CN100564428C - The electrophoresis particle preparation method of composite structure who is used for the core-pigment layer-shell of electric ink - Google Patents
The electrophoresis particle preparation method of composite structure who is used for the core-pigment layer-shell of electric ink Download PDFInfo
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- CN100564428C CN100564428C CNB2007101509447A CN200710150944A CN100564428C CN 100564428 C CN100564428 C CN 100564428C CN B2007101509447 A CNB2007101509447 A CN B2007101509447A CN 200710150944 A CN200710150944 A CN 200710150944A CN 100564428 C CN100564428 C CN 100564428C
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Abstract
The invention discloses a kind of electrophoresis particle preparation method of composite structure of the core-pigment layer-shell that is used for electric ink, belong to the electrophoresis particle technology of preparing.This procedure comprises: at first will be mixed with emulsion in wax and the tensio-active agent adding deionized water; To make colour particles in two kinds of inorganic salt solutions adding emulsions; Then colour particles is dispersed in adding tetraethyl silicate in back in the ethanol, makes the colour particles surface coat and go up silicon-dioxide, making nuclear is wax, and the middle layer is a pigment, and shell is the electrophoresis particle of the composite structure of silicon-dioxide.Perhaps colour particles is dispersed in the deionized water, adds gum arabic and gelatin and be coated on the colour particles surface, make nuclear and be wax, the middle layer is a pigment, and shell is the electrophoresis particle of the composite structure of gelatin.The invention has the advantages that technology is simple, raw material is easy to get.The electrophoresis particle particle diameter of the composite structure of prepared core-pigment layer-shell is even, the good dispersity in electric ink.
Description
Technical field
The present invention relates to a kind of electrophoresis particle preparation method of composite structure of the core-pigment layer-shell that is used for electric ink, belong to the electrophoresis particle technology of preparing.
Background technology
Electric ink is a kind of basic material that is applied to electrophoresis showed, and it is made up of charged particle and dispersion medium.The preparation of color electrophoresis particle in the past is that pigment, charge control agent, stablizer etc. are dispersed in the medium, by physical method such as polishing, ball milled and supersonic method preparation.It is wide that but the color electrophoresis particle diameter of this method preparation distributes, and the bigger and medium of the density of out-of-shape, particularly inorganic pigment particles does not match, thereby influence the display quality of electric ink.
In order to overcome the defective of traditional method, the method that people such as Dong-Guk Yu have invented with the polymer overmold dyestuff prepares color electrophoresis particle [1,2] [Dong-Guk Yu, Jeong Ho An, Jin-Young Bae, et al.Macromolecules, 2005,38,7485-7491.Dong-Guk Yu, Jeong Ho An, Jin-Young Bae, et al.Chem.Mater.2004,16 (23); 4693-4698], but the color electrophoresis particle of this method preparation exists dyestuff to separate out phenomenon in electrophoresis liquid, and also there is certain influence in the electric ink display effect.The king waits the method that the people invented dye-coated polymer quietly and prepares color electrophoresis particle [3] [Feng Yaqing, Wang Jing, the Li Xiang height, Xie Jianyu. application number: 200610013549.X, publication number: CN1844200A] though overcome dyestuff separating out in medium, but also exist of light color, the shortcoming that weathering resistance and solvent resistance are not strong.The method that people such as Honeyman have invented the polymer overmold mineral dye prepares color electrophoresis particle [4] [Honeyman C, Moran E, Libing Zhang, Pullen A, Emily P, Houde L, King M, Paolini J, Richard J.ElectropHoretic particles and processes for the production thereof.US6822782.Nov, 2004] though to have overcome the density of inorganic pigment granules bigger, the shortcoming that should not in medium, suspend, this procedure complexity, it is long to expend time in, the polymerizing condition harshness, the coating of polymkeric substance has simultaneously reduced the colourity of pigment, and the solvent resistance of whole particle also descends to some extent.
Summary of the invention
The object of the present invention is to provide a kind of electrophoresis particle preparation method of composite structure of the core-pigment layer-shell that is used for electric ink, this procedure is simple, prepared color electrophoresis particle diameter is even, it is excessive to have overcome existing inorganic pigment particles density, should not with the shortcoming of dispersion liquid coupling.
