CN102698668B - Electronic ink microcapsule and preparation method thereof - Google Patents
Electronic ink microcapsule and preparation method thereof Download PDFInfo
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- CN102698668B CN102698668B CN201110350156.9A CN201110350156A CN102698668B CN 102698668 B CN102698668 B CN 102698668B CN 201110350156 A CN201110350156 A CN 201110350156A CN 102698668 B CN102698668 B CN 102698668B
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Abstract
The invention provides an electronic ink microcapsule and a preparation method thereof. The electronic ink microcapsule of the invention comprises a capsule core and a capsule wall coating the capsule core, wherein materials forming the capsule wall comprise acidic nanometer silica sol. According to the invention, the electronic ink microcapsule is obtained by the following steps: mixing the acidic nanometer silica sol aqueous solution and an electrophoretic suspension to form a solid stabilization emulsion; adding an unsaturated carboxylic acid into the solid stabilization emulsion for reaction; adding a water-soluble anionic initiator, then adding other materials forming the capsule wall except the acidic nanometer silica sol to perform heterogeneous polymerization. The electronic ink microcapsule of the invention has low cost, good heat resistance, aging resistance and barrier properties, and high mechanical strength.
Description
Technical field
The present invention relates to a kind of electron ink microcapsule and preparation method thereof, belong to electron ink microcapsule technology.
Background technology
The fast development of information science and technology is calling the plane electronics Display Technique of brand-new slim, light weight, low driving voltage, low-power consumption to adapt with it, and electrophoretic display technology is a kind of of electronic display technology.Microcapsule-type electrophoretic display device (EPD) is a kind of novel electrophoretic display technology (US5961804) that U.S. E-ink company develops, its great advantage is that electrophoresis particle and insulation suspension are packaged in microcapsules, thereby the reunion and the deposition that have suppressed electrophoresis particle, stability and the service life of having improved electrophoretic display device (EPD).The operation principle of Electrophoretic display is a kind of Display Technique of reflection-type based on being suspended in the electrophoresis of the charged particle in decentralized medium, it utilizes principle of electrophoresis to make to be clipped in interelectrode charge species and moves under the effect of electric field, along with the conversion of extra electric field direction, and by two or more different colours of motion Alternation Display of charge species.Microcapsules can large-scale production make display production technology relatively simply and can entire volume automatically produce.Microcapsules may be combined in liquid adhesive and coat on base material by modes such as inkjet printing, brushings, therefore can be used for flexible demonstration.Microcapsule-type electrophoresis showed has very large research and application prospect.Barrett Comiskey etc. seals electrophoresis system with urea-formaldehyde resin microcapsule.Using Lauxite as the wall material of microcapsules, and microcapsules mechanical strength is larger, but pliability is poor, the flexible electrophoretic display scratch resistance of therefore making with this material but withstand voltage properties is poor.
Nakamura etc. have narrated a kind of microcapsules of gelatin-gum arabic system for the preparation method of electrophoretic display device (EPD).Gelatin is a kind of water miscible natural amphoteric macromolecular compound, nontoxic and have good film forming, and its strand is comprised of the different amino acid of many structures, is a kind of valuable raw material for coacervation microencapsulation.Can acid and the amphion electrolyte of alkali formula ionization owing to containing in amino acid molecular simultaneously.When isoelectric point, two kinds of group degree of ionization are equal, and amino acid exists with the form of neutral dipole ion or inner salt, is not subject to the effect of extra electric field.This gelatin is in water, when pH value surpasses isoelectric point, be electronegative, and when pH value positively charged during lower than isoelectric point, thereby need only the pH value of the change aqueous solution, amino acid whose CHARGE DISTRIBUTION can change, and just can control gelatin becomes polycation or polyanion.And in Arabic gum resin, only contain carboxylic group, and in water, be electronegative polyanion, its aqueous solution is not subject to the impact of pH value.Therefore the pH value that can control the aqueous solution, makes gelatin become polycation, and with Arabic gum generation electrostatic interaction, from water, condense and separate out, thereby be attached to, on capsule-core, form cyst wall.The method production efficiency is high, but the high cost of Arabic gum, Arabic gum is easily degraded in addition, the long-term barrier that can reduce capsule that uses.
Therefore be necessary to find the raw material of more low-cost and wide material sources, prepare electron ink microcapsule.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of low cost, high performance electron ink microcapsule and preparation method thereof.
