CN104140691A - Electrophoresis display particle and preparation method thereof - Google Patents
Electrophoresis display particle and preparation method thereof Download PDFInfo
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- CN104140691A CN104140691A CN201310169565.8A CN201310169565A CN104140691A CN 104140691 A CN104140691 A CN 104140691A CN 201310169565 A CN201310169565 A CN 201310169565A CN 104140691 A CN104140691 A CN 104140691A
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Abstract
The invention discloses an electrophoresis display particle. The electrophoresis display particle comprises a pigment particle; and the pigment particle is a nanometer pigment particle, the external surface of the nanometer pigment particle forms a lipophilic or hydrophilic surface modification layer, and the external surface of the lipophilic or hydrophilic surface modification layer is coated with a layer of an oil-soluble or water-soluble polymer with an active function group. The invention also discloses a preparation method of the electrophoresis display particle. The electrophoresis display particle has the advantages of adjustable density and particle size, single particle size distribution, perfect spherical shape of microspheres, good glossiness, and realization of charged particle electrophoresis performance enhancement due to a large amount of active function groups capable of a large amount of charges in the polymer layer. The preparation method has the advantages of simple operation, mild reaction, realization of the preparation of various complex polyphase electrophoresis display particles, single and stable particle size distribution, no agglomeration or rapid settlement phenomena, and low particle density, can promote the development of the electrophoresis display industry, can be applied in many future fields, and has inestimable values.
Description
Technical field
The invention belongs to electrophoretic display technology field, be specifically related to a kind of electrophoresis displaying particle and preparation method thereof.
Background technology
Electrophoretic display technology appears at colloidal solution and biomacromolecule field the earliest, under electric field action, utilizes the difference of the specific charge of material to separate the particle of different sizes or the material of different molecular weight size, to reach classification and the purification of different material.
In recent years, research staff adopts the method for electrophoresis to prepare display screen of new generation, the charged particle of different colours is prepared into suspension by they, after different suspension is mixed, carry out emulsification and be overmolding to microcapsule, again capsule is fixed on conducting film by the mode of coating, under alive effect, makes outside the particle of different colours show different pictures.The display screen of this new generation, rely on micro-voltage (5-40V) to show, and standby time approaches 1 month; Even if also can keep the high definition of early stage picture, stable state to show in the situation that there is no power supply; Its reflection source that relies on particle shows, as watched books, splendid to sight protectio; It is raw materials used is trace mineral, greening and environmental protection; It can be prepared into fexible film demonstration, light weight and easy to carry, practical space and extensive.
Although particle eletrophoresis technique of display market outlook are fine, also less stable of current technology, as excessive in the particle diameter of electrophoresis particle, distribute wide, pattern is various, and each particle specific charge is different, responds asynchronous; Electrophoresis liquid is organic reagent, and electrophoresis particle is main mainly with inorganics, and the two density difference, apart from excessive, has had a strong impact on electric field response time and the bistable display of particle; If adopting single polymer microsphere to prepare electrophoresis particle is completely to improve particle diameter, pattern, and and the density difference distance of electrophoresis liquid, but organic molecule color and luster is not good, and the phenomenons such as swelling and microballoon dissociates also easily occur in electrophoresis liquid.Therefore,, in order further to improve electrophoresis particle performance and to prepare higher-quality product, it is imperative developing a kind of new electrophoresis particle.
Summary of the invention
First object of the present invention provides one can carry high performance electrophoresis displaying particle, to solve the deficiencies in the prior art part.
Second object of the present invention is to provide the preparation method of above-mentioned electrophoresis displaying particle.
For reaching first object, the present invention adopts following technical scheme:
A kind of electrophoresis displaying particle, comprises pigment particles; Described pigment particles is nano-level pigment particle, and the outside surface of described nano-level pigment particle forms an oleophylic or hydrophilic surface modification layer, and the coated one deck of described oleophylic or hydrophilic surface modification layer outside surface is with oil soluble or the water-soluble polymers of active function groups.
Described nano-level pigment particle pattern can be any pattern, particle diameter is preferably 1-80 nanometer, more preferably 5-50 nanometer.
As preferably, described nano-level pigment particle is mainly inorganics, and should have high color and luster, as titanium dioxide, Z 250, chromium sesquioxide, ventilation breather (verdigris) and Sudan red.Inorganics composition can be that single component can be also multiple mixing; Can be oxide compound or inorganic salt.
