CN112745465A - Ionic liquid surface-coated inorganic pigment electrophoretic particle and preparation method thereof - Google Patents
Ionic liquid surface-coated inorganic pigment electrophoretic particle and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an ionic liquid surface-coated inorganic pigment electrophoretic particle and a preparation method thereof, the inorganic pigment electrophoretic particle consists of a core and a shell, the core is an inorganic pigment particle, the shell is an ionic liquid polymer and is coated on the surface of the core, and the particle size of the particle is 200-450 nm. The ionic liquid surface coating inorganic pigment electrophoretic particle prepared by the invention has the advantages that the surface charge performance is obviously improved, the sphericity degree of the electrophoretic particle is good, the particle size monodispersity is good, the particle size of the particle can be regulated and controlled by changing the using amount of raw materials according to needs, the density of the prepared ionic liquid surface coating modified inorganic pigment electrophoretic particle can be obviously reduced, and the density value can be regulated and controlled by changing the using amount of the raw materials according to needs.
Description
Technical Field
The invention relates to the technical field of electrophoretic display, in particular to an inorganic pigment electrophoretic particle coated on the surface of an ionic liquid and a preparation method thereof.
Background
The electronic ink is a basic material applied to a reflection-type electronic paper display, and is formed by coating charged electrophoretic particles and a dispersion medium in microcapsules. The electronic paper is used as a display screen, and the display response speed of the electronic paper needs to be fast enough, for example, the response time needs to be less than 42 milliseconds, so that the universality requirement can be met.
When the charged electrophoretic particles dispersed in the electrophoretic display fluid undergo electrophoresis under the action of an applied electric field, the speed thereof mainly depends on the particle charge amount, the viscous damping experienced, the dielectric properties of the fluid, the electric field strength, and other factors. For electrophoretic particles, the electrophoretic properties of the particles are mainly determined by the electrical and electric properties of the charges carried on the surface of the particles.
In order to improve the charge performance of the electrophoretic particles, various polar groups (e.g., X, NH2, COOH, ester groups, etc.) have been introduced into the surface of the electrophoretic particles (Han j.j., Zhang w.h., Li x.g., Sun c., Shao j.z., Feng y.q., Materials Research Innovations, 2015, 19(1): 24-27) to change the surface properties thereof. Although the polar group can adjust and change the surface property of the electrophoretic particle, increase the surface polarity and improve the charge performance of the electrophoretic particle, the adjustment range is limited, the surface charge capacity cannot be effectively increased, and the electric field response speed of the electrophoretic particle is difficult to obviously improve.
Charge control agents have also been introduced into electrophoretic display fluid systems (B.J. Park, S.Y. Hong, H.H. Sim, H.J. Choi, Y.S. Yoon, Materials Chemistry and Physics, 2012, 135: 259-. Commonly used charge control agents are metal soaps, organic amines, organic sulfates or sulfonates, organic phosphates or phosphates, cetyltrimethylammonium bromide, and the like. The charge control agent can be partially ionized in an organic dispersion medium to generate positive and negative ions, and an electrostatic double electric layer is formed on the surface of an electrophoretic particle to enhance the charge performance of the electrophoretic particle, so that the electric field response speed of the electrophoretic particle is improved. The electric field response speed of the electrophoretic particles is improved due to the addition of the charge control agent, the electrophoretic mobility can be improved to 10 < -9 > -10 < -10 > orders of magnitude, and the electric field response time is also reduced to hundreds of milliseconds. But still cannot meet the requirement of dynamic display of the electronic paper.
In addition, since different electrophoretic particles have different structures and surface properties, their requirements for charge control agents are different. In an electrophoretic display system containing a plurality of electrophoretic particles, a plurality of charge control agents are used simultaneously, so that a plurality of components in the system are caused, the interaction among the components is complicated, and good electric field response performance and image display quality are difficult to obtain. Therefore, it is difficult to obtain good electric field response performance only by adding the charge control agent.
Disclosure of Invention
The invention aims to provide an ionic liquid surface-coated inorganic pigment electrophoretic particle with a composite structure for electronic ink and a preparation method thereof.
The invention is realized by the following technical scheme:
the electrophoretic particle of inorganic pigment coated on the surface of ionic liquid consists of core of inorganic pigment particle and shell of ionic liquid polymer coated on the surface of core. The particle size of the inorganic pigment electrophoretic particles is 200-450 nm.