Electron ink microcapsule provided by the present invention, comprises capsule-core and the cyst wall that is coated described capsule-core, and described capsule-core is electrophoresis suspensioning liquid, and the material that wherein forms cyst wall comprises acidic nano-sized silica colloidal sol.
According to an aspect of the present invention, the material of wherein said formation cyst wall also comprises and is selected from styrene, (methyl) methyl acrylate, (methyl) ethyl acrylate, (methyl) butyl acrylate, divinylbenzene, ethylene glycol diacrylate, butanediol double methacrylate, 1,6-hexylene glycol double methacrylate, two contracting propane diols double methacrylates, tripropylene glycol double methacrylate, trimethylolpropane triacrylate, tetramethylol methane tetraacrylate, any one or several in double pentaerythritol C5 methacrylate, double pentaerythritol methacrylate.
Preferably, the material of described formation cyst wall is comprised of acidic nano-sized silica colloidal sol, styrene, methyl methacrylate, butyl methacrylate, trimethylolpropane triacrylate, double pentaerythritol C5 methacrylate and double pentaerythritol methacrylate.
According to an aspect of the present invention, wherein said acidic nano-sized silica colloidal sol is to carry out surface-treated with unsaturated carboxylic acid.
Preferably, wherein said unsaturated carboxylic acid is methacrylic acid or acrylic acid.
The preparation method of electron ink microcapsule provided by the present invention, comprises the steps:
The acidic nano-sized silica colloidal sol aqueous solution is mixed with electrophoresis suspensioning liquid, form Pickering emulsion;
In described Pickering emulsion, add unsaturated carboxylic acid reaction;
Then add water soluble anion type initator, then add the material generation heterogeneous polymerization of other formation cyst walls except acid nano silicon dioxide sol, obtain described electron ink microcapsule.
The described material that other form cyst wall is selected from styrene, (methyl) methyl acrylate, (methyl) ethyl acrylate, (methyl) butyl acrylate, divinylbenzene, ethylene glycol diacrylate, butanediol double methacrylate, 1,6-hexylene glycol double methacrylate, two contracting propane diols double methacrylates, tripropylene glycol double methacrylate, trimethylolpropane triacrylate, tetramethylol methane tetraacrylate, any one or several in double pentaerythritol C5 methacrylate, double pentaerythritol methacrylate.
Preferably, the described material that other form cyst wall is comprised of styrene, methyl methacrylate, butyl methacrylate, trimethylolpropane triacrylate, double pentaerythritol C5 methacrylate and double pentaerythritol methacrylate.
Preferably, described unsaturated carboxylic acid is methacrylic acid or acrylic acid.
Preferably, the mass ratio of described electrophoresis suspensioning liquid and silica is (1～100): 1.
Preferably, the mass ratio of described unsaturated carboxylic acid and silica is (0.3～1): 20.
Preferably, described other form the material of cyst wall and the mass ratio of described Pickering emulsion is (5～45): 100, be preferably (13～25): 100.
The instantiation of described water soluble anion type initator can be potassium peroxydisulfate or ammonium persulfate.
Described electrophoresis suspensioning liquid comprises electrophoresis particle, dyestuff, charge control agent and tetrachloro-ethylene.Electrophoresis particle can be titanium dioxide or silica; Dyestuff can be azo or anthraquinone dyes; Charge control agent is as poly-isosuccinic acid acid anhydride.Electrophoresis suspensioning liquid specifically can comprise 9 quality % electrophoresis particles, 14 quality % dyestuffs, 2 quality % charge control agents and 75 quality % tetrachloro-ethylenes.
Electron ink microcapsule of the present invention adopts the acidic nano-sized silica colloidal sol of cheapness and wide material sources as one of cyst material, has not only reduced the cost of electric ink, and has improved heat resistance, endurance and the barrier of cyst wall.By the carboxyl of unsaturated carboxylic acid and the silicon hydroxyl generation condensation (being shown below) on Ludox surface, realize the chemical bond of inorganic material and organic material, improved mechanical strength and the endurance of microcapsules cyst walls.
Accompanying drawing explanation
Fig. 1 shows the preparation method's of electron ink microcapsule of the present invention flow chart.
