CN103336413A - Color toner and preparation method thereof - Google Patents
Color toner and preparation method thereof Download PDFInfo
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- CN103336413A CN103336413A CN2013102631259A CN201310263125A CN103336413A CN 103336413 A CN103336413 A CN 103336413A CN 2013102631259 A CN2013102631259 A CN 2013102631259A CN 201310263125 A CN201310263125 A CN 201310263125A CN 103336413 A CN103336413 A CN 103336413A
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Abstract
The invention discloses color toner which comprises the following components in parts by weight: 60-80 parts of styrene, 15-25 parts of butyl acrylate, 3-7 parts of composite wax, 3-6 parts of pigment, 0.2-1.5 parts of charge regulator, 1-2 parts of ammonium persulfate, 0.1-2 parts of molecular weight regulator, 1.0-3.0 parts of surfactant and 1-4 parts of silicon dioxide, wherein the composite wax comprises two or more of carnauba wax, polypropylene wax or C80 paraffin. According to the invention, the composite wax is added in the emulsion preparation stage, so that the polymerization speed can be properly reduced in comparison with the use of single wax, thus improving the toughness and printing durability; the use of the composite wax can lower the cost and ensure that the prepared color toner has better emulsibility, better gloss, better hardness and better stability; and the color toner is narrow in particle size distribution and has an average particle size D50 of 5-8 mu m, so that the particle size is easy to control.
Description
Technical field
The present invention relates to the electrophotographic image forming technical applications, be specifically related to color toner that a kind of duplicating machine, printer use and preparation method thereof.
Background technology
Color toner is that color laser printing, colored digital duplicate required crucial consumptive material, mainly is made up of resin, pigment, adjuvant etc.Along with infotech, network technology and office automation and development of modernization, and the popularizing of laser printer, laser digital duplicating machine, digital camera, and the direction to digitizing, colorize develops, and increasing for the demand of color toner, quality requirements is also more and more higher.
At present, the preparation method of color toner mainly contains two classes: physics method and chemical polymerization.The physics method, also claim " fusion method ", be that resin (being mainly the styrene-propene butyl acrylate copolymer), colorant (pigment or dyestuff), adjuvant (charge adjusting agent, mould release etc.) process are added operations such as hot milling, compressing tablet, mechanical disintegration, the qualified particle of sizing screening, obtain the color toner of the about 10um of granularity.Yet, this preparation method exists toner and is difficult for evenly disperseing in resin, the color toner grain size of preparation and defective such as the shape homogeneity is poor, particle diameter is bigger, cause printing, easy roll banding when duplicating, resolution are low, shade deviation, useless powder rate are higher, and in process of production, need carry out classification and handle, the technology more complicated, production cost is higher.Chemical polymerization prepares color toner and mainly comprises suspension polymerization and emulsion polymerization; Wherein, suspension polymerization can be controlled the size of toner particle effectively, and the flowing property of toner, charging performance are significantly improved, and can improve the stability of color toner photographic fixing, fixed performance, suppresses the print through phenomenon effectively.Makes printing, duplicating resolution and color and luster not good enough yet the weak point of " suspension polymerization " is the color toner broad particle distribution, color toner particle too circle causes remaining in the recovery of the color toner on the photoreceptor and cleans very difficult.At present, adopting maximum chemical polymerizations both at home and abroad is emulsion polymerization, adjustment by surfactant, shear rate can make powder granularity little of 5 μ m, its Size Distribution narrows down, can control the shape of powder effectively, thereby improve resolution and the color and luster of colour print, duplicating, the ink powder that the non-spherical structure of toner particles is conducive on the photoreceptor reclaims and cleaning.Zhou Xueliang, Zhang Weigang, employing emulsion polymerization in situ such as Zhou Dongliang are prepared printer, used in copy machines color toner, by choosing raw materials such as styrene, butyl acrylate, vibrin, polypropylene wax, AZO pigments, charge adjusting agent, azo-bis-isobutyl cyanide, surfactant and silicon dioxide, the color toner of making through steps such as reaction, separation, cleaning, drying and modification processing; But about the document of the research of wax in emulsion polymerization and report seldom, particularly complex wax just was blended in it wherein equably in the emulsion preparation stage, thus the printing durability of raising color toner, and the quality of 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 can suitably reduce polymerization speed, raising toughness and printing durability, reduce cost.
Another object of the present invention is to provide the preparation method of above-mentioned color toner.
The present invention is achieved by the following technical solution:
A kind of color toner by weight, comprises following component:
60 ~ 80 parts of styrene;
15 ~ 25 parts of butyl acrylates;
3 ~ 7 parts of complex wax;
3 ~ 6 parts of pigment;
0.2 ~ 1.5 part of charge adjusting agent;
1 ~ 2 part of ammonium persulfate;
0.1 ~ 2 part of molecular weight regulator;
1.0 ~ 3.0 parts in surfactant;
Silica 1 ~ 4 part;
Described complex wax comprises two or more of Brazil wax, polypropylene wax or C80 paraffin.
