CN1768921A - Method for preparing quasi-uniform electronic ink micro capsule - Google Patents
Method for preparing quasi-uniform electronic ink micro capsule Download PDFInfo
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- CN1768921A CN1768921A CN 200410073226 CN200410073226A CN1768921A CN 1768921 A CN1768921 A CN 1768921A CN 200410073226 CN200410073226 CN 200410073226 CN 200410073226 A CN200410073226 A CN 200410073226A CN 1768921 A CN1768921 A CN 1768921A
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Abstract
The invention relates to a method for preparing quasi-uniform electronic ink micro-capsule. Wherein, the electronic ink is the electrophoretic display material of micro-capsule, which contains the paint particles and dyestuff solution into micro-capsule to use the electrophoretic display theory to realize the electrophoretic display in the micro-capsule, and it can be used in flat or flexible display. The invention uses dodecyl sodium sulfate (SDS) of negative ion surface activator as diffusion agent, the scarlet powder as paint particles, the ankilostin as organic solvent, and the solvent black as solvent dyestuff. First preparing quasi-uniform diffused electrophoretic base drop; then by adjusting the pH value, processing the composite aggregation reaction between gelatine and acacia gum to attain the quasi-uniform electronic ink micro-capsule. And via changing the concentration of SDS and the mixing speed, the quasi-uniform electronic ink micro-capsule whose diameter is controlled in 30-90mu m can be attained. The invention has simple method, and controllable reaction without special demand for devices.
Description
Technical field the present invention relates to a kind of preparation method of quasi-uniform electronic ink micro capsule, particularly is used for the preparation method of the quasi-uniform electronic ink micro capsule of flexibility or FPD.
It is the microencapsulation electrophoretic display technology that the background technology electric ink shows, it is meant pigment particle and dye solution is wrapped in the microcapsules, utilize the electrophoresis showed principle, in micro-capsule, realize electrophoresis showed, thereby suppressed the electrophoresis micelle greater than shortcomings such as the reunion in the capsule range scale, depositions, improve its stability, increase the service life.Electric ink is a kind of suspension of ink shape, under External Electrical Field, can realize reversible, bistable state, the flexible demonstration, be a kind of flexible display material and technology, have good visuality, low-power consumption, information and be written into strong, easy to carry, the advantages such as manufacturing process is cheap, electromagnetic-radiation-free of ability.
The core part that electron ink microcapsule shows as electric ink, its performance will directly have influence on the quality of display performance.For example the particle size of the concentration of the content of the middle solid particle of microcapsules, dyestuff, microcapsules and extra electric field intensity etc. all directly affect electronics contrast of display degree.At present, adopt the particle diameter of the urea formaldehyde resin base electron ink microcapsule of situ aggregation method preparation to distribute generally at 30～300 mu m ranges; What adopt the complex coacervation acquisition is the microcapsules of wall material with the gelatin-Arabic gum, its particle size distribution range also tens between the hundreds of micron, and be controlled by the factors such as addition of speed, mixing speed size and the water of monomer solution mixing, condition is wayward.
Summary of the invention the object of the invention provides a kind of preparation method of quasi-uniform electronic ink micro capsule, wherein adopts anionic (SDS) to be dispersant, and at first prepares accurate homodisperse electrophoresis base fluid drop; By regulating the pH value, make gelatin and Arabic gum generation complex coacervation prepared in reaction quasi-uniform electronic ink micro capsule again.Preparation is simple for this method, and course of reaction is easy to control, and equipment is not had specific (special) requirements.
Description of drawings
Under Figure 180 0rpm mixing speed, the optical photograph of prepared electron ink microcapsule when system contains the 0.01wt% lauryl sodium sulfate
Under Figure 28 00rpm mixing speed, the size distribution of prepared electron ink microcapsule when system contains the 0.01wt% lauryl sodium sulfate
Under Figure 38 00rpm mixing speed, the relation in the average grain diameter of electrophoresis base fluid drop and the system between the concentration of contained lauryl sodium sulfate
When containing the 0.015wt% lauryl sodium sulfate in Fig. 4 system, the relation between the logarithm of electrophoresis base fluid drop average grain diameter and the logarithm of mixing speed
Specific embodiment the present invention is that granules of pigments, nigrosine are that the quasi-uniform electronic ink micro capsule of organic solvent dyestuff is an example with the red, and the preparation method who obtains quasi-uniform electronic ink micro capsule is described.With the above grade raw material of chemical pure: red is the red pigment particle, and tetrachloro-ethylene is an organic solvent, and nigrosine is solvent dye; Gelatin and Arabic gum are raw material, and acetic acid and NaOH are the pH conditioning agent, and formalin (mass percent is 37%) is a curing agent, and sodium carboxymethylcellulose is a colloid protective agent.
At first, with Span80 dispersant with a certain amount of modification red granules of pigments, ultrasonic being scattered in the tetrachloro-ethylene solution that is dissolved with nigrosine forms the capsule heart.
