CN1298421C - Method for preparing blue electronic ink microcapsule in color lake class - Google Patents
Method for preparing blue electronic ink microcapsule in color lake class Download PDFInfo
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- CN1298421C CN1298421C CNB2003101189690A CN200310118969A CN1298421C CN 1298421 C CN1298421 C CN 1298421C CN B2003101189690 A CNB2003101189690 A CN B2003101189690A CN 200310118969 A CN200310118969 A CN 200310118969A CN 1298421 C CN1298421 C CN 1298421C
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Abstract
The present invention relates to a method for preparing a blue electronic ink microcapsule in the color lake class. Electronic ink is composed of the microcapsules which contain electrophoresis display liquid and are arrayed on a plane or a curved surface, wherein the liquid and the grains in the capsules can move under the function of an electric field so as to display different optical properties, and points having different optical properties can be used as picture elements to realize the display. The microcapsule of electronic ink is composed of electrophoresis grains, an electrophoresis base solution and a capsule wall, wherein the electrophoresis grains in the present invention are blue pigment in the color lake class; and the electrophoresis base solution is tetrachloroethylene which has the characteristics of low dielectric constant, low viscosity and high boiling point. Chemical and physical methods are utilized for coating octadecanamine on the grains so as to carry out surface modification to the pigment, and the pigment can have electric charge of a certain property; surface active agents of SPAN 80, etc. are added to the electrophoresis base solution in order to improve the dispersion stability of the pigment grains; an in-situ polymerization method in water phase is used; and a urea formaldehyde pre-polymer is used as a monomer to carry out micro-encapsulation to the electrophoresis display liquid. The method for preparing a blue electronic ink microcapsule in the color lake class makes the microcapsule of electronic ink have favorable reversible move characteristics under the action of the electric field, and completely overcomes the problem of the adsorption of the pigment grains on the inner wall of the microcapsule.
Description
Technical field the present invention relates to the blue preparing electronic ink microcapsule of color lake class, being particularly related to color lake class blue pigment is electrophoretic particles, low-k, low viscosity, high boiling organic solvent tetrachloro-ethylene are the electrophoresis base fluid, and Lauxite is the preparation of the blue electron ink microcapsule of capsule wall material.
The background technology electric ink is that the electrophoresis disclosing solution that will include particulate and electrophoresis base fluid is wrapped in the microcapsules, because the special stability of minute yardstick suspension system, when micro-capsule is applied electric field, in micro-capsule, realize electrophoresis showed, and can get back to original poised state after discharging electric field.Utilize the demonstration equipment of this fabrication techniques have contrast greatly, with great visual angle, high display brightness, low price, easily realize big plane, fine definition, low power consumption, can not power consumption keep that image, thickness are minimum, electromagnetic-radiation-free, can realize advantage such as flexible demonstration.Make at present color electric ink micro capsule unified method not as yet, we use the aqueous phase situ aggregation method that electrophoresis liquid is realized microencapsulation, the special blueness shallow lake serial pigment of selecting modification is for showing particle, can realize advantages such as quick reverse response to electric field but have technology blue electron ink microcapsule simple, with low cost, preparation.
Summary of the invention the purpose of this invention is to provide the blue preparing electronic ink microcapsule of a kind of color lake class, and its electrophoretic particles is a color lake class blue pigment; The electrophoresis base fluid is low-k, low viscosity, high boiling tetrachloro-ethylene; Utilize the Chemical Physics method on granules of pigments, to coat octadecylamine particle is carried out surface modification, make it have the electric charge of certain character; Utilize and add surfactant SPAN80 to improve the dispersion stabilization of granules of pigments; With the situ aggregation method of aqueous phase, be that monomer carries out microencapsulation to electrophoresis disclosing solution with the ureaformaldehyde performed polymer.
The objective of the invention is to be achieved through the following technical solutions, comprising:
The blue preparing electronic ink microcapsule of a kind of color lake class, this method utilizes tetrachloro-ethylene to be the electrophoresis base fluid, the blueness shallow lake class granules of pigments of surface modification is an electrophoretic particles, electrophoretic particles is dispersed in the capsule heart of forming microcapsules in the tetrachloro-ethylene, prepares the microcapsules that Lauxite is the wall material by situ aggregation method again.
