CN100476561C - Preparation method of microcapsule for electronic paper display - Google Patents
Preparation method of microcapsule for electronic paper display Download PDFInfo
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- CN100476561C CN100476561C CNB2007100687292A CN200710068729A CN100476561C CN 100476561 C CN100476561 C CN 100476561C CN B2007100687292 A CNB2007100687292 A CN B2007100687292A CN 200710068729 A CN200710068729 A CN 200710068729A CN 100476561 C CN100476561 C CN 100476561C
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Abstract
The invention discloses a method for preparing a micro capsule used in electric paper display, which engages polyelectrolyte salt and alkyl electrolyte, to be aggregated with dope to prepare the micro capsule. The method comprises that using right technique, via the surface activator function of the polyelectrolyte salt and alkyl electrolyte, to disperse the electrophoresis suspension in water phase into oil drops with uniform diameter distribution via the share emulsifying function of polyelectrolyte salt and alkyl electrolyte, adding dope, since the polyelectrolyte salt is anionic polymerization electrolyte, under changeable pH value, the polyelectrolyte salt can be engaged with the alkyl electrolyte to be aggregated with the dope, then via right technique, to prepare the round micro capsule with stable, seal property, and uniform diameter distribution. The invention has the advantages that via the engagement between polyelectrolyte salt and alkyl electrolyte, the invention can overcome the defect of arabin natural macromolecule which is degraded easily to affect the property of micro capsule, reduce cost, make diameter distribution uniform, and make property stable.
Description
Technical field
The present invention relates to a kind of preparation method of microcapsule for electronic paper display.
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.Compare with electronic display technology, tradition possesses superior performance with plain paper: the irradiates light of reflection 80%; Satisfied contrast (about 20: 1) is provided; Disperse reflected light to any direction; Inexpensive, in light weight, approach, be easy to carry, the song that can soften, folding can provide coloured image; Do not need just energy long preservation image of consumes energy, have long-acting Memorability.But it also has shortcoming: can not be as electronic console the instantly changing image, so can not be recycled.Therefore the advantages of plain paper and electronic console get up to research and develop a kind of low cost, high performance display technique is that people dream of always, thereby promoted the emergence and the development of Electronic Paper display technique.
The Electronic Paper display technique is to utilize the principle of electrophoresis to make to be clipped in interelectrode charge species to move under effect of electric field, and the motion of charge species causes two or more different color of Alternation Display.With such electrophoretic cell is a pixel, electrophoretic cell is carried out the two-dimensional matrix formula arrange the formation display plane, and pixel can show different colors as requested, and its combination just can obtain plane picture.Electrophoresis showed is compared very big advantage with existing display technique: the high brightness that high reflectance causes, high-contrast; Full visual angle; Long-term image stabilization, low-power consumption that reflection-type, bistability cause; Thin, light, the song that can soften have portability; Inexpensive, but large-area manufacturing.
The display technique that Paul F.Evans etc. just invented based on principle of electrophoresis as far back as 1969.Thereafter the portable computer display application is paid close attention in the research of many these aspects, because material does not at that time satisfy the requirement of this display technique, do not given play to the advantage of this technology, be defeated by the LCD technology in the competition in this field, the progress that Electronic Paper shows in recent two decades thereafter is little.Last century end, the development of material science (nanometer technology etc.), polymer science, electronics science (plastic crystal Manifold technology, active matrix technology etc.) shows very big impetus to Electronic Paper, the material that makes the preparation Electronic Paper show has important breakthrough, improved the performance that Electronic Paper shows greatly, thereby make people see its great application prospect, impel each company of large group to drop into bigger manpower and materials and go to research and develop this display technique.
