Ｄｉｃ株式会社 | Water-based ink for inkjet recording and method for producing the same |
| US6126731A (en) * | 1998-08-21 | 2000-10-03 | Idea Development Company | Polymerizable ink composition |
| JP5152630B2 (en) * | 2007-09-12 | 2013-02-27 | 株式会社リコー | Ink jet ink and image forming method |
| CN104212087B (en) * | 2014-09-19 | 2017-05-24 | 哈尔滨工业大学 | Preparation method of monodisperse fluorescent microspheres |
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