CN103336413B - A kind of color toner and preparation method thereof - Google Patents
A kind of color toner and preparation method thereof Download PDFInfo
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- CN103336413B CN103336413B CN201310263125.9A CN201310263125A CN103336413B CN 103336413 B CN103336413 B CN 103336413B CN 201310263125 A CN201310263125 A CN 201310263125A CN 103336413 B CN103336413 B CN 103336413B
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Abstract
The invention discloses a kind of color toner, by weight, comprise following component: styrene 60 ~ 80 parts; Butyl acrylate 15 ~ 25 parts; Complex wax 3 ~ 7 parts; Pigment 3 ~ 6 parts; Charge adjusting agent 0.2 ~ 1.5 part; Ammonium persulfate 1 ~ 2 part; Molecular weight regulator 0.1 ~ 2 part; 1.0 ~ 3.0 parts, surfactant; Silica 1 ~ 4 part; Described complex wax comprises two or more of Brazil wax, polypropylene wax or C80 paraffin; The present invention, by adding complex wax at emulsion preparatory phase, compared with the use of single wax, suitably can reduce polymerization speed, its toughness and printing durability are improved; The use of complex wax in addition, can reduce costs, and make the emulsibility of the color toner made better, glossiness is better, and hardness is better, and stability is better; And narrow diameter distribution, mean grain size D
50be 5 ~ 8 μm, particle diameter is easily controlled.
Description
Technical field
The present invention relates to electrophotographic image forming technical applications, be specifically related to the color toner and preparation method thereof of a kind of duplicating machine, printer.
Background technology
Color toner be color laser printing, colored digital duplicate needed for crucial consumptive material, primarily of compositions such as resin, pigment, adjuvants.Along with infotech, network technology and office automation and modern development, and laser printer, laser digital duplicating machine, digital camera universal, and to the future development of digitizing, colorize, the demand for color toner is increasing, and quality requirements is also more and more higher.
At present, the preparation method of color toner mainly contains two classes: Physical and chemical polymerization.Physical, also " fusion method " is claimed, be that resin (being mainly Styrene And Butyl-acrylate multipolymer), colorant (pigment or dyestuff), adjuvant (charge adjusting agent, mould release etc.) are passed through and add the operations such as hot milling, compressing tablet, mechanical crushing, sizing screening conforming particle, obtain the color toner that granularity is about 10um.But, it is not easily dispersed in resin that this preparation method also exists toner, the color toner grain size of preparation and the defect such as shape homogeneity is poor, particle diameter is larger, cause printing, easy roll banding, resolution are low when duplicating, shade deviation, useless powder rate are higher, and in process of production, need to carry out classification process, technics comparing is complicated, and production cost is higher.Chemical polymerization is prepared color toner and is mainly comprised suspension polymerization and emulsion polymerization; Wherein, suspension polymerization can control the size of toner particle effectively, makes the flowing property of toner, charging performance significantly improves, can improve the fixing stability of color toner, consolidation performance, effectively suppresses print through phenomenon.But the weak point of " suspension polymerization " is color toner broad particle distribution makes printing, duplicate resolution and color and luster not good enough, color toner particle too circle causes the recovery of the color toner remained on photoreceptor with clean very difficult.At present, the maximum chemical polymerization of domestic and international employing is emulsion polymerization, powder granularity can be made little of 5 μm by the adjustment of surfactant, shear rate, its Size Distribution narrows, effectively can control the shape of powder, thus the resolution of raising colour print, duplicating and color and luster, the number of other, non-spherical shapes ink powder be conducive on photoreceptor of toner particles reclaims with clean.Zhou Xueliang, Zhang Weigang, Zhou Dongliang etc. adopt emulsion polymerization in situ to prepare printer, used in copy machines color toner, by choosing the raw materials such as styrene, butyl acrylate, vibrin, polypropylene wax, AZO pigments, charge adjusting agent, azo-bis-isobutyl cyanide, surfactant and silicon dioxide, through the color toner that the steps such as reaction, separation, cleaning, drying and modification are made; But little with report about the document of the research of wax in emulsion polymerization, particularly complex wax just it be blended in wherein equably at emulsion preparatory phase, thus improve the printing durability of color toner, the quality finally improving color toner rarely has report.
Summary of the invention
Primary and foremost purpose of the present invention aims to provide a kind of color toner that suitably can reduce polymerization speed, raising toughness and printing durability, reduce costs.
Another object of the present invention is the preparation method providing above-mentioned color toner.
