CN102441354A - Preparation method for monochrome electrophoresis display microcapsules - Google Patents
Preparation method for monochrome electrophoresis display microcapsules Download PDFInfo
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- CN102441354A CN102441354A CN2011103298748A CN201110329874A CN102441354A CN 102441354 A CN102441354 A CN 102441354A CN 2011103298748 A CN2011103298748 A CN 2011103298748A CN 201110329874 A CN201110329874 A CN 201110329874A CN 102441354 A CN102441354 A CN 102441354A
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Abstract
The invention relates to a preparation method for a monochrome electrophoresis display microcapsules. The method comprises the following steps: 1) using gelatin and Arabic gum in a mass ratio of 1: 1 to 2: 1 as a wall material, preparing an aqueous solution by using deionized water at a temperature of 45 DEG C, adding a composite surfactant with HLB equal to 8 to 13 into the aqueous solution, and adjusting the pH value of the solution to be 6 to 7 with alkali; 2) adding electrophoresis liquid into the aqueous solution obtained in step 1) so as to obtain O/W type emulsion, adjusting the pH value of a system to be 4 to 5 with dilute acetic acid, and allowing gelatin-Arabic gum to undergo complex coacervation so as to form microcapsule walls; 3) cooling an obtained product to a temperature below 10 DEG C, adding the curing agent 5 wt % of glutaraldehyde for cross-linking and curing of the microcapsule walls for 1 h, adjusting the pH value of the system to be 9 to 11 with aqueous alkali, heating the system to a temperature of 45 to 60 DEG C, separating obtained microcapsules, and adding the microcapsules into a polyphenol solution for a further reaction at a temperature of 20 to 30 DEG C for 10 h. The microcapsules prepared by using the method provided in the invention have dispersive individuals, a uniform particle size and high yield; the microcapsule walls have high strength and good toughness, do not rupture at a high temperature, are not damaged even after severe deformation and enable a display device to obtain display images.
Description
Technical field
The present invention relates to a kind of preparation method of black and white electrophoretic display microcapsule, the particularly flexible electron ink microcapsule preparation field that shows.
Background technology
The microcapsules electrophoresis showed is to utilize the suspension of microcapsules wrap charged, and under electric field action, the charged particle in the microcapsules directed swimming takes place and realizes technique for displaying.The preparation of microcapsules then is one of key content of microcapsules electrophoretic display technology, and the single dispersion of microcapsules, particle diameter are even, and cyst wall intensity is high, and good toughness can make its preparation process at display device do not damaged, and is the basic demand that realizes electrophoresis showed.
The method of reporting in the document for preparing microcapsules is a lot, and mainly containing Lauxite is that situ aggregation method and gelatin-gum arabic are complex coacervation.With Lauxite is that capsule is compared, and the capsule of complex coacervation preparation has good sphericity, and closure is strong, and characteristics such as smoothness and transparency height, possess hydrophilic property and permeability are used more extensive.But reunion adhesion easily between the gelatin-gum arabic microcapsules, the difficult product that obtains single dispersion, and also the cyst wall mechanical strength is not enough, breaks easily, and like Fig. 4 a, this has had a strong impact on the display performance of device.
Summary of the invention
The present invention provides a kind of high strength electrophoresis to show that advantage is through controlling the HLB value and the concentration of composite dispersant, having improved the productive rate of microcapsules, like Fig. 1 with gelatin-gum arabic system microcapsule preparation method.Condition of cure and order in the technology; Microcapsules are not broken at 30 ℃ of oven dry 20～30min, dry the dehydration of 20～30min microcapsules down for 50 ℃ and deform, but do not break yet; Like Fig. 4 b, c, and can bear coating process and overstock the intact individual layer microcapsules demonstration film of formation such as Fig. 5 a.
