CN103257539A - Color toner and preparation method thereof - Google Patents
Color toner and preparation method thereof Download PDFInfo
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- CN103257539A CN103257539A CN2013101856541A CN201310185654A CN103257539A CN 103257539 A CN103257539 A CN 103257539A CN 2013101856541 A CN2013101856541 A CN 2013101856541A CN 201310185654 A CN201310185654 A CN 201310185654A CN 103257539 A CN103257539 A CN 103257539A
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Abstract
The invention discloses a color toner, which comprises the following components in parts by weight: 60-80 parts of styrene, 15-25 parts of butyl acrylate, 1-4 parts of a composite surface modifier, 3-7 parts of wax, 3-6 parts of pigment, 0.2-1.5 parts of a charge control agent, 1-2 parts of ammonium persulfate, 1.0-3.0 parts of a surfactant, and 0.1-2 parts of a molecular weight regulator, wherein the composite surface modifier includes a combination of silicon dioxide and silicon dioxide. According to the invention, through adding the composite surface modifier in the later stage of emulsion preparation, compared with methods only using silicon dioxide or titanium dioxide, the method has the beneficial effects that the fluidity and charging of the color toner can be improved, so that the charging is more uniform. The particle size is easy to control, the particle size distribution is narrow, and the mean particle size D50 is 5-8 micrometers.
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 surface modifier in emulsion polymerization and report seldom, particularly compound surface-treating agent was blended in it wherein equably in the emulsion preparation later stage, thereby improve liquidity and charging property, 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 can improving liquidity and charging property, makes its charging property more even, and particle size is the color toner of control easily.
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;
1 ~ 4 part of compound surface-treating agent;
3 ~ 7 parts in wax;
3 ~ 6 parts of pigment;
0.2 ~ 1.5 part of charge adjusting agent;
1 ~ 2 part of ammonium persulfate;
1.0 ~ 3.0 parts in surfactant;
0.1 ~ 2 part of molecular weight regulator;
Described compound surface-treating agent comprises the compound of silicon dioxide and titania.
Add compound surface-treating agent, compare with only using silicon dioxide or titania, because silicon dioxide electrifies soon, electronegative ability is strong, and titania relatively a little less than a bit, both are used, can improve flowability and the charging property of color toner, particle size is controlled easily.
The composite weight ratio (earth silicon/titanic oxide) of described compound surface-treating agent is 4:1 ~ 1:1; When composite weight ratio greater than 4:1, do not have the flowability of improving color toner and the effect of charging property, when composite weight ratio less than 1:1, the cost of ink powder can improve a lot, also is unfavorable for the carried charge control of ink powder.
The composite weight ratio (earth silicon/titanic oxide) of described compound surface-treating agent is preferably 4:1 ~ 2.5:1, under this compound proportion, can maximize flowability and the charging property of improving color toner, and particle size is controlled easily.
Described wax is selected from one or more of Brazil wax, polypropylene wax, C80 paraffin.
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, 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 compound surface-treating agent 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.
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 only using silicon dioxide or titania by adding compound surface-treating agent in the emulsion preparation later stage, can improve flowability and the charging property of color toner, and particle size is controlled easily.
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.
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;
Having taken by weighing styrene, butyl acrylate, 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 compound surface-treating agent 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 ~ 7 and the Comparative Examples 1 ~ 3
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 | |
| Styrene | 60 | 65 | 72 | 75 | 80 | 62 | 70 | 60 | 72 | 80 |
| Butyl acrylate | 15 | 20 | 22 | 19 | 25 | 23 | 21 | 15 | 22 | 25 |
| Silicon dioxide | 0.5 | 2 | 3 | 3 | 2.5 | 2 | 3 | / | 3.75 | 8 |
| Titania | 0.5 | 1 | 0.75 | 1 | 1 | 1 | 1 | 1 | / | / |
| Pigment | 3 | 5 | 6 | 4 | 3 | 3 | 5 | 3 | 6 | 3 |
| The DL-N28 metal complex | 0.5 | 1 | 1.5 | 0.2 | 1 | 1 | 1 | 0.5 | 1.5 | 1 |
| Ammonium persulfate | 1 | 1.5 | 1.5 | 2 | 1.5 | 1.5 | 1.5 | 1 | 1.5 | 1.5 |
| The CO-436 surfactant | 3 | 1.5 | 2 | 1 | 2.5 | 2 | 2 | 3 | 2 | 2.5 |
| Charging property (microcoulomb/gram) | 9~27 | 10~26 | 9~26 | 11~25 | 11~26 | 9~25 | 10~25 | 5~30 | 6~28 | 5~30 |
| Mean grain size D 50/μm | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~8 | 5~9 | 4~10 |
| Circularity | 0.95 | 0.97 | 0.96 | 0.98 | 0.97 | 0.96 | 0.97 | 0.93 | 0.94 | 0.92 |
| Softening point temperature/℃ | 119.4 | 112.7 | 112.9 | 119.0 | 112.7 | 107.5 | 114.5 | 120.1 | 113.1 | 113.1 |
Every performance test methods:
Charging property: the charging property of ink powder adopts the U.S. to produce TREK aspiration-type carried charge tester and measures;
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.