According to a kind of method for optimizing of the present invention, comprise the following steps:
By urea and 1: 1.6~1: 2 amount of getting of formaldehyde mole ratio, earlier formaldehyde is regulated pH value 8~9 with triethanolamine or NaOH, add the urea stirring again and make its dissolving, reacted 1~1.5 hour down at 70~80 ℃, for the volatilization of avoiding formalin should add the backflow device, reaction finishes, and cools off the stoste of the performed polymer that obtains urea formaldehyde resin fast with cold water.
Ratio according to volume ratio 1: 2~10 is mixed performed polymer stoste with water, add acid such as hydrochloric acid or acetic acid or citric acid, regulating the pH value is 2~4, in the capsule heart: performed polymer (stoste) is that 1: 1~1: 10 ratio joins it in performed polymer aqueous solution, mixing speed per minute 400~800 changes, reacted under the room temperature 1~2 hour, form the blank of microcapsules, slowly be warmed up to 60~90 ℃ and continue reaction 0.5~2 hour, the wall thickness of microcapsules is increased, and cooling naturally separates with the method for filtration or natural subsidence, washing, drying makes blue shallow lake electron ink microcapsule.
Method of the present invention is further characterized in that blue shallow lake class granules of pigments adopts chemiadsorption to carry out surface modification treatment, modifier option table surface-active agent octadecylamine, and consumption is 5~20% of a granules of pigments quality, surface modification may further comprise the steps:
Thermal air current or infrared lamp oven dry are selected in the oven dry of blue shallow lake pigment for use, and bake out temperature is 80~120 ℃; Adopt ball mill that blue particle is ground to less than 1 μ m; Octadecylamine is dissolved in 50~500 times of ethanol that are equivalent to the granules of pigments quality, again granules of pigments is dispersed in wherein, conventional method is taked in scatter operation, as stirring, ultrasonic, being lower than under 85 ℃ the temperature stirring and refluxing 1 to 2 hour, remove ethanol and obtain the modification blue shallow lake pigment of particle diameter less than 1 μ m.
According to method of the present invention, its another feature is the blue shallow lake of modification granules of pigments to be dispersed in it by ultra-sonic dispersion method make the microcapsules capsule heart in the tetrachloro-ethylene, add oil-soluble dispersion stabilizer SPAN80 during dispersion to improve its dispersibility, the addition of SPAN80 is the 1-5% of blue shallow lake class granules of pigments, and the weight ratio of blue shallow lake granules of pigments and tetrachloro-ethylene is 1: 10~1: 100.
The wall material of the blue electron ink microcapsule of the color lake class described in the present invention selects to have good light transmittance, certain mechanical strength, certain elastic modelling quantity and be insoluble to the organic high molecular compound Lauxite of electrophoresis base fluid.
The technology of preparing of microcapsules has been public technology, can select suitable method to carry out the preparation of capsule according to the different capsule hearts and wall material.Wall material among the present invention is a Lauxite, selects the situ aggregation method of aqueous phase.
The capsule heart among the present invention is that electrophoresis liquid is the blueness shallow lake granules of pigments composition of low-k, low viscosity, high boiling organic solvent and surface modification.Specifiable organic solvent can be alkanes such as nonane, certain herbaceous plants with big flowers alkane, toluene, dimethylbenzene, halogenated hydrocarbon such as tetrachloro-ethylene, tetrafluoroethene, ethers such as hexyl ether, isoamyl ether, butyl ether, ketone such as phorone, isophorone, ester class such as butyl formate, can be one or more combination, the tetrachloro-ethylene of preferred one pack system.Electrophoretic particles is a blue shallow lake class pigment, can select royal blue shallow lake, the blue shallow lake of sun-proof cyanines, peacock blue lake, preferred reddish blue color lake.Because granules of pigments is dispersive property and the charging property the subject of knowledge and the object of knowledge of limit itself in the organic solvent tetrachloro-ethylene, must carry out surface modification treatment to it.The present invention adopts chemiadsorption that the color lake granules of pigments is carried out the surface and coats octadecylamine.