Technical scheme of the present invention is following:
A kind of preparation method of black and white electrophoretic display microcapsule the steps include:
1) be that 1: 1～2: 1 gelatin and Arabic gum is as the wall material with mass ratio; The use temperature is the aqueous solution that 45 ℃ deionized water is made into 1wt%～4wt%; The compound surfactant of HLB=8～13 is added in the solution, and making its concentration is 0.0005～0.003gmL
-1, and with alkali regulator solution pH=6～7;
2) electrophoresis liquid is added in the aqueous solution of step 1), disperses 20～30min, the mass ratio of electrophoresis liquid and wall material is 2: 1～10: 1, obtains O/W type emulsion; With spirit of vinegar regulation system pH=4～5, make gelatin-gum arabic that multiple aggregation take place and form cyst wall, 45 ℃ of reaction temperatures, reaction time 1h.
3) with step 2) product is cooled to below 10 ℃; Add curing agent 5wt% glutaraldehyde with cyst wall crosslinking curing 1h, glutaraldehyde and gelatin mass ratio are 1: 1～5: 1, regulate pH=9～11 with the aqueous slkali regulation system; And make system temperature be heated to 45～60 ℃, continue reaction 90min; The microcapsules that obtain are separated in the adding polyphenol solution,, continue reaction down at 20～30 ℃ and got final product in 10 hours.
Said surfactant is the composite of nonionic surface active agent, HLB=8～13, and wherein nonionic surface active agent has: Span is serial, OP is serial and Tween is serial.
Described Span series is Span 85, Span 80 and Span 60; OP series is OP-9, OP-10 and OP-15; Tween series is: Tween 80, Tween 60 or Tween 40.
Said aqueous slkali is a weak base: comprise sodium carbonate, sodium acid carbonate, potash, saleratus, ammonium carbonate or carbonic hydroammonium, concentration is 0.02～0.1gmL
-1
Said polyphenol is: tannic acid, apple polyphenol or Tea Polyphenols, its concentration are 0.5wt%～3wt%.
Said optimum process condition is: step 1) gelatin and gumwater mass ratio are 1: 1, and concentration is 2wt%, and about surfactant HLB=10, concentration is 0.001gmL
-1Step 2) electrophoresis liquid and wall material mass ratio are 5: 1 in; Spirit of vinegar concentration is 5%～10%, multiple aggregation system pH=4.5～5.0, and glutaraldehyde concentration is 10wt% in the step 3); With the gelatin mass ratio be 4: 1; Rate of addition is 1～3mL/min, and polyphenol concentration is 1wt% in the step 4), volume 50mL.
Effect of the present invention is: the smooth and single dispersion of surface of microcapsule of this prepared of usefulness such as Fig. 3 c, d, and particle diameter is even, and productive rate is high; Like Fig. 1, Fig. 2, and cyst wall intensity is high, good toughness; At high temperature do not break, also not damaged behind the gross distortion, like Fig. 4 b, c; And make display device obtain display image, like Fig. 5 b.
Description of drawings
Fig. 1 is microcapsules productive rate and average grain diameter size and dispersant concentration graph of a relation;
Along with the increase of surfactant concentration, the microcapsules average grain diameter diminishes, and concentration is greater than 0.001gmL
-1After be stabilized in about 50 μ m; Surfactant concentration is lower than 0.001gmL
-1The time, the productive rate of microcapsules increases along with the increase of surfactant concentration, is higher than 0.001gmL
-1After, productive rate reduces, at 0.001gmL
-1The place reaches maximum.
Fig. 2 is a microcapsules particle diameter distribution histogram;
Utilize GMS image analysis system software analysis to record, microcapsules particle diameter distribution Normal Distribution, average grain diameter are between 30～60 μ m, and standard deviation is 1.5～2.0 μ m, and the microcapsules ratio of particle diameter in 20～80 mu m ranges is about 75%～85%.
Fig. 3 a, b are respectively the microcapsules transmitted light optical microscope image and the reverberation optical microscope image of traditional handicraft preparation; C, d are respectively the microcapsules transmitted light optical microscope image and the reverberation optical microscope image of optimum process condition preparation;
Fig. 4 a is an image after the microcapsules dehydration of traditional handicraft preparation, and b is microcapsules image behind 30 ℃ of oven dry 20min of preparation optimum process condition under, and c is microcapsules image after drying 20min under 50 ℃ of preparation optimum process condition under.