Can find out that from embodiment and the Comparative Examples of last table 1 the present invention compares with only using silicon dioxide or titania by adding compound surface-treating agent in the emulsion preparation later stage, can improve flowability and the charging property of color toner, makes its charging property more even; Particle size is controlled easily, and uniform particles 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.
Claims (6)
1. color toner is characterized in that: by weight, comprise following component:
60 ~ 80 parts of styrene;
15 ~ 25 parts of butyl acrylates;
1 ~ 4 part of compound surface-treating agent;
3 ~ 7 parts in 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;
Described compound surface-treating agent comprises the compound of silicon dioxide and titania.
2. color toner according to claim 1 is characterized in that, the composite weight ratio of described compound surface-treating agent is 4:1 ~ 1:1.
3. color toner according to claim 2 is characterized in that, the composite weight ratio of described compound surface-treating agent is preferably 4:1 ~ 2.5:1.
4. color toner according to claim 1 is characterized in that, described wax is selected from one or more of Brazil wax, polypropylene wax, C80 paraffin.
5. 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.
6. as the preparation method of each described color toner of claim 1 ~ 5, it is characterized in that, comprise the steps:
A) taking by weighing carefully according to the above ratio, styrene, butyl acrylate, wax, pigment, charge adjusting agent, ammonium persulfate, molecular weight regulator join 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 compound surface-treating agent 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310185654.1A CN103257539B (en) | 2013-05-20 | 2013-05-20 | A kind of color toner and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310185654.1A CN103257539B (en) | 2013-05-20 | 2013-05-20 | A kind of color toner and preparation method thereof |
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| Publication Number | Publication Date |
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| CN103257539A true CN103257539A (en) | 2013-08-21 |
| CN103257539B CN103257539B (en) | 2015-08-05 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107085359A (en) * | 2017-04-27 | 2017-08-22 | 安徽斌欣电子科技有限公司 | Environmentally friendly ink powder and preparation method thereof |
| CN110007571A (en) * | 2019-03-05 | 2019-07-12 | 湖北雨田科技有限公司 | A kind of color toner and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1851560A (en) * | 2005-04-22 | 2006-10-25 | 株式会社理光 | Electrophotographic toner, developer and image forming device |
| CN1892451A (en) * | 2005-07-08 | 2007-01-10 | 施乐公司 | Toner and developer compositions |
| CN102004403A (en) * | 2010-09-27 | 2011-04-06 | 河北丰华重工机电设备制造有限公司 | Copy toner |
-
2013
- 2013-05-20 CN CN201310185654.1A patent/CN103257539B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1851560A (en) * | 2005-04-22 | 2006-10-25 | 株式会社理光 | Electrophotographic toner, developer and image forming device |
| CN1892451A (en) * | 2005-07-08 | 2007-01-10 | 施乐公司 | Toner and developer compositions |
| CN102004403A (en) * | 2010-09-27 | 2011-04-06 | 河北丰华重工机电设备制造有限公司 | Copy toner |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107085359A (en) * | 2017-04-27 | 2017-08-22 | 安徽斌欣电子科技有限公司 | Environmentally friendly ink powder and preparation method thereof |
| CN110007571A (en) * | 2019-03-05 | 2019-07-12 | 湖北雨田科技有限公司 | A kind of color toner and preparation method thereof |
| CN110007571B (en) * | 2019-03-05 | 2023-07-04 | 湖北雨田科技有限公司 | Color toner and preparation method thereof |
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