The invention also provides a preparation method of the ionic liquid surface-coated inorganic pigment electrophoretic particle, which comprises the following steps:
the preparation method of the ionic liquid surface-coated inorganic pigment electrophoretic particle is characterized by comprising the following steps of:
s1, mixing methanol with alkyl bromide, adding 1-vinyl imidazole, heating the mixed solution to 40-80 ℃, and reacting for 12-48 hours under the conditions of stirring and refluxing to obtain vinyl alkyl imidazole bromide ionic liquid;
s2, adding inorganic pigment particles with the particle size range of 150-400nm into water, adding 1-vinyltriethoxysilane, performing ultrasonic dispersion for 15min, heating the mixed solution to 40-90 ℃, reacting for 12-48h under the condition of stirring, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product at 40-80 ℃ for 6-24h to obtain surface vinyl modified inorganic pigment particles;
s3, distilling the vinyl alkyl imidazole bromide ionic liquid under reduced pressure, adding the ionic liquid, the surface vinyl modified inorganic pigment particles and divinylbenzene into water, ultrasonically dispersing for 15min, heating the solution to 70 ℃, adding potassium persulfate, continuing to react for 2-24h, washing the product for 3 times with water and absolute ethyl alcohol, and then drying the product in vacuum at 40-80 ℃ for 6-24h to obtain the ionic liquid surface-coated inorganic pigment electrophoretic particles.
Further, the alkyl group of the bromoalkyl hydrocarbon of step S1 is one or more of propyl group, hexyl group, octyl group, dodecyl group or hexadecyl group.
Further, the inorganic pigment particles are one of titanium dioxide white particles, silica white particles, iron oxide red particles, and cobalt titanate blue particles.
Further, the mass amount of the alkane bromide in the step S1 is 0.1-1.5 times of that of the methanol, and then the 1-vinyl imidazole is added, wherein the mass amount of the 1-vinyl imidazole is 0.1-1.0 times of that of the methanol.
Further, the 1-vinyltriethoxysilane in step S2 is used in an amount of 0.1-10% by mass based on the inorganic pigment particles.
Further, the vinyl alkyl imidazole bromide ionic liquid in the step S3 is used in an amount of 1% to 15% by mass of the surface vinyl modified inorganic pigment particles, and divinylbenzene is used in an amount of 5% to 40% by mass of the surface vinyl modified inorganic pigment particles.
Further, the amount of potassium persulfate used in the step S3 is 5% to 20% by mass based on the surface vinyl-modified inorganic pigment particles.
Compared with the prior art, the ionic liquid surface-coated inorganic pigment electrophoretic particle and the preparation method thereof provided by the invention have the following beneficial effects:
(1) the surface charge performance of the prepared ionic liquid surface-coated inorganic pigment electrophoretic particle is remarkably improved, and the surface charge performance of the electrophoretic particle can be regulated and controlled by changing the type and the dosage of raw materials.
(2) The ionic liquid surface coating modified inorganic pigment electrophoretic particle prepared by the invention has good sphericity and good particle size monodispersity, and the particle size of the particle can be regulated and controlled by changing the consumption of raw materials according to the requirement.
(3) The density of the prepared ionic liquid surface coating modified inorganic pigment electrophoretic particles can be obviously reduced, and the density value can be regulated and controlled by changing the consumption of raw materials according to the requirement.
Drawings
FIG. 1 is a scanning electron microscope image of a vinyl dodecyl imidazole bromide ionic liquid surface coated silica white particle
FIG. 2 is a transmission electron microscope image of cobalt titanate blue particles coated on the surface of vinyl dodecyl imidazole bromide ionic liquid
Detailed Description
The present invention will be further described with reference to the following specific examples.
Embodiment 1, a method for preparing ionic liquid surface-coated titanium dioxide electrophoretic particles, comprising the following steps:
s1, mixing methanol with alkyl bromide, adding 1-vinylimidazole, heating the mixed solution to 40-80 ℃, and reacting for 12-48 hours under the conditions of stirring and refluxing to obtain vinyl alkyl imidazole bromide ionic liquid;
s2, adding titanium dioxide white pigment particles with the particle size range of 150-500nm into water, adding 1-vinyltriethoxysilane, carrying out ultrasonic dispersion for 15min, heating the mixed solution to 40-90 ℃, reacting for 12-48h under the stirring condition, washing the product for 3 times with water and absolute ethyl alcohol, and carrying out vacuum drying on the product for 6-24h at 40-80 ℃ to obtain surface vinyl modified titanium dioxide white pigment particles;
s3, distilling the vinyl alkyl imidazole bromide ionic liquid under reduced pressure, adding the vinyl alkyl imidazole bromide ionic liquid, the surface vinyl modified titanium dioxide particles and divinylbenzene into water, performing ultrasonic dispersion for 15min, heating the solution to 70 ℃, adding potassium persulfate, continuing to react for 2-24h, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product at 40-80 ℃ for 6-24h to obtain the ionic liquid surface-coated titanium dioxide electrophoretic particles.