The present invention is realized by following technical proposals.A kind of electrophoresis particle preparation method of composite structure of the core-pigment layer-shell that is used for electric ink, method one is characterized in that comprising following process:
(1) with montanin wax, Chinese wax, carnauba wax or polyethylene wax and be selected from a kind of tensio-active agent of Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, stearylamine, sodium stearate, stearic acid and OP-10, add by mass ratio 1: 0.02～0.2 that to be mixed with mass concentration in the deionized water be 1～10% suspension, then under 90～100 ℃ of temperature, stir with 500～800r/min and to stir 1～3h with 100～300r/min again behind 0.5～1h and make emulsion;
(2) the prepared emulsion of step (1) is heated to 50～70 ℃ after, be 1: 0.05～0.5 by wax and salt mass ratio, at first in emulsion, add sodium sulfide solution, sodium hydroxide solution, sodium hydrogen carbonate solution or the potassium ferrocyanide solution of 0.04～0.6M; And then add cadmium sulfate solution, copper nitrate solution, ferric chloride Solution, zinc nitrate solution or the copperas solution of 0.04～0.6M, stir 3～5h with the speed of 400～700r/min then, more than ageing 24h, cross that centrifugation, deionization washing, ethanol are washed, 70 ℃ of dryings obtain colour particles.
(3) colour particles that step (2) is prepared is after alcohol is washed, accounting for ethanol by colour particles is that 5～15% mass percent is dispersed in colour particles in the ethanol, under the condition of 20～60 ℃ and 200～300r/min, be 1: 0.5～3 and be that 1: 1～3 volume ratio adds ammoniacal liquor and tetraethyl silicate respectively by the mass ratio of particle and tetraethyl silicate according to tetraethyl silicate and ammoniacal liquor, reaction 1～5h, centrifugation, alcohol is washed after drying and is obtained coating uniformly on colour particles surface the electrophoresis particle of composite structure that fine and close transparent silicon dioxide is used for the core-pigment layer-shell of electric ink.
Method two is characterized in that comprising following process:
(1) with montanin wax, Chinese wax, carnauba wax or polyethylene wax and be selected from a kind of tensio-active agent of Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, stearylamine, sodium stearate, stearic acid and OP-10, add by mass ratio 1: 0.02～0.2 that to be mixed with mass concentration in the deionized water be 1～10% suspension, then under 90～100 ℃ of temperature, stir with 500～800r/min and to stir 1～3h with 100～300r/min again behind 0.5～1h and make emulsion;
(2) the prepared emulsion of step (1) is heated to 50～70 ℃ after, be 1: 0.05～0.5 by wax and salt mass ratio, at first in emulsion, add sodium sulfide solution, sodium hydroxide solution, sodium hydrogen carbonate solution or the potassium ferrocyanide solution of 0.04～0.6M; And then add cadmium sulfate solution, copper nitrate solution, ferric chloride Solution, zinc nitrate solution or the copperas solution of 0.04～0.6M, stir 3～5h with the speed of 400～700r/min then, more than ageing 24h, cross that centrifugation, deionization washing, ethanol are washed, 70 ℃ of dryings obtain colour particles.
(3) colour particles that step (2) is prepared is after alcohol is washed, by the mass ratio of colour particles and deionized water is 0.5～5% colour particles to be dispersed in the deionized water, by gum arabic and colour particles mass ratio is 1: 0.5～2, gum arabic is added in the deionized water, fully stirring 0.5～1h adjusting pH value under 50～80 ℃ condition is 3～6, by gum arabic and gelatin mass ratio is 1: 1～2 will be behind the gelatin wiring solution-forming to add in the deionized water back and continue to stir 30～100min, temperature is reduced to 10～30 ℃, centrifugation, the washing after drying obtains the electrophoresis particle that gelatin and gum arabic evenly are coated on the composite structure of the core-pigment layer-shell that is used for electric ink on the colour particles.
The invention has the advantages that technology is simple, raw material is easy to get.The electrophoresis particle particle diameter of the composite structure of prepared core-pigment layer-shell is even, the pigment electrophoresis particle size distribution that has overcome the physical method preparation is wide, shortcoming in irregular shape, and mineral dye coats organism and had both kept good weathering resistance of mineral dye and solvent resistance, it is excessive simultaneously to have overcome inorganic pigment particles density again, should not with the shortcoming of dispersion liquid coupling, outer silicon-dioxide and the gelatin that has different electric charges that coat again of mineral dye makes its result of use in electric ink better simultaneously.