Described oil soluble or water-soluble polymers should have high light transmittance and contain a large amount of active function groups, be selected from-OH of described active function groups ,-NH
3the combination that ,-COOH ,-CONH-,-Cl and they are at least two kinds.
For reaching second object, the present invention adopts following technical scheme:
A preparation method for electrophoresis displaying particle, is made up of following steps:
A, make nano-level pigment particle external surface form oleophylic or hydrophilic surface modification layer, obtain modified pigment particle;
B, make modified pigment particle surface coated oil soluble or water-soluble polymers with active function groups, obtain complex microsphere.
As preferably, in A step, after being dispersed to dispersion agent, nano-level pigment particle adds coupling agent, then carry out ultrasonication, finally carry out eccentric cleaning processing, obtain modified pigment particle.
As preferably, described coupling agent is selected from silane coupling agent and titanate coupling agent, preferably titanate coupling agent.
As preferably, in B step, modified pigment particle is dispersed in the oil soluble or water-soluble polymer solution with active function groups, obtain stable suspension; Stable suspension is carried out to emulsification, obtain emulsion; Emulsion is carried out to drying treatment, obtain complex microsphere.
As preferably, described polymkeric substance is selected from the mixture of at least two kinds of PVA, PMMA, PS, PE, PP, PEO, low molecule PEG400, glycerol and they.
As preferably, the emulsifying agent that described emulsification adopts can be macromole type, also can be small molecules type, it can be single agents, also can be multiple composite emulsifier, can be lipophilic or hydrophilic, be preferably the good macromolecule emulsifier of film properties, as PVA, gelatin, hydrolysis styrene-maleic anhydride copolymer, PEO and PEG20000 etc.
As preferably, the temperature of whole preparation process is 30～80 DEG C.
As preferably, in B step, in emulsification process, the rotating speed of emulsifying head is 1000～10000r/min, and emulsification times is 10～120 minutes.
As preferably, in B step, can adopt the first drying mode of centrifugal post-drying, also can adopt spraying drying mode, preferably adopt spraying drying mode, spraying drying temperature is 50～150 DEG C.
Electrophoresis displaying particle of the present invention, density and particle diameter can regulate and control, and size distribution is single, and it is perfect spherical that microballoon becomes, and glossiness is good, and a large amount of active function groups in macromolecule layer can adsorb a large amount of electric charges, and charged particle electrophoretic property is strengthened.And preparation method of the present invention is simple to operate, reaction temperature and, can prepare the heterogeneous electrophoresis displaying particle of various complexity, particle diameter distribution single stable, without reuniting and the phenomenon such as rapid subsidence, particle density is low; This method not only can promote the development of electrophoresis showed industry, can also be in multiple fields application in future, and its value is inestimable.
Brief description of the drawings
Fig. 1 is the structural representation of electrophoresis displaying particle of the present invention.
In figure:
1-nano-level pigment particle; 2-oleophylic or hydrophilic surface modification layer; 3-with oil soluble or the water-soluble polymers of active function groups.
Embodiment
Now the invention will be further described in conjunction with the accompanying drawings and embodiments:
As shown in Figure 1, electrophoresis displaying particle of the present invention, its kernel is nano-level pigment particle 1, the outside surface of this nano-level pigment particle forms an oleophylic or hydrophilic surface modification layer 2, and the coated one deck of described oleophylic or hydrophilic surface modification layer 2 outside surface is with oil soluble or the water-soluble polymers 3 of active function groups.
Above-mentioned nano-level pigment particle pattern can be any pattern, particle diameter is preferably 1-80 nanometer, is preferably 5-50 nanometer.
Above-mentioned nano-level pigment particle is mainly inorganics, and should have high color and luster, as titanium dioxide, Z 250, chromium sesquioxide, ventilation breather (verdigris) and Sudan red.Inorganics composition can be that single component can be also multiple mixing; Can be oxide compound or inorganic salt.
Above-mentioned oil soluble or water-soluble polymers should have high light transmittance and contain a large amount of active function groups, be selected from-OH of described active function groups ,-NH
3the combination that ,-COOH ,-CONH-,-Cl and they are at least two kinds.