Wherein the mass dosage of the alkane bromide in the step S1 is 0.1 time of that of the methanol, and the mass dosage of the 1-vinyl imidazole is 0.1 time of that of the methanol; the 1-vinyltriethoxysilane in step S2 accounts for 0.1% of the titanium dioxide particles by mass; the mass amount of the vinyl alkyl imidazole bromide ionic liquid in the step S3 is 1% of the surface vinyl modified inorganic pigment particles, the mass amount of divinylbenzene is 5% of the surface vinyl modified inorganic pigment particles, and the mass amount of potassium persulfate is 5% of the surface vinyl modified inorganic pigment particles.
Embodiment 2, a method for preparing an ionic liquid surface-coated silica electrophoretic particle, comprising the following steps:
s1, mixing methanol with alkyl bromide, adding 1-vinylimidazole, heating the mixed solution to 40-80 ℃, and reacting for 12-48 hours under the conditions of stirring and refluxing to obtain vinyl alkyl imidazole bromide ionic liquid;
s2, adding silicon dioxide with the particle size range of 150-500nm into water, adding 1-vinyltriethoxysilane, performing ultrasonic dispersion for 15min, heating the mixed solution to 40-90 ℃, reacting for 12-48h under the condition of stirring, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product for 6-24h at 40-80 ℃ to obtain surface vinyl modified silicon dioxide particles;
s3, distilling the vinyl alkyl imidazole bromide ionic liquid under reduced pressure, adding the vinyl alkyl imidazole bromide ionic liquid, the surface vinyl modified inorganic pigment particles and divinylbenzene into water, ultrasonically dispersing for 15min, heating the solution to 70 ℃, adding potassium persulfate, continuing to react for 2-24h, washing the product for 3 times with water and absolute ethyl alcohol, and then drying the product in vacuum at 40-80 ℃ for 6-24h to obtain the ionic liquid surface-coated silica electrophoretic particles.
Wherein, the mass dosage of the alkane bromide in the step S1 is 1.5 times of that of the methanol, and the mass dosage of the 1-vinyl imidazole is 1.0 time of that of the methanol; the 1-vinyltriethoxysilane in step S2 accounts for 10% by mass of the silica particles; the mass amount of the vinyl alkyl imidazole bromide ionic liquid in the step S3 is 15% of the surface vinyl modified inorganic pigment particles, the mass amount of divinylbenzene is 40% of the surface vinyl modified inorganic pigment particles, and the mass amount of potassium persulfate is 20% of the surface vinyl modified inorganic pigment particles.
Embodiment 3, a method for preparing blue electrophoretic cobalt titanate particles coated on the surface of ionic liquid, comprising the following steps:
s1, mixing methanol with alkyl bromide, adding 1-vinylimidazole, heating the mixed solution to 40-80 ℃, and reacting for 12-48 hours under the conditions of stirring and refluxing to obtain vinyl alkyl imidazole bromide ionic liquid;
s2, adding cobalt titanate blue particles with the particle size range of 150-500nm into water, adding 1-vinyltriethoxysilane, performing ultrasonic dispersion for 15min, heating the mixed solution to 40-90 ℃, reacting for 12-48h under the condition of stirring, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product for 6-24h at 40-80 ℃ to obtain surface vinyl modified cobalt titanate blue particles;
s3, distilling the vinyl alkyl imidazole bromide ionic liquid under reduced pressure, adding the ionic liquid, the surface vinyl modified cobalt titanate blue particles and divinylbenzene into water, performing ultrasonic dispersion for 15min, heating the solution to 70 ℃, adding potassium persulfate, continuing to react for 2-24h, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product at 40-80 ℃ for 6-24h to obtain the ionic liquid surface coated cobalt titanate blue electrophoretic particles.
Wherein the mass dosage of the alkane bromide in the step S1 is 0.8 time of that of the methanol, and the mass dosage of the 1-vinyl imidazole is 0.8 time of that of the methanol; the 1-vinyltriethoxysilane in step S2 accounts for 6% of the mass amount of the cobalt titanate particles; the mass amount of the vinyl alkyl imidazolium bromide ionic liquid in the step S3 is 8% of the surface vinyl modified inorganic pigment particles, the mass amount of divinylbenzene is 22% of the surface vinyl modified inorganic pigment particles, and the mass amount of potassium persulfate is 12% of the surface vinyl modified inorganic pigment particles.