Embodiment
Example 1
1.0g palm wax, 0.02g Trimethyllaurylammonium bromide are joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, and 200r/min stirred 1h after 800r/min stirred 0.5h, temperature was reduced to 50 ℃ then; Prepare stable emulsion.
Respectively the sodium sulfide solution 10ml of 0.2M and the cadmium sulfate solution 10ml of 0.2M are added wherein, after continuing to stir 3h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained yellow electrophoretic particle 1.5g.
Get the yellow particles 1g of method for preparing, alcohol is washed the back and just was dispersed in the 20ml ethanol before drying, fully stir under 50 ℃ the condition, add 1ml ammoniacal liquor, 1ml tetraethyl silicate, reaction 3h coats the yellow particles surface uniformly and goes up fine and close transparent silicon dioxide.Centrifugation, alcohol are washed, obtain that structure is more firm, the more slick yellow electrophoretic particle 1.2g in surface after the drying respectively.
Example 2
In 1.0g Chinese wax, 0.15g Sodium dodecylbenzene sulfonate 50ml pure water, temperature is elevated to more than 90 ℃, 500r/min stir 0.5h later on again 100r/min stir 1h, temperature is reduced to 70 ℃ then; Prepare stable emulsion.
Respectively the sodium sulfide solution 10ml of 0.25M and the cadmium sulfate solution 10ml of 0.25M are added wherein, after continuing to stir 5h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained yellow electrophoretic particle 1.8g.
Get the yellow particles 1g of method for preparing, particle is dispersed in the 50ml pure water again, fully stir under 70 ℃ the condition, continue to regulate pH=3 behind the stirring 30min after adding the 1g gum arabic, add after getting 1g gelatin wiring solution-forming then, after continuing to stir 30min temperature is reduced to 30 ℃, makes gelatin and gum arabic evenly be coated on the colour particles surface.Obtain respectively after centrifugation, washing, the drying that structure is more firm, the more slick yellow electrophoretic particle 1.3g in surface.
Example 3
1.0g palm wax, 0.1g cetyl trimethylammonium bromide are joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 600r/min stir 0.5h later on again 150r/min stir 1h, temperature is reduced to 70 ℃ then; Prepare stable emulsion.
Respectively the sodium sulfide solution 10ml of 0.3M and the zinc nitrate solution 10ml of 0.3M are added wherein, after continuing to stir 4h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained white electrophoretic particles 1.9g.
Get the white particles 1g of method for preparing, alcohol is washed the back and just was dispersed in the 20ml ethanol before drying, fully stir under 30 ℃ the condition, add 2ml ammoniacal liquor, 0.5ml tetraethyl silicate, reaction 1h coats the white particles surface uniformly and goes up fine and close transparent silicon dioxide.Centrifugation, alcohol are washed, obtain that structure is more firm, the more slick white electrophoretic particles 1.1g in surface after the drying respectively.
Example 4
1.0g Chinese wax, 0.08g Sodium dodecylbenzene sulfonate are joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 700r/min stir 0.5h later on again 200r/min stir 1h, temperature is reduced to 60 ℃ then; Prepare stable emulsion.
Respectively the sodium sulfide solution 10ml of 0.1M and the zinc nitrate solution 10ml of 0.1M are added wherein, after continuing to stir 3h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained white electrophoretic particles 1.2g.
Get the white particles 1g of method for preparing, particle is dispersed in the 50ml pure water again, fully stir under 60 ℃ the condition, continue to regulate pH=4 behind the stirring 30min after adding the 0.5g gum arabic, add after getting 1g gelatin wiring solution-forming then, after continuing to stir 50min temperature is reduced to 20 ℃, makes gelatin and gum arabic evenly be coated on the colour particles surface.Obtain respectively after centrifugation, washing, the drying that structure is more firm, the more slick white electrophoretic particles 1.1g in surface.
Example 5
The stearic acid of 1.0g polyethylene wax, 0.20g sodium stearate and 0.05g is joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, need temperature be elevated to more than 100 ℃ in autoclave in case of necessity.600r/min stir 0.5h later on again 100r/min stir 1h, temperature is reduced to 70 ℃ then; Prepare stable emulsion.
Respectively the sodium sulfide solution 10ml of 0.4M and the copper-bath 10ml of 0.4M are added wherein, after continuing to stir 3h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained black electrophoretic particles 2.0g.