The preparation method of above-mentioned electrophoresis displaying particle is as follows:
A, modified pigment particle preparation: be under the condition of 30～80 DEG C in temperature, after being dispersed to dispersion agent, nano-level pigment particle adds coupling agent, then carry out ultrasonication, make nano-level pigment particle external surface form oleophylic or hydrophilic surface modification layer, finally carry out eccentric cleaning processing, obtain modified pigment particle;
B, complex microsphere preparation: modified pigment particle is dispersed in the oil soluble or water-soluble polymer solution with active function groups, obtains stable suspension; Stable suspension is carried out to emulsification, and in emulsification process, the rotating speed of emulsifying head is 1000～10000r/min, and emulsification times is 10～120 minutes, obtains emulsion; Emulsion is carried out to drying treatment, make modified particle surface coated oil soluble or water-soluble polymers with active function groups, obtain complex microsphere.
Above-mentioned dispersion agent is selected from toluene, ethanol etc.; Above-mentioned coupling agent is selected from silane coupling agent and titanate coupling agent, preferably titanate coupling agent.
Above-mentioned polymkeric substance is selected from the mixture of at least two kinds of PVA, PMMA, PS, PE, PP, PEO, low molecule PEG400, glycerol and they.
The emulsifying agent that above-mentioned emulsification adopts can be macromole type, also can be small molecules type, it can be single agents, also can be multiple composite emulsifier, can be lipophilic or hydrophilic, be preferably the good macromolecule emulsifier of film properties, as PVA, gelatin, hydrolysis styrene-maleic anhydride copolymer, PEO and PEG20000 etc.
The volume ratio of aforementioned stable suspension and emulsifying agent is 1:1～1:20(V:V)
Above-mentioned drying treatment can adopt the first drying mode of centrifugal post-drying, also can adopt spraying drying mode, preferably adopts spraying drying mode, and spraying drying temperature is 50～150 DEG C.
Embodiment 1
The preparation of modified pigment particle:
By 10g titanium dioxide (TiO
2) powder (particle diameter 5～50nm) is dispersed in 100mL toluene, adds titanate coupling agent (TMC-201; Sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester) 1.5g, after ultrasonic 30min, the rotating speed eccentric cleaning by slurries with 3000r/min, 2～3 times repeatedly, obtains modification TiO
2.
Complex microsphere preparation:
By 5g modification TiO
2be scattered in containing in the toluene solution of 10% poly-dodecyl acrylate (Mn=50000～80000, d < 1.3) of 30mL, at 60～70 DEG C, fully stir 2～3h, obtain stable suspension; Gained suspension 10mL is dispersed to 100mL and contains 2% polyvinyl alcohol (PVA; Alcoholysis degree 98～99%, Mn=30000～60000) in the aqueous solution, after emulsifying head 5000r/min, emulsification 15～20min, emulsion is dried at 100 DEG C of degree, repeatedly clean 3 times with distilled water, obtain by poly-dodecyl acrylate, PVA and TiO
2the complex microsphere of composition, collecting particle microballoon test size distribution is 0.4～0.6 μ m, median size 0.51 μ m, particle density is 2.83g/mL (rutile titanium dioxide, ρ=4.2～4.3g/mL).
Embodiment 2
The preparation of modified pigment particle:
5g copper-chrome black powder (particle diameter 5～20nm) is dispersed in 100mL toluene, adds titanate coupling agent 2.5g, at 45 DEG C, after ultrasonic 30min, by slurries 3000r/min eccentric cleaning, 2～3 times repeatedly, both obtained Modified Cu chrome black.
By above-mentioned process modification 5g ferriferrous oxide nano-particle (Fe
3o
4, particle diameter 15～20nm).
Complex microsphere preparation:
By 3g Modified Cu chrome black and 3g MODIFIED Fe
3o
4be scattered in the toluene solution containing 15% poly-octadecyl acrylate (Mn=30000～50000, d < 1.5) of 30mL, at 60～70 DEG C, fully stir 2～3h, obtain stable suspension; Gained suspension 10mL is dispersed to 100mL and contains in 2% gelatin (emulsifying agent) aqueous solution, after emulsifying head 6000r/min, emulsification 15～20min, emulsion is sprayed at 100 DEG C dry, obtain by poly-octadecyl acrylate, gelatin, copper-chrome black and Fe
3o
4the complex microsphere of composition, collecting particle microballoon test size distribution is 0.2～0.45 μ m, median size 0.36 μ m, particle density is 2.33g/mL (copper-chrome black, ρ=4.6～4.8g/mL; Fe
3o
4, ρ=5.18g/mL).