The present invention is achieved by the following technical solution:
A kind of color toner, by weight, comprises following component:
Styrene 60 ~ 80 parts;
Butyl acrylate 15 ~ 25 parts;
Complex wax 3 ~ 7 parts;
Pigment 3 ~ 6 parts;
Charge adjusting agent 0.2 ~ 1.5 part;
Ammonium persulfate 1 ~ 2 part;
Molecular weight regulator 0.1 ~ 2 part;
1.0 ~ 3.0 parts, surfactant;
Silica 1 ~ 4 part;
Described complex wax comprises two or more of Brazil wax, polypropylene wax or C80 paraffin.
Add complex wax, compared with the use of single wax, suitably can reduce polymerization speed, thus material is more easily processed, its toughness and printing durability are improved; The use of complex wax in addition, can reduce costs, and make the emulsibility of the color toner made better, glossiness is better, and hardness is better, and stability is better.
The composite weight ratio of described complex wax is 1:2 ~ 1:5; When composite weight ratio is less than 1:2, do not have the effect improving its toughness and printing durability.
The composite weight ratio of described complex wax is preferably 1:3 ~ 1:4, under this compound proportion, can maximize reduction polymerization speed, improve its toughness and printing durability, make the emulsibility of the color toner made better, glossiness is better, hardness is better, and stability is better.
Described pigment be selected from black pigment, yellow uitramarine, blue pigment, red pigment one or more.
A preparation method for color toner, comprises the steps:
A) taken styrene according to the above ratio, butyl acrylate, complex wax, pigment, charge adjusting agent, ammonium persulfate, molecular weight regulator joined in reactor, start stirrer to stir, speed of agitator is adjusted to 5 ~ 15Hz, and the dispersed with stirring time is 0.5 ~ 1h, stirs; After join in the reactor that surfactant and deionized water are housed, continue dispersed with stirring, speed of agitator is adjusted to 15 ~ 25Hz, and the dispersed with stirring time is 0.5 ~ 1h, stirs; Then be adjusted to 25 ~ 35Hz at speed of agitator, temperature of reaction is react at 75 ~ 95 DEG C, and the reaction time is 1.5 ~ 3.5h, and temperature retention time is 1.5 ~ 3h; Be cooled to normal temperature, obtain compound;
B) carry out breakdown of emulsion, separation with methyl alcohol to the compound obtained, make compound form liquid-solid two phase, removing liquid phase, obtains the material of the solid particle containing torispherical;
C) clean with the material of deionized water to the solid particle containing torispherical, obtain the solid particle of torispherical;
D) at the temperature of 40 ~ 45 DEG C, aim at spheric grain carry out drying process, make its water cut lower than 0.5wt%;
E) add silicon dioxide and carry out Homogeneous phase mixing, modification being carried out to dried torispherical particle, obtains mean grain size (D
50) be the color toner of 5 ~ 8 μm.
Wherein wherein speed of agitator 5 ~ 15Hz, 15 ~ 25Hz and 25 ~ 35Hz are frequency converter frequency value to speed of agitator.
Compared with prior art, beneficial effect is as follows in the present invention:
1) the present invention is by adding complex wax at emulsion preparatory phase, compared with the use of single wax, suitably can reduce polymerization speed, thus material is more easily processed, its toughness and printing durability are improved; The use of complex wax in addition, can reduce costs, and make the emulsibility of the color toner made better, glossiness is better, and hardness is better, and stability is better;
2) the color toner uniform particles for preparing of the present invention, in torispherical, color toner circularity >0.93, softening point temperature is 105 ~ 120 DEG C, and narrow diameter distribution, mean grain size D
50be 5 ~ 8 μm, particle diameter is easily controlled;
3) in production run of the present invention without classification, compared with traditional handicraft, can production run be simplified, Reaction time shorten, reduce production cost.
Embodiment
Further illustrate the present invention below by embodiment, following examples are the present invention's preferably embodiment, but embodiments of the present invention are not by the restriction of following embodiment.
Now following explanation is done to embodiment and comparative example starting material used, but is not limited to these materials:
Black pigment used is import pigment black R330R, and yellow uitramarine forever consolidates transparent yellow PY83, and blue pigment is phthalocyanine blue PB15:3, and red pigment forever consolidates bright red PR170.
Surfactant used is the CO-436 surfactant that production base, French Rhodia Wuxi produces;
Described molecular weight regulator is the lauryl mercaptan of Guangzhou San Wang chemical material company limited;
Charge adjusting agent used is the DL-N28 metal complex that Long-Ting of Hubei Chemical Co produces;
Silicon dioxide used is the R972 hydrophobic silica that German goldschmidt chemical corporation is produced.