People in all sorts of ways Electrophoresis Lab and are separated into tiny microcavity to suppress reunion, the caking of electrophoresis particle, reduce production craft step simultaneously, reduce production costs.Wherein the microcapsule-type Electronic Paper shows it is one of comparatively promising technology.The microcapsule-type Electronic Paper shows it is earlier electrophoresis particle and insulation suspending liquid to be encapsulated in the microcapsules, and microcapsules are placed between electrode.Microcapsules can large-scale production, and the display production technology is simple relatively and can put in order volume and produce automatically.Microcapsules may be combined in the liquid adhesive and coat on the base material with modes such as inkjet printing, brushings, therefore can produce gentle bent display.The microcapsule-type Electronic Paper shows very large research and application prospect.Barrett Comiskey etc. seals electrophoresis system with urea-formaldehyde resin microcapsule.The physical strength of urea resin microcapsule wall material is bigger, but pliability is relatively poor, the therefore bent electrophoresis showed scratch resistance that softens made from this material, pressure poor-performing.The microcapsules that Nakamura etc. have narrated a kind of gelatin-gum arabic system are used for the preparation method of electrophoresis showed, this microcapsules solvent stability is fine, but because gelatin and Arabic gum all are natural prodcuts, stability is relatively poor relatively, and Arabic gum is a kind of imported product concerning China, and large-scale commercial use will be a kind of raw material of costliness; In addition, Arabic gum is easily degraded, and long-term use will influence the performance of microcapsules.Therefore, seek a kind of relative low price, and the polyanionic polymer of stable performance as an alternative product be the interested problem of people always.
The present invention is used for the synthetic of gelatin microcapsules with polyelectrolyte salts, cooperates to have the alkyl electrolyte of Action of Surfactant, to make the electrophoresis liquid oil droplet emulsification under both actings in conjunction that is dispersed in aqueous phase, can make the size distribution of oil droplet more even.Used polyelectrolyte salts is a polyanion electrolyte simultaneously, and can send out with the multiple cohesion of gelatin generation simultaneously with the alkyl electrolyte should.Therefore just can prepare stable, sealing, the uniform circular microcapsules of size distribution by suitable technology.With this polymer manufacture microcapsules, the microcapsules cost that obtains is lower with making, and performance is more superior.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of microcapsule for electronic paper display.
Its preparation process is:
1) with mass ratio be 1～100: 1 polyelectrolyte salts and alkyl electrolyte dissolution in 40-100 ℃ water, obtain aqueous solution;
2) electrophoresis suspensioning liquid is joined in the described aqueous solution of step 1) and disperseed 1～100 minute, electrophoresis suspensioning liquid and polyelectrolyte salts mass ratio are 1～100: 1, obtain O/W type emulsion;
3) gelatin is dissolved in 40-70 ℃ the water, obtaining quality is the aqueous gelatin solution of 1-50% than concentration, joins step 2 then) in the described O/W type emulsion, the mass ratio of gelatin and polyelectrolyte salts is 0.1～20: 1;
4) acid is added in the step 3) product, make it to take place multiple aggregation;
5) reaction product with step 4) cools to 0-15 ℃, adds crosslinking chemical and makes it curing cross-linked;
6) aqueous slkali is joined in the reaction product of step 5), adjusting pH value heats to 40-80 ℃ to 7.5-12, reacts to get final product in 0.5-3 hour.
Advantage of the present invention is to cooperate by polyelectrolyte salts and alkyl are electrolytical, overcome easily degraded and influence the shortcoming of microcapsules performance of Arabic gum, reduced cost.And prepare stable, sealing, the uniform circular microcapsules of size distribution by suitable technology.
Description of drawings
Fig. 1 is to be the optical microscope picture of the microcapsules that contain electrophoresis liquid of feedstock production with carboxyl sodium lignosulfonate, sodium cetanesulfonate, gelatin;
Embodiment
The present invention is described in further detail by following embodiment:
Embodiment 1
1) 10 gram carboxyl sodium lignosulfonates and 0.1 gram sodium cetanesulfonate are dissolved in 80 ℃ of water, obtain aqueous solution;
2) 5 gram silicon dioxide granules, 0.5 gram solvent blue are joined in the 300 gram zellons,, make it to become uniform electrophoresis suspensioning liquid, get this electrophoresis suspensioning liquid 70 grams, join in the above-mentioned aqueous solution, stir and obtained O/W type emulsion in 20 minutes in 40 ℃ of following sonic oscillations;
3) 200 gram gelatin are dissolved in 50 ℃ of water, are made into 50% aqueous solution, add 20% acetum, adjust pH to 6.5 joins the aqueous gelatin solution for preparing in the above-mentioned O/W type emulsion;
4) under 50 ℃, in the step 3) product, add 20% acetum, adjust pH to 4.5;
5) temperature of the reaction product of step 4) is reduced to 10 ℃ in stirring, splash into 2.5 milliliter of 37% formalin, make microcapsule wall crosslinked, continue reaction 1 hour;
6) add 3% sodium hydroxide solution in the reaction product of step 5), adjust pH to 9 continues reaction 1.5 hours down in 45 ℃, obtains containing the microcapsules of electrophoresis liquid.