Add complex wax, compare with the use of single wax, can suitably reduce polymerization speed, thereby make the easier processing of material, its toughness and printing durability are improved; The use of complex wax in addition can reduce cost, and the emulsibility of the feasible color toner of making is better, and 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 less than 1:2, do not have the effect that improves 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 the reduction polymerization speed, improve its toughness and printing durability, the emulsibility of the feasible color toner of making is better, and glossiness is better, hardness is better, and stability is better.
Described pigment is selected from one or more of black pigment, yellow uitramarine, blue pigment, red pigment.
A kind of preparation method of color toner comprises the steps:
A) having taken by weighing styrene, butyl acrylate, complex wax, pigment, charge adjusting agent, ammonium persulfate, molecular weight regulator according to the above ratio joins in the reactor, starting stirrer stirs, speed of agitator is adjusted to 5 ~ 15 Hz, and the dispersed with stirring time is 0.5 ~ 1 h, stirs; After join in the reactor that surfactant and deionized water are housed, continue dispersed with stirring, speed of agitator is adjusted to 15 ~ 25 Hz, the dispersed with stirring time is 0.5 ~ 1 h, stirs; Be adjusted to 25 ~ 35 Hz at speed of agitator then, temperature of reaction is 75 ~ 95 ℃ of reactions down, and the reaction time is 1.5 ~ 3.5 h, and temperature retention time is 1.5 ~ 3 h; Be cooled to normal temperature, obtain compound;
B) with methyl alcohol the compound that obtains is carried out breakdown of emulsion, separation, make compound form liquid-solid two-phase, remove liquid phase, obtain containing the material of the solid particle of torispherical;
C) clean with the material of deionized water to the solid particle that contains torispherical, obtain the solid particle of torispherical;
D) under 40 ~ 45 ℃ temperature, aim at spheric grain and carry out the drying processing, make its water cut be lower than 0.5wt%;
E) add silicon dioxide and evenly mixing, dried torispherical particle is carried out modification handle, obtain mean grain size (D
50) be the color toner of 5 ~ 8 μ m.
Wherein wherein speed of agitator 5 ~ 15 Hz, 15 ~ 25 Hz and 25 ~ 35 Hz are the frequency converter frequency value to speed of agitator.
The present invention compared with prior art, beneficial effect is as follows:
1) the present invention compares with the use of single wax by adding complex wax in the emulsion preparation stage, can suitably reduce polymerization speed, thereby make the easier processing of material, and its toughness and printing durability are improved; The use of complex wax in addition can reduce cost, and the emulsibility of the feasible color toner of making is better, and glossiness is better, and hardness is better, and stability is better;
2) the color toner uniform particles for preparing of the present invention is torispherical, the color toner circularity〉0.93, softening point temperature is 105 ~ 120 ℃, and narrow diameter distribution, mean grain size D
50Be 5 ~ 8 μ m, make particle diameter control easily;
3) in the production run of the present invention without classification, compare with traditional handicraft, can simplify production run, shorten the reaction time, reduce production costs.
Embodiment
Further specify the present invention below by embodiment, following examples are preferred implementation of the present invention, but embodiments of the present invention are not subjected to the restriction of following embodiment.
Now embodiment and the used starting material of Comparative Examples are done following explanation, but are not limited to these materials:
Used black pigment is import pigment black R330R, and yellow uitramarine is to consolidate transparent yellow PY83 forever, and blue pigment is phthalocyanine blue PB15:3, and red pigment is to consolidate bright red PR170 forever.
Used surfactant 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;
Used charge adjusting agent is the DL-N28 metal complex that Long-Ting of Hubei Chemical Co produces;
Used silicon dioxide is the R972 hydrophobic silica that German goldschmidt chemical corporation is produced.
Taking by weighing styrene, butyl acrylate, complex wax, pigment, charge adjusting agent, ammonium persulfate, molecular weight regulator by the formula rate in the table 1 joins in the reactor, starting stirrer stirs, speed of agitator is adjusted to 5 ~ 15 Hz, and the dispersed with stirring time is 0.5 ~ 1 h, stirs; After join in the reactor that surfactant and deionized water are housed, continue dispersed with stirring, speed of agitator is adjusted to 15 ~ 25 Hz, the dispersed with stirring time is 0.5 ~ 1 h, stirs; Be adjusted to 25 ~ 35 Hz at speed of agitator then, temperature of reaction is 75 ~ 95 ℃ of reactions down, and the reaction time is 1.5 ~ 3.5 h, and temperature retention time is 1.5 ~ 3 h; Be cooled to normal temperature, obtain compound; With methyl alcohol it is carried out breakdown of emulsion, separation, make compound form liquid-solid two-phase, remove liquid phase, obtain containing the material of the solid particle of torispherical; Clean with the material of deionized water to the solid particle that contains torispherical again, obtain the solid particle of torispherical; Under 40 ~ 45 ℃ temperature, aim at spherical solid particle and carry out the drying processing, make its water cut be lower than 0.5wt%; At last, add silicon dioxide and also evenly mix, the solid particle of dried torispherical is carried out modification handle, obtain mean grain size D
50It is the color toner of 5 ~ 8 μ m.