Take styrene by the formula rate in table 1, butyl acrylate, complex wax, pigment, charge adjusting agent, ammonium persulfate, molecular weight regulator join in reactor, start stirrer to stir, speed of agitator is adjusted to 5 ~ 15Hz, and the dispersed with stirring time is 0.5 ~ 1h, stirs; After join in the reactor that surfactant and deionized water are housed, continue dispersed with stirring, speed of agitator is adjusted to 15 ~ 25Hz, and the dispersed with stirring time is 0.5 ~ 1h, stirs; Then be adjusted to 25 ~ 35Hz at speed of agitator, temperature of reaction is react at 75 ~ 95 DEG C, and the reaction time is 1.5 ~ 3.5h, and temperature retention time is 1.5 ~ 3h; Be cooled to normal temperature, obtain compound; Carry out breakdown of emulsion, separation with methyl alcohol to it, make compound form liquid-solid two phase, removing liquid phase, obtains the material of the solid particle containing torispherical; Clean with the material of deionized water to the solid particle containing torispherical again, obtain the solid particle of torispherical; At the temperature of 40 ~ 45 DEG C, aim at spherical solid particle carry out drying process, make its water cut lower than 0.5wt%; Finally, add silicon dioxide and carry out Homogeneous phase mixing, modification being carried out to the solid particle of dried torispherical, obtains mean grain size D
50it is the color toner of 5 ~ 8 μm.
The concrete proportioning (weight portion) of each composition and test performance result thereof in table 1 embodiment 1 ~ 8 and comparative example 1 ~ 3
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Styrene | 60 | 65 | 72 | 75 | 80 | 68 | 70 | 78 | 60 | 72 | 80 |
| Butyl acrylate | 15 | 20 | 22 | 18 | 25 | 24 | 21 | 19 | 15 | 22 | 25 |
| Brazil wax | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | / | / | 10 |
| Polypropylene wax | 2 | / | 1 | 3 | 1.5 | 1 | 2 | / | / | 6 | / |
| C80 paraffin | / | 2 | 1 | 0.5 | 3 | 2 | 3 | 3 | / | / | |
| Pigment | 3 | 5 | 6 | 4 | 3 | 3 | 5 | 4 | 3 | 6 | 3 |
| DL-N28 metal complex | 0.5 | 1 | 1.5 | 0.2 | 1 | 1 | 1 | 1 | 0.5 | 1.5 | 1 |
| Ammonium persulfate | 1 | 1.5 | 1.5 | 2 | 1.5 | 1.5 | 1.5 | 1.5 | 1 | 1.5 | 1.5 |
| CO-436 surfactant | 3 | 1.5 | 2 | 1 | 2.5 | 2 | 2 | 1 | 3 | 2 | 2.5 |
| Silicon dioxide | 2 | 3 | 4 | 1 | 2 | 4 | 1 | 2 | 2 | 4 | 2 |
| Particle diameter/μm (D 50） | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~9 | 3~9 |
| Circularity | 0.96 | 0.95 | 0.95 | 0.97 | 0.95 | 0.97 | 0.96 | 0.96 | 0.92 | 0.93 | 0.90 |
| Softening point temperature/DEG C | 119.4 | 112.6 | 114.1 | 121.8 | 113.5 | 108.5 | 114.0 | 121.2 | 119.8 | 113.7 | 113.2 |
Properties method of testing:
Mean grain size (D
50): toner particle diameter and distribution thereof adopt Beckman Ku Erte LS13320 series laser particle-size analyzer to measure;
Circularity: the circularity of toner particles adopts the American-European gram figure instrument in Zhuhai to measure;
Softening point temperature: the thermal deformation vicat softening point temperature analyzer adopting the Kunlun, Dongguan.
As can be seen from embodiment and the comparative example of upper table 1, the present invention, by adding complex wax at emulsion preparatory phase, compared with the use of single wax, suitably can reduce polymerization speed, its toughness and printing durability are improved; The use of complex wax in addition, can reduce costs, and make the emulsibility of the color toner made better, glossiness is better, and hardness is better, and stability is better; Uniform particles, in torispherical, color toner circularity >0.93, softening point temperature is 105 ~ 125 DEG C, and narrow diameter distribution, mean grain size D
50be 5 ~ 8 μm, particle diameter is easily controlled.