Class blue preparing electronic ink microcapsule in color lake of the present invention makes electron ink microcapsule have good reversible moving characteristic under electric field action, and has overcome the absorption of granules of pigments on the microcapsules inwall fully.
The specific embodiment
1. blue shallow lake granules of pigments surface modification treatment: after a certain amount of mordant pigment particle drying, the grinding, it is some to add polarity low boiling point organic solvent absolute ethyl alcohol, after the supersonic oscillations 20 minutes, add the octadecylamine modifier that is equivalent to pigment mass 5~10%, in 80 ℃ water-bath, added hot reflux 1 hour, absolute ethyl alcohol is removed in decompression distillation, with particle powder taking-up, the drying that obtains.
2. the preparation of electrophoresis liquid: the base fluid of electrophoresis liquid is aforesaid organic solvent, to join through the blueness shallow lake of surface modification treatment granules of pigments and prepare electrophoresis disclosing solution in the base fluid, in order to make particle good dispersion in oil phase, can add oil soluble surfactant SPAN80 and help its dispersion.
3. the preparation of blue electron ink microcapsule: blue preparing electronic ink microcapsule is the same with the capsule preparation of knowing, and has many methods to select, chemical method such as interfacial polymerization, situ aggregation method; Physical-chemical process such as complex coacervation, single coacervation, oil-phase separating method, dry bath method, fusing disperse condensation method, powder art bed method etc.; Physics method such as pot wrap method, air suspension film forming method, spray-on process, inclusion complexometry etc.The present invention preferably is the situ aggregation method of the aqueous phase of wall material with the urea formaldehyde resin.
Its preparation process is: by urea and formaldehyde mole ratio is 1: 6~1: 2 amount of getting, earlier formaldehyde is regulated pH value 8~9 with triethanolamine or sodium hydroxide solution, again urea is dissolved in wherein, 70~80 ℃ are reacted 1~1.5 hour (adding backflow) down, cool off the performed polymer that obtains urea formaldehyde resin fast with cold water.According to volume ratio 1: 2~10 performed polymer and water are mixed, adding acid for adjusting pH value is 2~4.The oil-soluble electrophoresis disclosing solution is added in the aqueous solution, mixing speed per minute 400~800 changes, reacted under the room temperature 1~2 hour, slowly be warmed up to 60~90 ℃ and continue reaction 0.5~2 hour, naturally cooling, method separation, washing, drying with filtration, washing or natural subsidence make blue electron ink microcapsule.
Embodiment one: the formalin of 10mL37~40%, hydro-oxidation sodium are regulated pH=9.0, add 5g urea and stir and make it dissolving, 75 ℃ of reactions one hour down, cold water cool off performed polymer.Add 30mL water in this performed polymer, stir.
0.5g reddish blue color lake in the ultrasonic absolute ethyl alcohol that is scattered in 20mL, adds the 50mg octadecylamine again behind mill-drying, be warmed up to 80 ℃ under the backflow stirring condition, keeps 1 hour.Absolute ethyl alcohol is removed in decompression, granularity coats reddish blue color lake granules of pigments less than 1 micron octadecylamine.
Aforementioned blue pigment particle 50mg and the 5mgSPAN80 that has wrapped up octadecylamine added in the 2ml tetrachloro-ethylene, pour in the aforementioned performed polymer aqueous solution after the dispersion down ultrasonic, regulating pH with citric acid-sodium hydroxide buffer solution is 3, and at room temperature vigorous stirring is warmed up to 60 ℃ of maintenances 1 hour gradually after 60 minutes.Make the capsule that diameter is 20~30 μ m.
Embodiment two: the 0.5g Fast Malachite Blue lake in the ultrasonic acetone that is scattered in 20mL, adds the 50mg octadecylamine again behind mill-drying, be warmed up to 50 ℃ under the backflow stirring condition, keeps 1 hour.Acetone is removed in decompression, granularity coats the Fast Malachite Blue lake granules of pigments less than 1 micron octadecylamine.
Encapsulation process is with embodiment one.
