CN101210120B - Hollow titanium dioxide white electrophoresis ion for electrophoresis displaying and preparing method thereof - Google Patents
Hollow titanium dioxide white electrophoresis ion for electrophoresis displaying and preparing method thereof Download PDFInfo
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- CN101210120B CN101210120B CN2007100601573A CN200710060157A CN101210120B CN 101210120 B CN101210120 B CN 101210120B CN 2007100601573 A CN2007100601573 A CN 2007100601573A CN 200710060157 A CN200710060157 A CN 200710060157A CN 101210120 B CN101210120 B CN 101210120B
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Abstract
The invention provides a preparation method for white hollow titanic oxide microsphere. Hollow microsphere of a crylic acid polymer or of a styrene polymer is taken as a seed and an outer layer of the hollow microsphere is wrapped with titanyl hydrate; after being dried, the seed wrapped with titanyl hydrate is baked at the high temperature so as to prepare the titanic oxide microsphere with hollow structure. The white oxide has the spherical diameter of 40 nanometers to 450 nanometers, relative density of 1.0 to 3.1g/cm<3> and specific surface of 40 to 95m<2>/g. The titanic oxide microsphereprepared by the invention has a regular shape, a glabrous surface and an even size and diameter of particles is easily controlled. The invention also has the advantages that the preparation process of the method is simple and the raw materials are easily obtained.
Description
Technical field
The present invention relates to the technology of electrophoresis particle, particularly a kind of hollow titanium dioxide white electrophoresis particle that is used for electrophoresis showed and preparation method thereof is applied to the preparation of the white hollow electrophoresis particle in the microcapsule electrophoresis display electronic paper.
Technical background
The microcapsule electrophoresis showed is the main direction of present Electronic Paper research, it adopts microcapsule to coat the electrophoresis disclosing solution of being made up of electrophoresis particle, suspension, charge control agent and stablizer etc., utilizes electrophoresis particle shown by electric field action generation electrophoretic migration.The traditional method of preparation titanium dioxide electrophoresis particle is that pigment particles is carried out surface modification with tensio-active agent (anion surfactant, cats product or nonionogenic tenside), is prepared into the pigment particles with lipophilic surface.But can not improve the original surface topography of particle, size distribution and particle surface roughness via the electrophoresis particle that this method surface modification makes, can not effectively reduce the relative density of particle, the density difference of electrophoresis particle and dispersion medium is bigger, must select the high-density dispersion medium and make that the selectable range of dispersion medium is narrow, make the electrophoresis dispersion poor stability of preparation, cause electronic paper display device time of response of preparing long, picture contrast is poor, and work-ing life is short.
Summary of the invention
The object of the present invention is to provide a kind of white hollow electrophoresis particle that is used for the Electronic Paper demonstration and preparation method thereof, as the spheroidal particle of rule, be prepared into the relative density that hollow-particle effectively reduces particle, thereby can overcome the defective of the electrophoresis particle of traditional method preparation.The present invention prepares the spherical particle of hollow structure titanium dioxide, has improved the apparent pattern and the optical property of TiO 2 particles, has reduced density.This method preparation process is simple, and sphere, any surface finish, size that prepared electrophoresis particle is shaped as rule are even, and the hollow structure of particle makes that its density is lower, has the dispersion agent selectable range of broad.
The invention provides a kind of hollow titanium dioxide white electrophoresis particle that is used for electrophoresis showed, its particle diameter is 40～450nm, and relative density is 1.0～3.1g/cm
3, specific surface is 40～95m
2/ g; It is to be raw material with olefinic organic hydrocarbon polymer [for example: the kind of (methyl) acrylic polymer comprises (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate and (methyl) Octyl acrylate etc.)] hollow microsphere and titanic acid ester, according to olefinic organic hydrocarbon polymer microballoon and titanic acid ester ratio is to prepare burden in 1: 12～1: 96, its preparation method is to be seed with olefinic organic hydrocarbon polymer hollow microsphere, the outer titanyl hydrate that coats, drying, roasting is prepared from.
The invention provides a kind of preparation method who is used for the hollow titanium dioxide white electrophoresis particle of electrophoresis showed comprises the steps:
1) the polymeric hollow microsphere particle is scattered in the dehydrated alcohol, adds titanic acid ester and less water, 10～80 ℃ down behind the reaction 30min, in 30～100 ℃ down oven dry obtain white spheric hollow polymer/titanium dioxide complex particle.