With gelatin and Arabic gum with etc. quality be dissolved in respectively in 40～70 ℃ the water.After the mixing, add the SDS of accurate weighing; After treating the SDS dissolving, add the capsule heart, and turn on agitator, make mixing speed slowly rise to a certain fixed value, stirred for several ten minutes can obtain accurate homodisperse electrophoresis base fluid drop; Then, regulate the pH value to the isoelectric point of gelatin, make gelatin and Arabic gum generation aggregation with dilute acetic acid aqueous solution; Behind the stoichiometric number ten minutes, system is cooled to below 10 ℃, adds several milliliters of formalins and be cured reaction; Then, add a certain amount of sodium carboxymethylcellulose, stir and make its dissolving, greater than 9, be heated to 50～70 ℃ with dilute sodium hydroxide regulation system pH, stoichiometric number is ten minutes again; At last, cooling naturally, washing can obtain quasi-uniform electronic ink micro capsule in certain range scale.
Concrete enforcement of the present invention is described in detail by following examples:
Embodiment 1:
Nigrosine is dissolved in the tetrachloro-ethylene, crosses filtering and get residue; Taking by weighing the red of 30mg through surface modification, is dispersant with 45mgSpan80, in the tetrachloro-ethylene that contains nigrosine of the ultrasonic 6mL of being scattered in.
0.75g gelatin and 0.75g Arabic gum are dissolved in respectively in the 100mL distilled water, keep 40～45 ℃, stir down two kinds of solution are mixed; A certain amount of SDS of weighing simultaneously accurately makes that SDS concentration is 0.01wt% in the solution; Add the 2mL capsule-core, slowly open and stir, make mixing speed reach 800rpm (time that 15s is above) gradually, keep 40～45 ℃ to stir 30min down, promptly obtain accurate homodisperse electrophoresis base fluid drop; Acetum with 5wt% slow (time that 5min is above) is regulated the pH=3.7 that makes solution, make gelatin and Arabic gum that multiple cohesion take place, after condensed phase forms, after making mixture system leave water-bath to naturally cool to room temperature, with ice-water bath system is cooled to below 10 ℃ again, keep 40min, add 5～10mL formalin and solidify 60min; Then, add the 10g sodium carboxymethylcellulose, stir and make its dissolving, greater than 9, be heated to 50～70 ℃, reaction 60min with dilute sodium hydroxide regulation system pH; At last, cooling naturally, washing promptly obtains the quasi-uniform electronic ink micro capsule emulsion (as Fig. 1,2) that average grain diameter is about 40 μ m.
Embodiment 2:
Nigrosine is dissolved in the tetrachloro-ethylene, crosses filtering and get residue; Taking by weighing the red of 30mg through surface modification, is dispersant with 45mgSpan80, in the tetrachloro-ethylene that contains nigrosine of the ultrasonic 6mL of being scattered in.
0.75g gelatin and 0.75g Arabic gum are dissolved in respectively in the 100mL distilled water, keep 40～45 ℃, stir down two kinds of solution are mixed; A certain amount of SDS of weighing simultaneously accurately makes that SDS concentration is 0.005wt% in the solution; Add the 2mL capsule-core, slowly open and stir, make mixing speed reach 800rpm (time that 15s is above) gradually, keep 40～45 ℃ to stir 30min down, promptly obtain accurate homodisperse electrophoresis base fluid drop; Acetum with 5wt% slow (time that 5min is above) is regulated the pH=3.7 that makes solution, make gelatin and Arabic gum that multiple cohesion take place, after condensed phase forms, after making mixture system leave water-bath to naturally cool to room temperature, with ice-water bath system is cooled to below 10 ℃ again, keep 40min, add 5～10mL formalin and solidify 60min; Then, add the 10g sodium carboxymethylcellulose, stir and make its dissolving, greater than 9, be heated to 50～70 ℃, reaction 60min with dilute sodium hydroxide regulation system pH; At last, cooling naturally, washing promptly obtains the quasi-uniform electronic ink micro capsule emulsion that average grain diameter is about 60 μ m.
Embodiment 3:
Nigrosine is dissolved in the tetrachloro-ethylene, crosses filtering and get residue; Taking by weighing the red of 30mg through surface modification, is dispersant with 45mgSpan80, in the tetrachloro-ethylene that contains nigrosine of the ultrasonic 6mL of being scattered in.
0.75g gelatin and 0.75g Arabic gum are dissolved in respectively in the 100mL distilled water, keep 40～45 ℃, stir down two kinds of solution are mixed; A certain amount of SDS of weighing simultaneously accurately makes that SDS concentration is 0.015wt% in the solution; Add the 2mL capsule-core, slowly open and stir, make mixing speed reach 900rpm (time that 15s is above) gradually, keep 40～45 ℃ to stir 30min down, promptly obtain accurate homodisperse electrophoresis base fluid drop; Acetum with 5wt% slow (time that 5min is above) is regulated the pH=3.7 that makes solution, make gelatin and Arabic gum that multiple cohesion take place, after condensed phase forms, after making mixture system leave water-bath to naturally cool to room temperature, with ice-water bath system is cooled to below 10 ℃ again, keep 40min, add 5～10mL formalin and solidify 60min; Then, add the 10g sodium carboxymethylcellulose, stir and make its dissolving, greater than 9, be heated to 50～70 ℃, reaction 60min with dilute sodium hydroxide regulation system pH; At last, cooling naturally, washing promptly obtains the quasi-uniform electronic ink micro capsule emulsion that average grain diameter is about 45 μ m.