Embodiment 3
The preparation of modified pigment particle:
By 8g chromoxide green (Cr
2o
3) powder (particle diameter 20～50nm) is dispersed in 100mL toluene, adds titanate coupling agent 1.5g, after ultrasonic 30min, slurries, with 3000r/min eccentric cleaning, 2～3 times repeatedly, obtained to modification Cr
2o
3.
Complex microsphere preparation:
By 4g modification Cr
2o
3be scattered in 10% poly-dodecyl acrylate (Mn=50000～80000 that contain of 50mL, d<1.3) and 2% polystyrene (Mn=50000～80000, d<1.3) in toluene solution, fully stir 2～3h at 75 DEG C, obtain stable suspension; Gained suspension 10mL is dispersed to 100mL and contains 2% PVA(emulsifying agent) in the aqueous solution, after emulsifying head 4500r/min, emulsification 15～20min, emulsion is sprayed under 100 DEG C of degree dry, obtain by poly-dodecyl acrylate, polystyrene, PVA, Cr
2o
3the complex microsphere of composition, collecting particle microballoon test size distribution is 0.5～0.63 μ m, median size 0.58 μ m, particle density is 3.02g/mL (Cr
2o
3, ρ=5.21g/mL).
Embodiment 4
The preparation of modified pigment particle:
By 15g titanium dioxide (TiO
2) powder (particle diameter 5～50nm) is dispersed in 100mL ethanol, adds titanate coupling agent (TMC-201; Sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester) 2.5g, after ultrasonic 30min, by slurries 3000r/min eccentric cleaning, 2～3 times repeatedly, obtain hydrophilic modification TiO
2.
Complex microsphere preparation:
By 5g modification TiO
2be scattered in 8% the PVA(alcoholysis degree 98～99% of 30mL, Mn=30000～60000) and the solution of 1% gelatin in, at 60～70 DEG C, fully stir 1-2h, obtain stable suspension; Gained suspension 10mL is dispersed to 100mL to be contained in 2% the politef solution of propylene glycol fatty acid ester (emulsifying agent), after emulsifying head 3000r/min, emulsification 30min, emulsion is sprayed under 120 DEG C of degree dry, obtain by gelatin, PVA, propylene glycol fatty acid ester and TiO
2the complex microsphere of composition, collecting particle microballoon test size distribution is 0.3～0.6 μ m, median size 0.43 μ m, particle density is 2.94g/mL (rutile titanium dioxide, ρ=4.2～4.3g/mL).
Embodiment 5
The preparation of modified pigment particle:
By 15g titanium dioxide (TiO
2) powder (particle diameter 5～50nm) is dispersed in 100mL ethanol, adds silane coupling agent (KH-550; γ-aminopropyl triethoxysilane) 1.5g, after ultrasonic 30min, by slurries 3000r/min eccentric cleaning, 2～3 times repeatedly, obtain hydrophilic modification TiO
2.
Complex microsphere preparation:
By 5g modification TiO
2be scattered in 8% the PEO(Mn=50000 of 30mL) and the solution of 1% gelatin in, at 60～70 DEG C, fully stir 1-2h, obtain stable suspension; Gained suspension 10mL is dispersed to 100mL to be contained in 2% the politef solution of propylene glycol fatty acid ester (emulsifying agent), after emulsifying head 3000r/min, emulsification 30min, emulsion is sprayed under 120 DEG C of degree dry, obtain by gelatin, PEO, propylene glycol fatty acid ester and TiO
2the complex microsphere of composition, collecting particle microballoon test size distribution is 0.3～0.6 μ m, median size 0.43 μ m, particle density is 2.94g/mL (rutile titanium dioxide, ρ=4.1g/mL).
Embodiment 6
The preparation of modified pigment particle:
Adopt the method for embodiment 1 or embodiment 4 or embodiment 5 to obtain modification TiO
2.
Complex microsphere preparation:
By 5g modification TiO
2be scattered in 4% the PEO(Mn=50000 of 30mL), 4% PVA(alcoholysis degree 98～99%, Mn=30000～60000) in 1% hydrolysis styrene-maleic anhydride copolymer solution, at 60～70 DEG C, fully stir 1-2h, obtain stable suspension; Gained suspension 10mL is dispersed to 100mL and contains 2% Span80(emulsifying agent) politef solution in, after emulsifying head 3000r/min, emulsification 30min, emulsion is sprayed under 120 DEG C of degree dry, obtain by hydrolysis styrene-maleic anhydride copolymer, PEO, PVA, Span80 and TiO
2the complex microsphere of composition, collecting particle microballoon test size distribution is 0.3～0.6 μ m, median size 0.43 μ m, particle density is 2.94g/mL (rutile titanium dioxide, ρ=3.9～4.1g/mL).