Fig. 5 a is a microcapsules display layer micro-image, and b is a display device.Can find out that from figure microcapsules are excellent, and can demonstrate distinct image.
The specific embodiment
(1) 1.0g gelatin and 1.0g Arabic gum are mixed with the 1wt% aqueous solution with 45 ℃ of deionized waters, regulate pH=6～7, the maintenance system adds the compound surfactant 0.0005gmL of HLB=8 under 45 ℃
-1, disposable injection 4g electrophoresis liquid, the 600rpm rotating speed disperses 15min down, makes it generate the emulsion of O/W, about 0.5h, transfers pH=4～5 with dilute acetic acid solution, and isothermal reaction 1h reduces to room temperature then.
(2) on the rocks (1) system temperature is cooled to below 10 ℃, adds the 40mL5wt% glutaraldehyde and be cured about 1h; With weak caustic solution system is transferred to pH=9, again reaction temperature is risen to 45 ℃, and keep 90min, reduce to room temperature, stirred overnight separates obtaining microcapsules.
(3) microcapsules that (2) obtained join in the 50mL0.5wt% tannic acid, react 10h down at 20 ℃, reduce to room temperature, and washing separates.
Instance 2
(1) 1.5g gelatin and 1.0g Arabic gum are mixed with the 3wt% aqueous solution with 45 ℃ of deionized waters, regulate pH=6～7, the maintenance system adds the compound surfactant 0.0015gmL of HLB=9 under 45 ℃
-1, disposable injection 15g electrophoresis liquid, the 600rpm rotating speed disperses 15min down, makes it generate the emulsion of O/W, about 0.5h, transfers pH=4～5 with dilute acetic acid solution, and isothermal reaction 1h reduces to room temperature then.
(2) on the rocks (1) system temperature is cooled to below 10 ℃, adds the 90mL5% glutaraldehyde and be cured 1h; With weak caustic solution system is transferred to pH=10, again reaction temperature is risen to 45 ℃, and keep 90min, reduce to room temperature, stirred overnight separates obtaining microcapsules.
(3) microcapsules that (2) obtained join in the 50mL1wt% tannic acid, react 10h down at 25 ℃, reduce to room temperature, and washing separates.
Instance 3
(1) 2.0g gelatin and 1.0g Arabic gum are mixed with the 4wt% aqueous solution with 45 ℃ of deionized waters, regulate pH=6～7, the maintenance system adds the compound surfactant 0.003gmL of HLB=13 under 45 ℃
-1, disposable injection 30g electrophoresis liquid, the 600rpm rotating speed disperses 15min down, makes it generate the emulsion of O/W, about 0.5h, transfers pH=4～5 with dilute acetic acid solution, and isothermal reaction 1h reduces to room temperature then.
(2) on the rocks (1) system temperature is cooled to below 10 ℃, adds the 200mL5wt% glutaraldehyde and be cured about 1h; With weak caustic solution system is transferred to pH=11, again reaction temperature is risen to 45 ℃, and keep 90min, reduce to room temperature, stirred overnight separates obtaining microcapsules.
(3) microcapsules that (2) obtained join in the 50mL 3wt% apple polyphenol, react 10h down at 30 ℃, reduce to room temperature, and washing separates.
Instance 4
(1) 1.0g gelatin and 1.0g Arabic gum are mixed with the 2wt% aqueous solution with 45 ℃ of deionized waters, regulate pH=6～7, the maintenance system adds the compound surfactant 0.001gmL of HLB=10 under 45 ℃
-1, disposable injection 10g electrophoresis liquid, the 600rpm rotating speed disperses 15min down, makes it generate the emulsion of O/W, about 0.5h, transfers pH=4～5 with dilute acetic acid solution, and isothermal reaction 1h reduces to room temperature then.
(2) on the rocks (1) system temperature is cooled to below 10 ℃, adds the 40mL5% glutaraldehyde and be cured about 1h; With weak caustic solution system is transferred to pH=10, again reaction temperature is risen to 45 ℃, and keep 90min, reduce to room temperature, stirred overnight separates obtaining microcapsules.