Get the black particles 1g of method for preparing, alcohol is washed the back and just was dispersed in the 20ml ethanol before drying, fully stir under 40 ℃ the condition, add 3ml ammoniacal liquor, 1.5ml tetraethyl silicate, reaction 4h coats the black particles surface uniformly and goes up fine and close transparent silicon dioxide.Centrifugation, alcohol are washed, obtain that structure is more firm, the more slick black electrophoretic particles 1.3g in surface after the drying respectively.
Example 6
The stearylamine of 1.0g palm wax, 0.15g cetyl trimethylammonium bromide and 0.05g is joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 800r/min stir 0.5h later on again 150r/min stir 1h, temperature is reduced to 50 ℃ then; Prepare stable emulsion.
Respectively the sodium sulfide solution 10ml of 0.04M and the copper-bath 10ml of 0.04M are added wherein, after continuing to stir 4h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained black electrophoretic particles 1.1g.
Get the black particles 1g of method for preparing, particle is dispersed in the 50ml pure water again, fully stir under 80 ℃ the condition, continue to regulate pH=3.5 behind the stirring 30min after adding the 2g gum arabic, add after getting 1.5g gelatin wiring solution-forming then, after continuing to stir 80min temperature is reduced to 10 ℃, makes gelatin and gum arabic evenly be coated on the colour particles surface.Obtain respectively after centrifugation, washing, the drying that structure is more firm, the more slick black electrophoretic particles 1.4g in surface.
Example 7
1.0g Chinese wax, 0.06g cetyl trimethylammonium bromide are joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 700r/min stir 0.5h later on again 100r/min stir 1h, temperature is reduced to 50 ℃ then; Prepare stable emulsion.
Respectively the sodium hydroxide solution 10ml of 0.6M and the ferric chloride Solution 10ml of 0.2M are added wherein, after continuing to stir 3h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained red electrophoresis particle 1.5g.
Get the red particles 1g of method for preparing, alcohol is washed the back and just was dispersed in the 20ml ethanol before drying, fully stir under 20 ℃ the condition, add 4ml ammoniacal liquor, 2ml tetraethyl silicate, reaction 5h coats the red particles surface uniformly and goes up fine and close transparent silicon dioxide.Centrifugation, alcohol are washed, obtain that structure is more firm, surface more slick red electrophoresis particle 1.4g after the drying respectively.
Example 8
The stearic acid of 1.0g montanin wax, 0.18g sodium stearate and 0.05g is joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 600r/min stir 0.5h later on again 150r/min stir 1h, temperature is reduced to 70 ℃ then; Prepare stable emulsion.
Respectively the sodium hydroxide solution 10ml of 0.4M and the copper-bath 10ml of 0.2M are added wherein, after continuing to stir 3h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained brown electrophoresis particle 1.6g.
Get the brown particles 1g of method for preparing, particle is dispersed in the 50ml pure water again, fully stir under 50 ℃ the condition, regulate pH=5 after continuing to stir 30min behind the adding 3g gum arabic., add after getting 2g gelatin wiring solution-forming then, after continuing to stir 100min temperature is reduced to 20 ℃, make gelatin and gum arabic evenly be coated on the colour particles surface.Obtain respectively after centrifugation, washing, the drying that structure is more firm, the more slick brown electrophoresis particle 1.6g in surface.
Example 9
The OP-10 of 1.0g montanin wax, 0.08g is joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 700r/min stir 0.5h later on again 100r/min stir 1h, temperature is reduced to 70 ℃ then; Prepare stable emulsion.
Respectively the sodium hydroxide solution 10ml of 0.1M and the copper-bath 10ml of 0.05M are added wherein, after continuing to stir 3h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained brown electrophoresis particle 1.2g.
Get the brown particles 1g of method for preparing, alcohol is washed the back and just was dispersed in the 20ml ethanol before drying, fully stir under 60 ℃ the condition, add 5ml ammoniacal liquor, 3ml tetraethyl silicate, reaction 2h coats the green particles surface uniformly and goes up fine and close transparent silicon dioxide.Centrifugation, alcohol are washed, obtain that structure is more firm, the more slick brown electrophoresis particle 1.6g in surface after the drying respectively.