Claims (10)
1. an electrophoresis displaying particle, comprise pigment particles, it is characterized in that, described pigment particles is nano-level pigment particle, the outside surface of described nano-level pigment particle forms an oleophylic or hydrophilic surface modification layer, and the coated one deck of described oleophylic or hydrophilic surface modification layer outside surface is with oil soluble or the water-soluble polymers of active function groups.
2. a kind of electrophoresis displaying particle according to claim 1, is characterized in that, the particle diameter of described nano-level pigment particle is 1-80 nanometer.
3. a kind of electrophoresis displaying particle according to claim 1 and 2, is characterized in that, described pigment particles is selected from titanium dioxide, Z 250, chromium sesquioxide, ventilation breather and Sudan red.
4. a kind of electrophoresis displaying particle according to claim 1, is characterized in that, be selected from-OH of described active function groups ,-NH
3the combination that ,-COOH ,-CONH-,-Cl and they are at least two kinds.
5. a kind of preparation method of electrophoresis displaying particle as claimed in claim 1, is characterized in that, is made up of following steps:
A, make nano-level pigment particle external surface form oleophylic or hydrophilic surface modification layer, obtain modified pigment particle;
B, make modified pigment particle surface coated oil soluble or water-soluble polymers with active function groups, obtain complex microsphere.
6. preparation method according to claim 5, is characterized in that, in A step, adds coupling agent after nano-level pigment particle is dispersed to dispersion agent, then carries out ultrasonication, finally carries out eccentric cleaning processing, obtains modified pigment particle.
7. preparation method according to claim 6, is characterized in that, described coupling agent is selected from silane coupling agent and titanate coupling agent.
8. according to the arbitrary described preparation method of claim 5 to 7, it is characterized in that, in B step, modified pigment particle is dispersed in the oil soluble or water-soluble polymer solution with active function groups, obtain stable suspension; Stable suspension is carried out to emulsification, obtain emulsion; Emulsion is carried out to drying treatment, obtain complex microsphere.
9. preparation method according to claim 8, is characterized in that, described polymkeric substance is selected from the mixture of at least two kinds of PVA, PMMA, PS, PE, PP, PEO, low molecule PEG400, glycerol and they.
10. preparation method according to claim 8, is characterized in that, the emulsifying agent that described emulsification adopts is selected from the macromolecule emulsifier that film forming properties is good, comprises PVA, gelatin, hydrolysis styrene-maleic anhydride copolymer, PEO and PEG20000.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019056915A1 (en) * | 2017-09-20 | 2019-03-28 | 广州奥翼电子科技股份有限公司 | Pigment particle and electrophoretic display unit applied to electrophoretic display |
| CN111129507A (en) * | 2019-12-13 | 2020-05-08 | 同济大学 | Gas diffusion layer for fuel cell and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816463A (en) * | 2011-06-09 | 2012-12-12 | 希毕克斯影像有限公司 | Silane-containing pigment particles for electrophoretic display, electrophoretic fluid and electrophoretic display device |
-
2013
- 2013-05-06 CN CN201310169565.8A patent/CN104140691A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816463A (en) * | 2011-06-09 | 2012-12-12 | 希毕克斯影像有限公司 | Silane-containing pigment particles for electrophoretic display, electrophoretic fluid and electrophoretic display device |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019056915A1 (en) * | 2017-09-20 | 2019-03-28 | 广州奥翼电子科技股份有限公司 | Pigment particle and electrophoretic display unit applied to electrophoretic display |
| US11124655B2 (en) | 2017-09-20 | 2021-09-21 | Guangzhou Oed Technologies, Inc. | Surface-modified pigment particles for electrophoretic display and electrophoretic display device |
| CN111129507A (en) * | 2019-12-13 | 2020-05-08 | 同济大学 | Gas diffusion layer for fuel cell and preparation method and application thereof |
| CN111129507B (en) * | 2019-12-13 | 2021-02-02 | 同济大学 | Gas diffusion layer for fuel cell and preparation method and application thereof |
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Application publication date: 20141112 |