Claims (3)
1. a color toner, is characterized in that: by weight, comprises following component:
Styrene 60 ~ 80 parts;
Butyl acrylate 15 ~ 25 parts;
Complex wax 3 ~ 7 parts;
Pigment 3 ~ 6 parts;
Charge adjusting agent 0.2 ~ 1.5 part;
Ammonium persulfate 1 ~ 2 part;
Molecular weight regulator 0.1 ~ 2 part;
1.0 ~ 3.0 parts, surfactant;
Silica 1 ~ 4 part;
Described complex wax comprises two or more of Brazil wax, polypropylene wax or C80 paraffin; The composite weight ratio of described complex wax is 1:2 ~ 1:5;
Its preparation method, comprises the steps:
A) taken styrene according to the above ratio, butyl acrylate, complex wax, pigment, charge adjusting agent, ammonium persulfate, molecular weight regulator joined in reactor, start stirrer to stir, speed of agitator is adjusted to 5 ~ 15Hz, and the dispersed with stirring time is 0.5 ~ 1h, stirs; After join in the reactor that surfactant and deionized water are housed, continue dispersed with stirring, speed of agitator is adjusted to 15 ~ 25Hz, and the dispersed with stirring time is 0.5 ~ 1h, stirs; Then be adjusted to 25 ~ 35Hz at speed of agitator, temperature of reaction is react at 75 ~ 95 DEG C, and the reaction time is 1.5 ~ 3.5h, and temperature retention time is 1.5 ~ 3h; Be cooled to normal temperature, obtain compound;
B) carry out breakdown of emulsion, separation with methyl alcohol to the compound obtained, make compound form liquid-solid two phase, removing liquid phase, obtains the material of the solid particle containing torispherical;
C) clean with the material of deionized water to the solid particle containing torispherical, obtain the solid particle of torispherical;
D) at the temperature of 40 ~ 45 DEG C, aim at spheric grain carry out drying process, make its water cut lower than 0.5wt%;
E) add silicon dioxide and carry out Homogeneous phase mixing, modification being carried out to dried torispherical particle, obtains mean grain size D
50it is the color toner of 5 ~ 8 μm.
2. color toner according to claim 1, is characterized in that, the composite weight ratio of described complex wax is preferably 1:3 ~ 1:4.
3. color toner according to claim 1, is characterized in that, described pigment be selected from black pigment, yellow uitramarine, blue pigment, red pigment one or more.
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| CN103336413B true CN103336413B (en) | 2016-01-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103543622B (en) * | 2013-10-24 | 2016-04-20 | 南京理工大学 | A kind of adopt mini-emulsion polymerization to prepare color toner and method |
| CN107329381A (en) * | 2017-08-29 | 2017-11-07 | 邯郸汉光办公自动化耗材有限公司 | Color toner and preparation method thereof and the method for digital thermal transfer printing |
Citations (5)
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| CN101059665A (en) * | 2006-04-20 | 2007-10-24 | 京瓷美达株式会社 | Toner, selecting method thereof and image forming device using the same |
| CN101077967A (en) * | 2006-03-01 | 2007-11-28 | 信越化学工业株式会社 | Epoxy resin composition for enveloping semiconductor and semiconductor device |
| CN101702080A (en) * | 2009-10-30 | 2010-05-05 | 无锡佳腾磁性粉有限公司 | Method for preparing color toner by in-situ emulsion polymerization method |
| CN102303459A (en) * | 2011-07-26 | 2012-01-04 | 大连富士山办公设备有限公司 | High-resolution thermal transfer colored tape |
| CN103257538A (en) * | 2013-05-20 | 2013-08-21 | 金发科技股份有限公司 | Color toner and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080286677A1 (en) * | 2006-11-30 | 2008-11-20 | Kyocera Mita Corporation | Toner for developer |
| KR20130012770A (en) * | 2011-07-26 | 2013-02-05 | 주식회사 엘지화학 | Polymerized toner and preparation method of the same |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077967A (en) * | 2006-03-01 | 2007-11-28 | 信越化学工业株式会社 | Epoxy resin composition for enveloping semiconductor and semiconductor device |
| CN101059665A (en) * | 2006-04-20 | 2007-10-24 | 京瓷美达株式会社 | Toner, selecting method thereof and image forming device using the same |
| CN101702080A (en) * | 2009-10-30 | 2010-05-05 | 无锡佳腾磁性粉有限公司 | Method for preparing color toner by in-situ emulsion polymerization method |
| CN102303459A (en) * | 2011-07-26 | 2012-01-04 | 大连富士山办公设备有限公司 | High-resolution thermal transfer colored tape |
| CN103257538A (en) * | 2013-05-20 | 2013-08-21 | 金发科技股份有限公司 | Color toner and preparation method thereof |
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