Embodiment 4, a method for preparing ionic liquid surface-coated titanium dioxide electrophoretic particles, comprising the following steps:
s1, mixing methanol with alkyl bromide, adding 1-vinylimidazole, heating the mixed solution to 40-80 ℃, and reacting for 12-48 hours under the conditions of stirring and refluxing to obtain vinyl alkyl imidazole bromide ionic liquid;
s2, adding titanium dioxide particles with the particle size range of 150-500nm into water, adding 1-vinyltriethoxysilane, performing ultrasonic dispersion for 15min, heating the mixed solution to 40-90 ℃, reacting for 12-48h under the condition of stirring, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product for 6-24h at 40-80 ℃ to obtain surface vinyl modified titanium dioxide inorganic pigment particles;
s3, distilling the vinyl alkyl imidazole bromide ionic liquid under reduced pressure, adding the ionic liquid, the surface vinyl modified titanium dioxide inorganic pigment particles and divinylbenzene into water, performing ultrasonic dispersion for 15min, heating the solution to 70 ℃, adding potassium persulfate, continuing to react for 2-24h, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product at 40-80 ℃ for 6-24h to obtain the ionic liquid surface coated titanium dioxide white electrophoretic particles.
Wherein the mass dosage of the alkane bromide in the step S1 is 0.8 time of that of the methanol, and the mass dosage of the 1-vinyl imidazole is 0.8 time of that of the methanol; the 1-vinyltriethoxysilane in step S2 accounts for 6% of the titanium dioxide particles by mass; the mass amount of the vinyl alkyl imidazolium bromide ionic liquid in the step S3 is 8% of the surface vinyl modified inorganic pigment particles, the mass amount of divinylbenzene is 22% of the surface vinyl modified inorganic pigment particles, and the mass amount of potassium persulfate is 12% of the surface vinyl modified inorganic pigment particles.
Embodiment 5, a method for preparing ionic liquid surface-coated iron oxide electrophoretic particles, comprising the following steps:
s1, mixing methanol and alkyl bromide, adding 1-vinylimidazole, heating the mixed solution to 40-80 ℃, and reacting for 12-48 hours under the conditions of stirring and refluxing to obtain a vinyl alkyl imidazole bromide ionic liquid;
s2, adding iron oxide particles with the particle size range of 150-500nm into water, adding 1-vinyltriethoxysilane, carrying out ultrasonic dispersion for 15min, heating the mixed solution to 40-90 ℃, reacting for 12-48h under the condition of stirring, washing the product for 3 times with water and absolute ethyl alcohol, and carrying out vacuum drying on the product for 6-24h at 40-80 ℃ to obtain surface vinyl modified titanium dioxide inorganic pigment particles;
s3, distilling the vinyl alkyl imidazole bromide ionic liquid under reduced pressure, adding the ionic liquid, the surface vinyl modified titanium dioxide inorganic pigment particles and divinylbenzene into water, performing ultrasonic dispersion for 15min, heating the solution to 70 ℃, adding potassium persulfate, continuing to react for 2-24h, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product at 40-80 ℃ for 6-24h to obtain the ionic liquid surface coated titanium dioxide white electrophoretic particles.
Wherein the mass dosage of the alkane bromide in the step S1 is 0.8 time of that of the methanol, and the mass dosage of the 1-vinyl imidazole is 0.8 time of that of the methanol; the 1-vinyltriethoxysilane in step S2 accounts for 6% of the iron oxide particles by mass; the mass amount of the vinyl alkyl imidazolium bromide ionic liquid in the step S3 is 8% of the surface vinyl modified inorganic pigment particles, the mass amount of divinylbenzene is 22% of the surface vinyl modified inorganic pigment particles, and the mass amount of potassium persulfate is 12% of the surface vinyl modified inorganic pigment particles.