The specific embodiment
Electron ink microcapsule of the present invention is prepared as follows:
It is 0.5%～25% that acidic nano-sized silica colloidal sol is diluted with water to mass fraction, and stirring or ultrasonic concussion are uniformly dispersed Nano silica sol particle.Take electrophoresis suspensioning liquid: the mass ratio of silica is (1～100): 1 ratio joins electrophoresis suspensioning liquid in the Ludox of above-mentioned dilution, ultrasonic or high degree of agitation forms Pickering emulsion (Pickering emulsion).In the Pickering emulsion making, add unsaturated carboxylic acid under stirring, be warming up to 50 ℃～90 ℃, wherein the mass ratio of unsaturated carboxylic acid and silica is (0.3～1): 20, react 1～5 hour, add again water soluble anion type initator, slowly drip mix monomer.After dropwising, be warming up to 80 ℃～120 ℃, continue to react individual and be cooled to room temperature after 2～5 hours, discharging, obtains inorganic organic composite electron ink microcapsule.
Above-mentioned electrophoresis suspensioning liquid comprises electrophoresis particle, dyestuff, charge control agent and tetrachloro-ethylene.Electrophoresis particle can be titanium dioxide or silica; Dyestuff can be azo or anthraquinone dyes; Charge control agent is as poly-isosuccinic acid acid anhydride.
Described water soluble anion type initator is potassium peroxydisulfate or ammonium persulfate.
In the preparation of electron ink microcapsule of the present invention, adopt acidic nano-sized silica colloidal sol to form Pickering emulsion as Pickering agent and electrophoresis suspensioning liquid.Pickering emulsion can be thought the stable emulsion by solid particle substitution list surface-active agent (emulsifying agent).Insoluble solid fine powder mixes while disperseing with water and some oil-based solvents, and solid fines is wrapped in the surface of dispersed phase drop, forms a solid encasement; When dispersed phase drop collides mutually, solid encasement plays inhibition to the distortion of drop and gathering, can form comparatively stable emulsion, i.e. Pickering emulsion.Therefore do not use emulsifying agent, avoid emulsifying agent to cover electrophoresis drop surface, hinder the coated of cyst wall, and affect the performance of microcapsule product.
In the preparation of electron ink microcapsule of the present invention, make acidic nano-sized silica Sol-gel Coated on capsule-core (electrophoresis suspensioning liquid) drop surface, form the inorganic particle layer of positively charged, add after anionic initator, initator is electronegative, under electrostatic interaction, initator is attracted to electrophoresis suspensioning liquid particle surface, now drip polymerization single polymerization monomer, can make monomer that heterogeneous polymerization occurs on electrophoresis suspensioning liquid drop top layer and form cyst wall parcel, after reaction finishes, can form inorganic organic composite microcapsules.
In the preparation of electron ink microcapsule of the present invention owing to adopting the inorganic material of this low-carbon (LC) of acidic nano-sized silica colloidal sol, cheapness, wide material sources as one of cyst material, not only reduce the cost of electric ink, and improved heat resistance, endurance and the barrier of cyst wall.By unsaturated carboxylic acid and acidic nano-sized silica colloidal sol generation chemical reaction, realize the chemical bond of inorganic material and organic material, further improved mechanical strength and the endurance of microcapsules cyst walls.
Embodiment 1
2.0g methyl methacrylate, 3.0g butyl methacrylate, 4.0g double pentaerythritol C5 methacrylate are mixed and form mix monomer 1.
5.0g methyl methacrylate, 4.0g styrene, 4.0g butyl methacrylate, 3.0g trimethylolpropane triacrylate are mixed and form mix monomer 2.
The acidic nano-sized silica colloidal sol that is 25% by 50.0g solid content is diluted to 84.0g by deionized water, stirs nano silicon dioxide sol particle and is uniformly dispersed.Add wherein 21.0g electrophoresis suspensioning liquid, the component of electrophoresis suspensioning liquid is: 9 quality % electrophoresis particles, 14 quality % dyestuffs, 2 quality % charge control agents and 75 quality % tetrachloro-ethylenes.Through ultrasonic homogenizing, form Pickering emulsion.Add 0.50g acrylic acid, be warming up to 78 ℃, react 2 hours, add wherein again 1.1g potassium peroxydisulfate initator, and slowly drip successively mix monomer 1, mix monomer 2, after dropwising, be warming up to 90 ℃, react 3 hours, cooling discharge, obtains the electron ink microcapsule of inorganic organic composite.
Embodiment 2
3.0g methyl methacrylate, 2.0g butyl methacrylate, 4.0g double pentaerythritol C5 methacrylate are mixed and form mix monomer 1.
6.0g methyl methacrylate, 1.0g styrene, 4.0g butyl methacrylate, 4.0g trimethylolpropane triacrylate are mixed and form mix monomer 2.