Each concrete proportioning (weight portion) and test performance result thereof who forms in table 1 embodiment 1 ~ 8 and the Comparative Examples 1 ~ 3
Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 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 |
The 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 |
The 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/μ m(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/℃ | 119.4 | 112.6 | 114.1 | 121.8 | 113.5 | 108.5 | 114.0 | 121.2 | 119.8 | 113.7 | 113.2 |
Every performance test methods:
Mean grain size (D
50): toner particle diameter and the employing Beckman Ku Erte LS 13 320 serial laser particle size analyzers that distribute thereof are measured;
Circularity: the circularity of toner particles adopts Zhuhai American-European gram figure instrument to measure;
Softening point temperature: the thermal deformation vicat softening point temperature analyzer that adopts the Kunlun, Dongguan.
From the embodiment of last table 1 and Comparative Examples as can be seen, the present invention compares with the use of single wax by adding complex wax in the emulsion preparation stage, can suitably reduce polymerization speed, and its toughness and printing durability are improved; The use of complex wax in addition can reduce cost, and the emulsibility of the feasible color toner of making is better, and glossiness is better, and hardness is better, and stability is better; Uniform particles is torispherical, the color toner circularity〉0.93, softening point temperature is 105 ~ 125 ℃, and narrow diameter distribution, mean grain size D
50Be 5 ~ 8 μ m, make particle diameter control easily.
Claims (5)
1. color toner is characterized in that: by weight, comprise following component:
60 ~ 80 parts of styrene;
15 ~ 25 parts of butyl acrylates;
3 ~ 7 parts of complex wax;
3 ~ 6 parts of pigment;
0.2 ~ 1.5 part of charge adjusting agent;
1 ~ 2 part of ammonium persulfate;
0.1 ~ 2 part of molecular weight regulator;
1.0 ~ 3.0 parts in surfactant;
Silica 1 ~ 4 part;
Described complex wax comprises two or more of Brazil wax, polypropylene wax or C80 paraffin.
2. color toner according to claim 1 is characterized in that, the composite weight ratio of described complex wax is 1:2 ~ 1:5.
3. color toner according to claim 2 is characterized in that, the composite weight ratio of described complex wax is preferably 1:3 ~ 1:4.
4. color toner according to claim 1 is characterized in that, described pigment is selected from one or more of black pigment, yellow uitramarine, blue pigment, red pigment.
5. as the preparation method of each described color toner of claim 1 ~ 4, it is characterized in that, comprise the steps:
A) having taken by weighing styrene, butyl acrylate, complex wax, pigment, charge adjusting agent, ammonium persulfate, molecular weight regulator according to the above ratio joins in the reactor, starting stirrer stirs, speed of agitator is adjusted to 5 ~ 15 Hz, and the dispersed with stirring time is 0.5 ~ 1 h, stirs; After join in the reactor that surfactant and deionized water are housed, continue dispersed with stirring, speed of agitator is adjusted to 15 ~ 25 Hz, the dispersed with stirring time is 0.5 ~ 1 h, stirs; Be adjusted to 25 ~ 35 Hz at speed of agitator then, temperature of reaction is 75 ~ 95 ℃ of reactions down, and the reaction time is 1.5 ~ 3.5 h, and temperature retention time is 1.5 ~ 3 h; Be cooled to normal temperature, obtain compound;
B) with methyl alcohol the compound that obtains is carried out breakdown of emulsion, separation, make compound form liquid-solid two-phase, remove liquid phase, obtain containing the material of the solid particle of torispherical;
C) clean with the material of deionized water to the solid particle that contains torispherical, obtain the solid particle of torispherical;
D) under 40 ~ 45 ℃ temperature, aim at spheric grain and carry out the drying processing, make its water cut be lower than 0.5wt%;
E) add silicon dioxide and evenly mixing, dried torispherical particle is carried out modification handle, obtain mean grain size D
50It is the color toner of 5 ~ 8 μ m.
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Cited By (2)
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CN103543622A (en) * | 2013-10-24 | 2014-01-29 | 南京理工大学 | A kind of color toner prepared by miniemulsion polymerization and its 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 |
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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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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 |
US20080286677A1 (en) * | 2006-11-30 | 2008-11-20 | Kyocera Mita Corporation | Toner for developer |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103543622A (en) * | 2013-10-24 | 2014-01-29 | 南京理工大学 | A kind of color toner prepared by miniemulsion polymerization and its method |
CN103543622B (en) * | 2013-10-24 | 2016-04-20 | 南京理工大学 | Color ink powder prepared by miniemulsion polymerization and method thereof |
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 |
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