Claims (3)
1. blue preparing electronic ink microcapsule of color lake class, its principal character is that this method utilizes tetrachloro-ethylene to be the electrophoresis base fluid, the blueness shallow lake class granules of pigments of surface modification is an electrophoretic particles, electrophoretic particles is dispersed in the capsule heart of forming microcapsules in the tetrachloro-ethylene, prepare the microcapsules that Lauxite is the wall material by situ aggregation method again, this method comprises the following steps:
(1) be 1: 1.6~1: 2 amount of getting by urea and formaldehyde mole ratio, earlier formaldehyde is regulated pH value 8~9 with triethanolamine or NaOH, again urea is dissolved in wherein, reacts 1~1.5 hour (adding backflow) down, cool off the performed polymer that obtains urea formaldehyde resin fast with cold water at 70~80 ℃;
(2) according to the ratio of volume ratio 1: 2~10 performed polymer is mixed with water, adding acid for adjusting pH value is 2~4, in the capsule heart: performed polymer (stoste) is that 1: 1~1: 10 ratio joins it in performed polymer aqueous solution, mixing speed per minute 400~800 changes, reacted under the room temperature 1~2 hour, and slowly be warmed up to 60~90 ℃ and continue reaction 0.5~2 hour, naturally cooling, method with filtration or natural subsidence is separated, washing, drying.
2. according to the blue preparing electronic ink microcapsule of the described color lake of claim 1 class, it is characterized in that blue shallow lake class granules of pigments adopts chemiadsorption to carry out surface modification treatment, modifier is the surfactant octadecylamine, and consumption is 5~20% of a granules of pigments quality, may further comprise the steps:
(1) thermal air current or infrared lamp oven dry are selected in the oven dry of blue shallow lake pigment for use, and bake out temperature is 80~120 ℃;
(2) adopt ball mill that blue particle is ground to less than 1 μ m;
(3) octadecylamine is dissolved in 50~500 times of ethanol that are equivalent to the granules of pigments quality, again granules of pigments is dispersed in wherein, under heat up (temperature is lower than 85 ℃) stirs, refluxed 1 to 2 hour, remove ethanol, obtain particle diameter and form sediment less than the modification of 1 μ m is blue.
3. according to the blue preparing electronic ink microcapsule of the described color lake of claim 1 class, it is characterized in that ultrasonic being dispersed in of the blue shallow lake granules of pigments of modification made the microcapsules capsule heart in the electrophoresis base fluid tetrachloro-ethylene, add oil-soluble dispersion stabilizer SPAN80 to improve its dispersibility, the consumption of SPAN80 is 1~5% of the blue shallow lake of a modification granules of pigments, and the weight ratio of blue shallow lake granules of pigments and electrophoresis base fluid is 1: 10~1: 100.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US5961804A (en) * | 1997-03-18 | 1999-10-05 | Massachusetts Institute Of Technology | Microencapsulated electrophoretic display |
US6067185A (en) * | 1997-08-28 | 2000-05-23 | E Ink Corporation | Process for creating an encapsulated electrophoretic display |
US6249271B1 (en) * | 1995-07-20 | 2001-06-19 | E Ink Corporation | Retroreflective electrophoretic displays and materials for making the same |
US6262833B1 (en) * | 1998-10-07 | 2001-07-17 | E Ink Corporation | Capsules for electrophoretic displays and methods for making the same |
US6262706B1 (en) * | 1995-07-20 | 2001-07-17 | E Ink Corporation | Retroreflective electrophoretic displays and materials for making the same |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6249271B1 (en) * | 1995-07-20 | 2001-06-19 | E Ink Corporation | Retroreflective electrophoretic displays and materials for making the same |
US6262706B1 (en) * | 1995-07-20 | 2001-07-17 | E Ink Corporation | Retroreflective electrophoretic displays and materials for making the same |
US5961804A (en) * | 1997-03-18 | 1999-10-05 | Massachusetts Institute Of Technology | Microencapsulated electrophoretic display |
US6067185A (en) * | 1997-08-28 | 2000-05-23 | E Ink Corporation | Process for creating an encapsulated electrophoretic display |
US6262833B1 (en) * | 1998-10-07 | 2001-07-17 | E Ink Corporation | Capsules for electrophoretic displays and methods for making the same |
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