(3) microcapsules that (2) obtained join in the 50mL 1wt% apple polyphenol, react 10h down at 25 ℃, reduce to room temperature, and washing separates.
Claims (5)
1. the preparation method of a black and white electrophoretic display microcapsule is characterized in that the steps include:
1) be that 1: 1～2: 1 gelatin and Arabic gum is as the wall material with mass ratio; The use temperature is the aqueous solution that 45 ℃ deionized water is made into 1wt%～4wt%; The compound surfactant of HLB=8～13 is added in the solution, and making its concentration is 0.0005～0.003gmL
-1, and with alkali regulator solution pH=6～7;
2) electrophoresis liquid is added in the aqueous solution of step 1), disperses 20～30min, the mass ratio of electrophoresis liquid and wall material is 2: 1～10: 1, obtains O/W type emulsion; With spirit of vinegar regulation system pH=4～5, make gelatin-gum arabic that multiple aggregation take place and form cyst wall, 45 ℃ of reaction temperatures, reaction time 1h;
3) with step 2) product is cooled to below 10 ℃; Add curing agent 5wt% glutaraldehyde with cyst wall crosslinking curing 1h, glutaraldehyde and gelatin mass ratio are 1: 1～5: 1, regulate pH=9～11 with the aqueous slkali regulation system; And make system temperature be heated to 45～60 ℃, continue reaction 90min; The microcapsules that obtain are separated in the adding 50mL polyphenol solution, continue reaction down at 20～30 ℃ and got final product in 10 hours.
2. preparation method according to claim 1 is characterized in that surfactant is the composite of nonionic surface active agent, HLB=8～13, and wherein nonionic surface active agent has: Span series, OP is serial and Tween is serial.
3. preparation method as claimed in claim 2 is characterized in that described Span series is Span 85, Span 80 and Span 60; OP series is OP-9, OP-10 and OP-15; Tween series is: Tween 80, Tween 60 or Tween 40.
4. preparation method according to claim 1 is characterized in that said aqueous slkali is weak base: comprise sodium carbonate, sodium acid carbonate, potash, saleratus, ammonium carbonate or carbonic hydroammonium.
5. preparation method according to claim 1, it is characterized in that said polyphenol is: tannic acid, apple polyphenol or Tea Polyphenols, its concentration are 0.5wt%～3wt%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2732240A1 (en) * | 1995-03-30 | 1996-10-04 | Arneodo Christophe Jean Franco | Micro-encapsulation by coacervation at low temp. |
| US20040041306A1 (en) * | 2002-09-03 | 2004-03-04 | Anandaraman Subramaniam | Preparation of microcapsules |
| CN1772364A (en) * | 2005-10-27 | 2006-05-17 | 天津大学 | Prepn process of microcapsule containing Hansa yellow 100 electrophoresis liquid |
| CN101451014A (en) * | 2007-12-03 | 2009-06-10 | 东北农业大学 | Method for preparing novel microcapsule wall material crosslinking gelatin |
-
2011
- 2011-10-27 CN CN2011103298748A patent/CN102441354A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2732240A1 (en) * | 1995-03-30 | 1996-10-04 | Arneodo Christophe Jean Franco | Micro-encapsulation by coacervation at low temp. |
| US20040041306A1 (en) * | 2002-09-03 | 2004-03-04 | Anandaraman Subramaniam | Preparation of microcapsules |
| CN1772364A (en) * | 2005-10-27 | 2006-05-17 | 天津大学 | Prepn process of microcapsule containing Hansa yellow 100 electrophoresis liquid |
| CN101451014A (en) * | 2007-12-03 | 2009-06-10 | 东北农业大学 | Method for preparing novel microcapsule wall material crosslinking gelatin |
Non-Patent Citations (2)
| Title |
|---|
| 裴春岚等: "磁泳微胶囊的制备及其涂膜显示性能", 《过程工程学报》 * |
| 郭慧林等: "准均匀分散电子墨水微胶囊的制备研究", 《功能材料》 * |
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Application publication date: 20120509 |