The acidic nano-sized silica colloidal sol that is 25% by 80.0g solid content is diluted to 84.0g by deionized water, stirs nano silicon dioxide sol particle and is uniformly dispersed.Add wherein 20.0g electrophoresis suspensioning liquid, electrophoresis suspensioning liquid component is: 9 quality % electrophoresis particles, 14 quality % dyestuffs, 2 quality % charge control agents and 75 quality % tetrachloro-ethylenes.Through ultrasonic homogenizing, form Pickering emulsion.Add 0.30g acrylic acid, be warming up to 50 ℃, react 5 hours, add wherein again 1.1g potassium peroxydisulfate initator, and slowly drip successively mix monomer 1, mix monomer 2, after dropwising, be warming up to 80 ℃, react 5 hours, cooling discharge, obtains the electron ink microcapsule of inorganic organic composite.
Embodiment 3
3.0g methyl methacrylate, 2.0g butyl methacrylate, 4.0g double pentaerythritol C5 methacrylate are mixed and form mix monomer 1.
5.0g methyl methacrylate, 2.0g styrene, 4.0g butyl methacrylate, 4.0g trimethylolpropane triacrylate are mixed and form mix monomer 2.
The acidic nano-sized silica colloidal sol that is 25% by 2.0g solid content is diluted to 50.0g by deionized water, stirs nano silicon dioxide sol particle and is uniformly dispersed.Add wherein 50.0g electrophoresis suspensioning liquid, electrophoresis suspensioning liquid component is: 9 quality % electrophoresis particles, 14 quality % dyestuffs, 2 quality % charge control agents and 75 quality % tetrachloro-ethylenes.Through ultrasonic homogenizing, form Pickering emulsion.Add 0.025g acrylic acid, be warming up to 90 ℃, react 1 hour, add wherein again 1.1g potassium peroxydisulfate initator, and slowly drip successively mix monomer 1, mix monomer 2, and after dropwising, be warming up to 120 ℃, react 2 hours, cooling discharge, obtains the electron ink microcapsule of inorganic organic composite.
Embodiment 4
Under SEM, observe the electron ink microcapsule preparing in embodiment 1～3, its particle diameter is 1 μ m～5 μ m, is circular, and surface of microcapsule is substantially even, in the visual field without silicon dioxide granule.
Permeability evaluation is soaked the electron ink microcapsule preparing in embodiment 1～3 ultrasonic 30 minutes in acetone soln, and result is without electrophoresis suspensioning liquid seepage.Prove thus electron ink microcapsule that the present invention the prepares excellent in barrier property to electrophoretic medium.
Utilize in addition the electron ink microcapsule preparing in embodiment 1～3 to make Electronic Paper device, picture is by complete black in the white response time is respectively 1.1 seconds, 1.33 seconds and 1.36 seconds entirely after tested, after cutting off the electricity supply, still all can maintain complete white picture, meet the characteristic of electron ink microcapsule bistable display.
Claims (4)
1. a preparation method for electron ink microcapsule, comprises the steps:
The acidic nano-sized silica colloidal sol aqueous solution is mixed with electrophoresis suspensioning liquid, form Pickering emulsion;
In described Pickering emulsion, add unsaturated carboxylic acid reaction;
Then add water soluble anion type initator, then add the material generation heterogeneous polymerization of other formation cyst walls except acid nano silicon dioxide sol, obtain described electron ink microcapsule;
The described material that other form cyst wall is selected from styrene, (methyl) methyl acrylate, (methyl) ethyl acrylate, (methyl) butyl acrylate, divinylbenzene, ethylene glycol diacrylate, butanediol double methacrylate, 1,6-hexylene glycol double methacrylate, two contracting propane diols double methacrylates, tripropylene glycol double methacrylate, trimethylolpropane triacrylate, tetramethylol methane tetraacrylate, any one or several in double pentaerythritol C5 methacrylate, double pentaerythritol methacrylate.
2. preparation method according to claim 1, is characterized in that the described material that other form cyst wall is comprised of styrene, methyl methacrylate, butyl methacrylate, trimethylolpropane triacrylate, double pentaerythritol C5 methacrylate and double pentaerythritol methacrylate.
3. preparation method according to claim 2, is characterized in that described unsaturated carboxylic acid is methacrylic acid or acrylic acid.
4. according to the preparation method described in any one in claim 1-3, the mass ratio that it is characterized in that described electrophoresis suspensioning liquid and silica is (1～100): 1; The mass ratio of described unsaturated carboxylic acid and silica is (0.3～1): 20; Described other form the material of cyst wall and the mass ratio of described Pickering emulsion is (5～45): 100.
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