Example 10
The stearic acid of 1.0g Chinese wax, 0.20g sodium stearate and 0.05g is joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 500r/min stir 0.5h later on again 200r/min stir 1h, temperature is reduced to 60 ℃ then; Prepare stable emulsion.
Respectively the sodium hydrogen carbonate solution 10ml of 0.4M and the Cupric Chloride Solution 10ml of 0.2M are added wherein, after continuing to stir 5h, ageing 24h.Centrifugation, washing, alcohol are washed back 70 ℃ of dryings and are obtained green electrophoresis particle 1.8g.
Get the green particles 1g of method for preparing, particle is dispersed in the 50ml pure water again, fully stir under 70 ℃ the condition, regulate pH=6 after continuing to stir 30min behind the adding 3.5g gum arabic., add after getting 2g gelatin wiring solution-forming then, after continuing to stir 50min temperature is reduced to 30 ℃, make gelatin and gum arabic evenly be coated on the colour particles surface.Obtain respectively after centrifugation, washing, the drying that structure is more firm, the more slick green electrophoresis particle 1.6g in surface.
Example 11
1.0g palm wax, 0.12g cetyl trimethylammonium bromide are joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 600r/min stir 0.5h later on again 150r/min stir 1h, temperature is reduced to 70 ℃ then, prepare stable emulsion.
Respectively K4Fe (CN) the 6 solution 10ml of 0.2M and the FeSO4 solution 10ml of 0.2M are added wherein, after continuing to stir 0.5h, temperature is reduced to 20 ℃, make it separate out white precipitate earlier and be coated on the organic ball surface, behind the 20min, temperature is elevated to 90 ℃, the dilute sulphuric acid that adds 10ml 10% behind the 10min continues to keep temperature and stir 2h uniformly, bubbling air 5min cools the temperature to 70 ℃, adds the KClO3 solution 5ml oxidation 3h of 0.1M.Ageing 24h, centrifugation, washing, alcohol wash back 70 ℃ of dryings and obtain blue electrophoresis particle 1.4g.
Get the blue particles 1g of method for preparing, alcohol is washed the back and just was dispersed in the 20ml ethanol before drying, fully stir under 60 ℃ the condition, add 2ml ammoniacal liquor, 1.5ml tetraethyl silicate, reaction 5h coats the blue particles surface uniformly and goes up fine and close transparent silicon dioxide.Centrifugation, alcohol are washed, obtain that structure is more firm, surface more slick blue electrophoresis particle 1.3g after the drying respectively.
Example 12
1.0g Chinese wax, 0.06g Sodium dodecylbenzene sulfonate are joined in the 50ml pure water, and temperature is elevated to more than 90 ℃, 700r/min stir 0.5h later on again 200r/min stir 1h, temperature is reduced to 70 ℃ then, prepare stable emulsion.
Respectively K4Fe (CN) the 6 solution 10ml of 0.1M and the FeSO4 solution 10ml of 0.1M are added wherein, after continuing to stir 0.5h, temperature is reduced to 20 ℃, make it separate out white precipitate earlier and be coated on the organic ball surface, behind the 20min, temperature is elevated to 90 ℃, the dilute sulphuric acid that adds 10ml 10% behind the 10min continues to keep temperature and stir 2h uniformly, bubbling air 5min cools the temperature to 70 ℃, adds the KClO3 solution 5ml oxidation 3h of 0.05M.Ageing 24h, centrifugation, washing, alcohol wash back 70 ℃ of dryings and obtain blue electrophoresis particle 1.2g.
Get the blue particles 1g of method for preparing, particle is dispersed in the 50ml pure water again, fully stir under 50 ℃ the condition, regulate pH=5 after continuing to stir 30min behind the adding 4g gum arabic., add after getting 2g gelatin wiring solution-forming then, after continuing to stir 60min temperature is reduced to 10 ℃, make gelatin and gum arabic evenly be coated on the colour particles surface.Obtain respectively after centrifugation, washing, the drying that structure is more firm, surface more slick blue electrophoresis particle 1.8g.