2) with spherical hollow polymer/titanium dioxide complex particle in air atmosphere, in 100～1800 ℃ (being preferably in 600～1200 ℃) down roasting 3～5 hours, obtain the white hollow titanium dioxide microballoon sphere.
Said hollow polymer is an acrylic polymer, and the monomer of said acrylic polymer is methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate and Octyl methacrylate.
White hollow titanium dioxide microballoon sphere that is used for electrophoresis showed provided by the invention and preparation method thereof can overcome the defective of traditional method.The present invention with the polymer spherical particle as carrier make the spherical particle shape rule of the hollow titanium dioxide prepare, any surface finish, size evenly and particle diameter be easy to control, hollow structure makes the shell of TiO 2 particles have different refraction coefficients with hollow parts simultaneously, light scattering efficiency is higher than the solid particle suitable with its density, have good light scattering property, and density is lower.The present invention be advantageous in that this method preparation process is simple, raw material is easy to get.
Description of drawings
Fig. 1 is the result that the white hollow nanometer titanium dioxide micro-sphere that makes is observed under transmission electron microscope.
Embodiment
Example 1
1. methyl methacrylate polymeric hollow microsphere 0.10g is scattered in the 95mL dehydrated alcohol, adds 5.10g titanic acid ester and 0.90g deionized water, stirs 30min, leaves standstill and obtains white powder, is spherical hollow polymer/titanium dioxide complex particle.
2. with hollow polymer/titanium dioxide complex particle in air atmosphere, at 1000 ℃ of following roasting 5h, obtain the spherical particle of white hollow titanium dioxide, size is even, is about 180nm, relative density is 1.36g/cm
3
Example 2
1. get Jia Jibingxisuanyizhi polymer hollow particles 0.25g and be scattered in the 95mL dehydrated alcohol, add 2.98g titanic acid ester and 0.16g deionized water, stir 30min, leave standstill and obtain white powder, be spherical hollow polymer/titanium dioxide complex particle.
What 2. will prepare obtains white hollow polymer/titanium dioxide complex particle in air atmosphere, at 900 ℃ of following roasting 5h, obtains the spherical particle of white hollow titanium dioxide, and size is even, is about 320nm, and relative density is 2.04g/cm
3
Example 3
1. get polystyrene hollow microsphere 0.17g and be scattered in the 95mL dehydrated alcohol, add 4.30g titanic acid ester and 0.90g deionized water, stir 30min, leave standstill and obtain white powder, be spherical hollow polymer/titanium dioxide complex particle.
What 3. will prepare obtains white hollow polymer/titanium dioxide complex particle in air atmosphere, at 900 ℃ of following roasting 5h, obtains the spherical particle of white hollow titanium dioxide, and size is even, is about 180nm, and relative density is 1.84g/cm
3
Example 4
1. get Jia Jibingxisuanyizhi polymer microballoon 0.33g and be scattered in the 90mL dehydrated alcohol, add 7.63g titanic acid ester and 1.03g deionized water, stir 30min, leave standstill and obtain white powder, be spherical hollow polymer/titanium dioxide complex particle.
What 2. will prepare obtains white powder polymkeric substance/titanium dioxide complex particle 800 ℃ of following roasting 3h in air atmosphere, obtains the spherical particle of white hollow titanium dioxide, and size is even, is about 245nm, and relative density is 1.78g/cm
3
Example 5
1. get polystyrene hollow microsphere 0.26g and be scattered in the 90mL dehydrated alcohol, add 5.21g titanic acid ester and 1.03g deionized water, stir 30min, leave standstill and obtain white powder, be spherical hollow polymer/titanium dioxide complex particle, particle diameter is even, be about 350nm, relative density is 1.29g/cm
3
What 2. will prepare obtains white hollow polymer/titanium dioxide complex particle in air atmosphere, at 700 ℃ of following roasting 3h, obtains the spherical particle of white hollow titanium dioxide, and size is even, is about 205nm, and relative density is 1.64g/cm
3
Example 6
1. get polystyrene hollow microsphere 0.20g and be scattered in the 90mL dehydrated alcohol, add 7.20g titanic acid ester and 1.03g deionized water, stir 30min, leave standstill and obtain white powder, be spherical hollow polymer/titanium dioxide complex particle.