The vinyl dodecyl imidazole bromide ionic liquid polymer-coated silica white particles and the vinyl dodecyl imidazole bromide ionic liquid polymer-coated cobalt titanate blue particles prepared according to the embodiments 2 and 3 of the invention are detected, and the following performance data are obtained:
| sample (I) | Density/g/cm3 | Average particle diameter/nm | Contact angle-o | Y | x | y | Electrophoretic Property/cm2/(V s) |
| Example 2 | 1.3342 | 200 | 97.80 | 92.80 | 0.3078 | 0.3093 | 1.172×10-6 |
| Example 3 | 1.8353 | 168 | 94.68 | 8.9 | 0.2142 | 0.1831 | 2.568×10-6 |
By combining the electron microscope images shown in fig. 1 and fig. 2, it can be known that the ionic liquid surface coating inorganic pigment electrophoretic particles prepared by the invention have higher surface charge performance, good sphericity and good particle size monodispersity.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The preparation method of the ionic liquid surface-coated inorganic pigment electrophoretic particle is characterized by comprising the following steps of:
s1, mixing methanol with alkyl bromide, adding 1-vinyl imidazole, heating the mixed solution to 40-80 ℃, and reacting for 12-48 hours under the conditions of stirring and refluxing to obtain vinyl alkyl imidazole bromide ionic liquid;
s2, adding inorganic pigment particles with the particle size range of 150-400nm into water, adding 1-vinyltriethoxysilane, performing ultrasonic dispersion for 15min, heating the mixed solution to 40-90 ℃, reacting for 12-48h under the condition of stirring, washing the product for 3 times with water and absolute ethyl alcohol, and performing vacuum drying on the product at 40-80 ℃ for 6-24h to obtain surface vinyl modified inorganic pigment particles;
s3, distilling the vinyl alkyl imidazole bromide ionic liquid under reduced pressure, adding the ionic liquid, the surface vinyl modified inorganic pigment particles and divinylbenzene into water, ultrasonically dispersing for 15min, heating the solution to 70 ℃, adding potassium persulfate, continuing to react for 2-24h, washing the product for 3 times with water and absolute ethyl alcohol, and then drying the product in vacuum at 40-80 ℃ for 6-24h to obtain the ionic liquid surface-coated inorganic pigment electrophoretic particles.
2. The method of claim 1, wherein the alkyl group of the bromoalkyl hydrocarbon of step S1 is one or more of propyl, hexyl, octyl, dodecyl, or hexadecyl.
3. The method of claim 1, wherein the inorganic pigment particles of step S2 are selected from titanium dioxide white particles, silicon dioxide white particles, iron oxide red particles, and cobalt titanate blue particles.
4. The method for preparing the ionic liquid surface-coated inorganic pigment electrophoretic particle as claimed in claim 1, wherein the mass amount of the alkyl bromide in the step S1 is 0.1-1.5 times of the mass amount of the methanol, and 1-vinylimidazole is further added, wherein the mass amount of the 1-vinylimidazole is 0.1-1.0 times of the mass amount of the methanol.
5. The method for preparing the ionic liquid surface-coated inorganic pigment electrophoretic particles as claimed in claim 1, wherein the 1-vinyltriethoxysilane accounts for 0.1-10% by weight of the inorganic pigment particles in the step S2.
6. The method for preparing the ionic liquid surface-coated inorganic pigment electrophoretic particles as claimed in claim 1, wherein the mass amount of the vinyl alkyl imidazole bromide ionic liquid in the step S3 is 1% -15% of the surface vinyl modified inorganic pigment particles, and the mass amount of the divinylbenzene is 5% -40% of the surface vinyl modified inorganic pigment particles.
7. The method for preparing ionic liquid surface-coated inorganic pigment electrophoretic particles according to claim 1, wherein the amount of the potassium persulfate in the step S3 is 5 to 20% by mass based on the surface vinyl modified inorganic pigment particles.
8. The ionic liquid surface-coated inorganic pigment electrophoretic particle prepared by the preparation method of claim 1, which consists of a core and a shell layer, wherein the core is the inorganic pigment electrophoretic particle, the shell layer is an ionic liquid polymer and is coated on the surface of the core, and the particle size of the inorganic pigment electrophoretic particle is 200-450 nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196235A (en) * | 2021-12-17 | 2022-03-18 | 深圳秋田微电子股份有限公司 | Electrophoretic particle and preparation method and application thereof |
| CN116589871A (en) * | 2023-04-23 | 2023-08-15 | 电子科技大学中山学院 | Preparation method of core-shell structure electrophoretic particles based on ionic liquid modification |
-
2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196235A (en) * | 2021-12-17 | 2022-03-18 | 深圳秋田微电子股份有限公司 | Electrophoretic particle and preparation method and application thereof |
| CN116589871A (en) * | 2023-04-23 | 2023-08-15 | 电子科技大学中山学院 | Preparation method of core-shell structure electrophoretic particles based on ionic liquid modification |
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