Embodiment 2
1) 10 gram polyacrylamides and 1 gram cetyl benzene sulfonic acid sodium salt are dissolved in 40 ℃ of water, obtain aqueous solution;
2) 5 gram silicon dioxide granules, 0.5 gram nigrosine are joined in the 200 gram zellons,, make it to become uniform electrophoresis suspensioning liquid, get this electrophoresis suspensioning liquid 10 grams, join in the above-mentioned aqueous solution, stir and obtained O/W type emulsion in 5 minutes in 50 ℃ of following sonic oscillations;
3) 1 gram gelatin is dissolved in 40 ℃ of water, is made into 1% aqueous solution, add 5% sulfuric acid solution, adjust pH to 6.0 joins the aqueous gelatin solution for preparing in the above-mentioned O/W type emulsion;
4) under 40 ℃, in the step 3) product, add 5% sulfuric acid solution, adjust pH to 4.0;
5) temperature of the reaction product of step 4) is reduced to 0 ℃ in stirring, adds 4 milliliter of 15% formalin, make microcapsule wall crosslinked, continue to react 0.5 hour;
6) add 1% sodium hydroxide solution in the reaction product of step 5), adjust pH to 10 continues reaction 3 hours down in 60 ℃, obtains containing the microcapsules of electrophoresis liquid.
Embodiment 3
1) 1 gram sodium alginate and 1 gram α-sodium olefin sulfonate are dissolved in 100 ℃ of water, obtain aqueous solution;
2) 10 gram TiO 2 particles, 0.5 gram solvent blue are joined in the 300 gram zellons, in 70 ℃ of following sonic oscillations, make it to become uniform electrophoresis suspensioning liquid, get this electrophoresis suspensioning liquid 100 grams, join in the above-mentioned aqueous solution, stir and obtained O/W type emulsion in 70 minutes;
3) 10 gram gelatin are dissolved in 70 ℃ of water, are made into 2% aqueous solution, add 0.05% hydrochloric acid solution, adjust pH to 6.2 joins the aqueous gelatin solution for preparing in the above-mentioned O/W type emulsion;
4) under 40 ℃, in the step 3) product, add 0.05% hydrochloric acid solution, adjust pH to 4.8;
5) temperature of the reaction product of step 4) is reduced to 15 ℃ in stirring, adds 6 milliliter of 25% formalin, make microcapsule wall crosslinked, continue to react 3 hours;
6) add 5% ammonia spirit in the reaction product of step 5), adjust pH to 7.5 continues reaction 1 hour down in 80 ℃, obtains containing the microcapsules of electrophoresis liquid.
Embodiment 4
1) 5 gram sodium carboxymethyl celluloses and 0.25 gram lauryl sodium sulfate are dissolved in 60 ℃ of water, obtain aqueous solution;
2) 5 gram silicon dioxide granules, 0.5 gram solvent blue are joined in the 1000 gram zellons, in 50 ℃ of following sonic oscillations, make it to become uniform electrophoresis suspensioning liquid, get this electrophoresis suspensioning liquid 100 grams, join in the above-mentioned aqueous solution, stir and obtained O/W type emulsion in 1 minute;
3) 5 gram gelatin are dissolved in 60 ℃ of water, are made into 20% aqueous solution, add 15% citric acid solution, adjust pH to 5.7 joins the aqueous gelatin solution for preparing in the above-mentioned O/W type emulsion;
4) under 40 ℃, in the step 3) product, add 15% citric acid solution, the pH value is reduced to 4.6;
5) temperature of the reaction product of step 4) is reduced to 5 ℃ in stirring, splash into 7 milliliter of 15% glutaraldehyde water solution, make microcapsule wall crosslinked, continue reaction 1 hour;
6) add 1% ammonia spirit in the reaction product of step 5), adjust pH to 11 continues reaction 0.5 hour down in 40 ℃, obtains containing the microcapsules of electrophoresis liquid.