White hollow polymer/the titanium dioxide complex particle that 2. will prepare at 600 ℃ of following roasting 3h, obtains the spherical particle of white hollow titanium dioxide in air atmosphere, size is even, is about 205nm, and relative density is 1.64g/cm
3
Claims (1)
1. preparation method who is used for the hollow titanium dioxide white electrophoresis particle of electrophoresis showed, its particle diameter is 40～450nm, relative density is 1.0～3.1g/cm
3, specific surface is 40～95m
2/ g; It is to be seed with the polymer hollow particles, the outer titanyl hydrate that coats, and drying, roasting is prepared from, and it is characterized in that it comprises the steps:
1) the polymeric hollow microsphere particle is scattered in the dehydrated alcohol, adds titanic acid ester and less water, 10～80 ℃ down behind the reaction 30min, in 30～100 ℃ down oven dry obtain white spheric hollow polymer/titanium dioxide complex particle;
2) with spherical hollow polymer/titanium dioxide complex particle in air atmosphere, 600～1200 ℃ of following roastings 3～5 hours, obtain the white hollow titanium dioxide microballoon sphere;
Said polymer hollow particles and titanic acid ester mass ratio are 1: 12-1: 96;
Said hollow polymer is acrylic polymer or polystyrene; The monomer of said acrylic polymer is methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate or Octyl methacrylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100601573A CN101210120B (en) | 2007-12-25 | 2007-12-25 | Hollow titanium dioxide white electrophoresis ion for electrophoresis displaying and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100601573A CN101210120B (en) | 2007-12-25 | 2007-12-25 | Hollow titanium dioxide white electrophoresis ion for electrophoresis displaying and preparing method thereof |
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| Publication Number | Publication Date |
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| CN101210120A CN101210120A (en) | 2008-07-02 |
| CN101210120B true CN101210120B (en) | 2011-08-10 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI395714B (en) * | 2009-09-16 | 2013-05-11 | Univ Nat Chunghsing | Inorganic hollow microspheres and its preparation method |
| US9993397B2 (en) | 2010-11-23 | 2018-06-12 | Conopco Inc. | Composite particles and compositions with composite particles |
| CN102174276B (en) * | 2011-03-09 | 2013-03-20 | 东南大学 | Method for preparing cerium-doped hollow nano titanium dioxide yellow pigment for electronic paper |
| CN102502807A (en) * | 2011-10-27 | 2012-06-20 | 天津大学 | White hollow titanium dioxide microsphere and preparation method thereof |
| CN103760731B (en) * | 2013-12-19 | 2017-02-08 | 北京京东方光电科技有限公司 | Electronic ink, electronic paper and method for preparing electronic ink |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772363A (en) * | 2004-11-11 | 2006-05-17 | 中国科学院化学研究所 | Template process of preparing hollow ball and composite hollow ball |
| CN1803938A (en) * | 2005-01-10 | 2006-07-19 | 北京化工大学 | TiO2/CaCO3 nano composite particle, hollow TiO2 nano material and method for preparing the same |
-
2007
- 2007-12-25 CN CN2007100601573A patent/CN101210120B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772363A (en) * | 2004-11-11 | 2006-05-17 | 中国科学院化学研究所 | Template process of preparing hollow ball and composite hollow ball |
| CN1803938A (en) * | 2005-01-10 | 2006-07-19 | 北京化工大学 | TiO2/CaCO3 nano composite particle, hollow TiO2 nano material and method for preparing the same |
Non-Patent Citations (5)
| Title |
|---|
| Arnout Imhof.Preparation and Characterization of Titania-Coated Polystyrene Spheres and Hollow Titania Shells.Langmuir 2001, 17, 3579-358517 12.2001,17(12),3579-3584. |
| Arnout Imhof.Preparation and Characterization of Titania-Coated Polystyrene Spheres and Hollow Titania Shells.Langmuir 2001, 17, 3579-358517 12.2001,17(12),3579-3584. * |
| 卢海强.模板法制备无机中空纤维和无机中空微球.南京工业大学学位论文.2006,55-56. * |
| 徐志兵,魏先文.TiO2空心微球的制备及其表征.电子显微学报25 3.2006,25(3),226-230. |
| 徐志兵,魏先文.TiO2空心微球的制备及其表征.电子显微学报25 3.2006,25(3),226-230. * |
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