Claims (4)
1. the preparation method of a quasi-uniform electronic ink micro capsule, this method adopt gelatin and Arabic gum complex coacervation to prepare quasi-uniform electronic ink micro capsule; Its principal character is: with anionic (SDS) is dispersant, obtains particle diameter at the controlled quasi-uniform electronic ink micro capsule of 30～90 mu m ranges by the control mixing speed.
2. a kind of preparation method of quasi-uniform electronic ink micro capsule according to claim 1, it is characterized in that: dispersant SDS optimum concentration range is 0.003～0.018g/L;
3. a kind of preparation method of quasi-uniform electronic ink micro capsule according to claim 1, it is characterized in that: slowly turn on agitator (time is controlled at more than the 15s), and control mixing speed is between 500～1200rpm;
4. a kind of preparation method of quasi-uniform electronic ink micro capsule according to claim 1 is characterized in that preparation technology may further comprise the steps:
(1) selecting red, nigrosine, tetrachloro-ethylene, gelatin, Arabic gum, distilled water for use is raw material; NaOH, acetic acid are the pH conditioning agent; SDS is a dispersant, and Span-80 is a surfactant;
(2) press red: nigrosine: tetrachloro-ethylene: SDS: water: gelatin: Arabic gum=1～20: 0.01～0.1: 0.005～0.015: 100: 7500～12500: 30～50: 30～50 (mass ratioes) batching;
(3) a certain amount of nigrosine is dissolved in the tetrachloro-ethylene, removes by filter residue; Be dispersed in the tetrachloro-ethylene solution that contains an amount of Span-80 surface treated red is ultrasonic, obtain capsule-core;
(4) with gelatin and Arabic gum with etc. quality be dissolved in respectively in 40～70 ℃ of hot water of water.After the mixing, add SDS by proportioning; After treating the SDS dissolving, add capsule-core, and turn on agitator, mixing speed is slowly risen (time is controlled at more than the 15s), under suitable mixing speed, disperse 20～40min, can obtain having accurate homodisperse electrophoresis base fluid drop;
(5) slowly regulate pH value (time is controlled at more than the 5min) to the gelatin isoelectric point with rare acetum, make gelatin and Arabic gum generation aggregation, carry out 40～60min;
(6) system is cooled to below 10 ℃, adds an amount of formalin, curing reaction 60～80min; Add an amount of sodium carboxymethylcellulose again, stirring and dissolving, and, be heated to 50～70 ℃ of reaction 50～80min with more than the diluted sodium hydroxide solution regulation system pH value to 9; To obtain microcapsule emulsion and stir nature cooling down, washing promptly obtains at the controlled quasi-uniform electronic ink micro capsule of 30～90 mu m ranges.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969874A (en) * | 2014-04-28 | 2014-08-06 | 京东方科技集团股份有限公司 | Liquid crystal display panel, manufacturing method, semitransparent and semi-reflecting display device and display control method |
| CN109621855A (en) * | 2019-01-02 | 2019-04-16 | 北京尚唐印刷包装有限公司 | Fragrant microcapsule and its preparation method and application |
| CN113741113A (en) * | 2021-09-23 | 2021-12-03 | 广东志慧芯屏科技有限公司 | Pressure-bearing electronic paper film and manufacturing process thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6517618B2 (en) * | 2001-05-24 | 2003-02-11 | Xerox Corporation | Photochromic electrophoretic ink display |
| CN1216948C (en) * | 2002-10-21 | 2005-08-31 | 西北工业大学 | Red electronic ink display material and its preparing technology |
| CN1228401C (en) * | 2002-12-09 | 2005-11-23 | 西北工业大学 | Prepn of green electronic ink |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969874A (en) * | 2014-04-28 | 2014-08-06 | 京东方科技集团股份有限公司 | Liquid crystal display panel, manufacturing method, semitransparent and semi-reflecting display device and display control method |
| US9740045B2 (en) | 2014-04-28 | 2017-08-22 | Boe Technology Group Co., Ltd. | Liquid crystal panel, method of manufacturing liquid crystal panel, transflective display device, and a method of controlling displaying of transflective display device |
| CN109621855A (en) * | 2019-01-02 | 2019-04-16 | 北京尚唐印刷包装有限公司 | Fragrant microcapsule and its preparation method and application |
| CN109621855B (en) * | 2019-01-02 | 2021-11-30 | 北京尚唐印刷包装有限公司 | Fragrant microcapsule and preparation method and application thereof |
| CN113741113A (en) * | 2021-09-23 | 2021-12-03 | 广东志慧芯屏科技有限公司 | Pressure-bearing electronic paper film and manufacturing process thereof |
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