Embodiment 5
1) 20 gram sodium polyacrylates and 0.4 gram hexadecyl hydrosulfate potassium are dissolved in 70 ℃ of water, obtain aqueous solution;
2) 50 gram TiO 2 particles, 8 gram solvent blues are joined in the 3000 gram zellons, in 50 ℃ of following sonic oscillations, make it to become uniform electrophoresis suspensioning liquid, get this electrophoresis suspensioning liquid 1000 grams, join in the above-mentioned aqueous solution, stir and obtained O/W type emulsion in 100 minutes;
3) 300 gram gelatin are dissolved in 65 ℃ of water, are made into 10% aqueous solution, add 10% tartaric acid solution, adjust pH to 6.4 joins the aqueous gelatin solution for preparing in the above-mentioned O/W type emulsion;
4) under 40 ℃, in the step 3) product, add 10% tartaric acid solution, adjust pH to 4.8;
5) temperature of the reaction product of step 4) is slowly reduced to 3 ℃ in stirring, adds 6 milliliter of 5% glutaraldehyde water solution, make microcapsule wall crosslinked, continue to react 2 hours;
6) add 5% sodium hydrate aqueous solution in the reaction product of step 5), adjust pH to 12 continues reaction 3 hours down in 80 ℃, obtains containing the microcapsules of electrophoresis liquid.
Claims (1)
1. the preparation method of a microcapsule for electronic paper display is characterized in that its preparation process is:
1) with mass ratio be 1～100: 1 polyelectrolyte salts and alkyl electrolyte dissolution in 40-100 ℃ water, obtain aqueous solution;
2) electrophoresis suspensioning liquid is joined in the described aqueous solution of step 1) and disperseed 1～100 minute, electrophoresis suspensioning liquid and polyelectrolyte salts mass ratio are 1～100: 1, obtain O/W type emulsion;
3) gelatin is dissolved in 40-70 ℃ the water, obtaining quality is the aqueous gelatin solution of 1-50% than concentration, joins step 2 then) in the described O/W type emulsion, the mass ratio of gelatin and polyelectrolyte salts is 0.1～20: 1;
4) acid is added in the step 3) product, make it to take place multiple aggregation;
5) reaction product with step 4) cools to 0-15 ℃, adds crosslinking chemical and makes it curing cross-linked;
6) aqueous slkali is joined in the reaction product of step 5), adjusting pH value heats to 40-80 ℃ to 7.5-12, reacts to get final product in 0.5-3 hour;
Described polyelectrolyte salts is sodium alginate, sodium carboxymethyl cellulose, polyacrylamide, carboxyl sodium lignosulfonate or sodium polyacrylate, the alkyl electrolyte is straight-chain alkyl sulfate, linear alkylbenzene sulfonate, α-Xi Jihuangsuanyan or linear alkyl benzene sulphonic acid, acid is hydrochloric acid, sulfuric acid, acetic acid, citric acid or tartrate, the concentration of acid is 0.05～20%, and crosslinking chemical is formaldehyde or glutaraldehyde.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103212350A (en) * | 2012-01-18 | 2013-07-24 | 广州奥熠电子科技有限公司 | Mono-disperse electrophoretic display microcapsule preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649038B (en) * | 2011-07-26 | 2014-06-25 | 京东方科技集团股份有限公司 | Preparation method of inorganic-organic composite electronic iron microcapsules |
| CN102698668B (en) * | 2011-11-08 | 2014-11-12 | 京东方科技集团股份有限公司 | Electronic ink microcapsule and preparation method thereof |
| CN108252151B (en) * | 2017-12-30 | 2020-05-29 | 武汉晨鸣汉阳纸业股份有限公司 | Preparation method of paper stiffness agent |
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Non-Patent Citations (4)
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| 电子墨水微胶囊及电泳显示原型器件的制备. 荣宇等.高等学校化学学报，第26卷第5期. 2005 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103212350A (en) * | 2012-01-18 | 2013-07-24 | 广州奥熠电子科技有限公司 | Mono-disperse electrophoretic display microcapsule preparation method |
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