Claims (2)
1. the electrophoresis particle preparation method of the composite structure of a core-pigment layer-shell that is used for electric ink is characterized in that comprising following process:
(1) with montanin wax, Chinese wax, carnauba wax or polyethylene wax and be selected from a kind of tensio-active agent of Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, stearylamine, sodium stearate, stearic acid and OP-10, add by mass ratio 1: 0.02～0.2 that to be mixed with mass concentration in the deionized water be 1～10% suspension, then under 90～100 ℃ of temperature, stir to stir with 100～300r/min again after 0.5～1 hour with 500～800r/min and made emulsion in 1～3 hour;
(2) the prepared emulsion of step (1) is heated to 50～70 ℃ after, be 1: 0.05～0.5 by wax and salt mass ratio, at first in emulsion, add sodium sulfide solution, sodium hydroxide solution, sodium hydrogen carbonate solution or the potassium ferrocyanide solution of 0.04～0.6M; And then add cadmium sulfate solution, copper nitrate solution, ferric chloride Solution, zinc nitrate solution or the copperas solution of 0.04～0.6M, stirred 3～5 hours with the speed of 400～700r/min then, through ageing more than 24 hours, cross that centrifugation, deionization washing, ethanol are washed, 70 ℃ of dryings obtain colour particles;
(3) colour particles that step (2) is prepared is after alcohol is washed, accounting for ethanol by colour particles is that 5～15% mass percent is dispersed in colour particles in the ethanol, under the condition of 20～60 ℃ and 200～300r/min, be 1: 0.5～3 and be that 1: 1～3 volume ratio adds ammoniacal liquor and tetraethyl silicate respectively by the mass ratio of particle and tetraethyl silicate according to tetraethyl silicate and ammoniacal liquor, reacted centrifugation 1～5 hour, alcohol is washed after drying and is obtained coating uniformly on colour particles surface the electrophoresis particle of composite structure that fine and close transparent silicon dioxide is used for the core-pigment layer-shell of electric ink.
2. the electrophoresis particle preparation method of the composite structure of a core-pigment layer-shell that is used for electric ink is characterized in that comprising following process:
(1) with montanin wax, Chinese wax, carnauba wax or polyethylene wax and be selected from a kind of tensio-active agent of Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, stearylamine, sodium stearate, stearic acid and OP-10, add by mass ratio 1: 0.02～0.2 that to be mixed with mass concentration in the deionized water be 1～10% suspension, then under 90～100 ℃ of temperature, stir to stir with 100～300r/min again after 0.5～1 hour with 500～800r/min and made emulsion in 1～3 hour;
(2) the prepared emulsion of step (1) is heated to 50～70 ℃ after, be 1: 0.05～0.5 by wax and salt mass ratio, at first in emulsion, add sodium sulfide solution, sodium hydroxide solution, sodium hydrogen carbonate solution or the potassium ferrocyanide solution of 0.04～0.6M; And then add cadmium sulfate solution, copper nitrate solution, ferric chloride Solution, zinc nitrate solution or the copperas solution of 0.04～0.6M, stirred 3～5 hours with the speed of 400～700r/min then, through ageing more than 24 hours, cross that centrifugation, deionization washing, ethanol are washed, 70 ℃ of dryings obtain colour particles;
(3) colour particles that step (2) is prepared is after alcohol is washed, by the mass ratio of colour particles and deionized water is 0.5～5% colour particles to be dispersed in the deionized water, by gum arabic and colour particles mass ratio is 1: 0.5～2, gum arabic is added in the deionized water, fully stirring under 50～80 ℃ condition and regulating the pH value in 0.5～1 hour is 3～6, by gum arabic and gelatin mass ratio is 1: 1～2 will be behind the gelatin wiring solution-forming to add in the deionized water back and continue to stir 30～100 minutes, temperature is reduced to 10～30 ℃, centrifugation, the washing after drying obtains the electrophoresis particle that gelatin and gum arabic evenly are coated on the composite structure of the core-pigment layer-shell that is used for electric ink on the colour particles.
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| CN101833217B (en) * | 2010-04-21 | 2011-09-21 | 天津大学 | Modified yellow electrophoretic particle with shell-core composite structure and preparation method thereof |
| 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 |
| CN103467829B (en) * | 2013-09-25 | 2015-10-28 | 南京天诗新材料科技有限公司 | Wax aqueous dispersion of loaded with nano silicon-dioxide and its production and use |
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| 电泳显示微胶囊的制备和性能. 裴广玲等.物理化学学报，第21卷第4期. 2005 |
| 电泳显示微胶囊的制备和性能. 裴广玲等.物理化学学报，第21卷第4期. 2005 * |
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