CN107239011B - Preparation method of colored carbon powder - Google Patents

Preparation method of colored carbon powder Download PDF

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CN107239011B
CN107239011B CN201710577522.1A CN201710577522A CN107239011B CN 107239011 B CN107239011 B CN 107239011B CN 201710577522 A CN201710577522 A CN 201710577522A CN 107239011 B CN107239011 B CN 107239011B
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carbon powder
mixture
dispersion liquid
mass fraction
nano
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CN107239011A (en
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白娜娜
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Hefei Wanshui Information Technology Co ltd
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    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00Developers
    • G03G9/08Developers with toner particles
    • G03G9/0802Preparation methods
    • G03G9/0804Preparation methods whereby the components are brought together in a liquid dispersing medium
    • G03G9/0806Preparation methods whereby the components are brought together in a liquid dispersing medium whereby chemical synthesis of at least one of the toner components takes place

Abstract

The invention discloses a preparation method of colored carbon powder, relating to the technical field of office supplies, wherein (1) reaction components are respectively prepared; (2) adding the polymer emulsion, the wax dispersion liquid and the colorant dispersion liquid into deionized water to obtain a mixed solution, and adding humic acid grafted acrylic acid into the mixed solution to obtain a pretreated material; (3) adding a polymerization reaction monomer and an initiator into the pretreated material to carry out polymerization reaction, controlling the reaction temperature to be between 80 and 90 ℃, then carrying out ultrasonic treatment, and then carrying out cooling, separation and drying to obtain colored carbon powder; the color carbon powder prepared by the invention is not adhered to a roller, and the color can be preserved for a long time.

Description

Preparation method of colored carbon powder
Technical Field
The invention belongs to the technical field of office supplies, and particularly relates to a preparation method of colored carbon powder.
Background
The color toner is generally composed of a polymer resin, a colorant (pigment or dye), a wax, an external additive (charge control agent, etc.), and the like. The color carbon powder for electrostatic development is prepared through smelting and crushing process including the steps of smelting, mixing, extruding, cooling, crushing, superfine crushing, grading, adding additive, etc. to prepare color carbon powder. However, the preparation method has the defects that the coloring agent cannot be uniformly dispersed in the resin, the prepared color carbon powder has irregular shape, large particle size and wide distribution, and the like, so that the defects of poor fixability (easy roller sticking), low resolution, poor color, high waste powder rate and the like exist during printing and copying, and the method is relatively complex in process and high in cost.
Disclosure of Invention
The invention aims to provide a preparation method of colored carbon powder aiming at the existing problems.
The invention is realized by the following technical scheme:
a preparation method of color carbon powder comprises the following steps:
(1) respectively preparing reaction components:
preparing a high-molecular emulsion, wherein the high-molecular emulsion is formed by mixing styrene-acrylic polymer emulsion and polyacrylate emulsion according to the mass ratio of 5-8: 1;
adding polypropylene wax and activated nano diatomite particles into deionized water to prepare 5-7% of polypropylene wax dispersion liquid, wherein the mass percent of the activated nano diatomite in the polypropylene wax dispersion liquid is 0.2-0.4%;
adding a colorant and bismuth oxide coated nano silicon dioxide into deionized water to prepare a colorant dispersion liquid with the mass fraction of 1.2-1.5%, wherein the mass fraction of the bismuth oxide coated nano silicon dioxide in the colorant dispersion liquid is 0.3-0.5%;
(2) mixing the polymer emulsion, the wax dispersion liquid and the coloring agent dispersion liquid according to the weight ratio of 58-60: adding 3-5 mass percent of the mixture into deionized water for dispersion, adjusting the pH value of the mixture to 4.2-4.5, stirring at the rotating speed of 300r/min for 30-35min to obtain a mixed solution, adding 0.25-0.30 mass percent of humic acid grafted acrylic acid into the mixed solution, heating to 60-80 ℃, stirring at the rotating speed of 500r/min for 2 hours, and adjusting the pH value of the mixed solution to be neutral to obtain a pretreated material;
(3) adding 5-8% of polymerization reaction monomer and 0.01-0.03% of initiator into the pretreated material for polymerization reaction, controlling the reaction temperature between 80-90 ℃ and the reaction time between 3-5 hours, then carrying out ultrasonic treatment for 3-5min, cooling, separating and drying to obtain the colored carbon powder.
Further, the preparation method of the activated nano diatomite particles comprises the following steps: mixing a certain amount of nano kieselguhr and deionized water to prepare a nano kieselguhr water suspension with the mass fraction of 5.5-6.5%, then adopting hydrochloric acid with the mass fraction of 0.2% to adjust the pH value of the suspension to 4.5, heating to 60 ℃, stirring for 10min at the rotating speed of 500r/min, then adding ammonium persulfate with the mass fraction of 0.08% of the suspension, stirring uniformly, keeping the temperature at 80 ℃ for 12min, then carrying out vacuum filtration, and drying by adopting a vacuum drying oven to obtain the nano kieselguhr suspension.
Further, the preparation method of the bismuth oxide coated nano silicon dioxide comprises the following steps: according to the following steps of 100: 3.5-3.8, putting the nano silicon dioxide and the bismuth nitrate into a ball milling tank, and controlling the ball-material ratio to be 50: 1, adding absolute ethyl alcohol with the mass 3 times of that of the nano silicon dioxide, performing ball milling for 1 hour, and drying to remove the absolute ethyl alcohol to obtain a solid mixture; adding sodium carbonate accounting for 0.25-0.28% of the mass of the solid mixture into the solid mixture, then adding deionized water accounting for 0.25% of the mass of the solid mixture, uniformly stirring, and continuing ball milling for 30min to obtain a mixed material; placing the mixed material in a muffle furnace, calcining for 30min at the temperature of 400-450 ℃, naturally cooling to room temperature to obtain solid powder, and mixing the solid powder according to the weight ratio of 1: 5, adding the mixture into absolute ethyl alcohol, stirring the mixture for 1 hour at the rotating speed of 2500r/min, grinding the mixture for 2 hours, and then drying the mixture to room temperature in vacuum to obtain the catalyst.
Further, the colorant is an azo pigment.
Further, the initiator is diacyl peroxide.
Further, the ultrasonic power is 500W, and the frequency is 30 kHz.
Compared with the prior art, the invention has the following advantages: in the invention, the printing performances such as durability, fixing ability and the like of the color carbon powder can be comprehensively considered to control all quality parameters of the high molecular emulsion, and researches show that: by adding a certain amount of polyacrylate emulsion into the styrene-acrylic polymer emulsion, the durability and the fixing capability of the colored carbon powder can be obviously improved, and the particles can be dispersed more uniformly; according to the invention, through the synergistic effect of adding activated nano diatomite particles into carbon powder and humic acid grafted acrylic acid, the effects of helping flowability, enhancing charge performance, enhancing environmental stability and the like are mainly achieved, the effects of improving image color density, bottom ash, image uniformity and transfer efficiency in the printing process when the carbon powder is applied to an electrostatic developing aspect are finally improved, and the phenomenon that the carbon powder is easy to stick to a roller in the printing and copying process can be solved; the bismuth oxide coated nano silicon dioxide is added into the carbon powder, so that the defect that the color of the carbon powder commonly used for laser printers, ink-jet printers and common color laser printers can not be preserved for a long time is overcome, the bismuth oxide coated nano silicon dioxide has the effect of stabilizing and uniformly coloring agents, and the color durability of the archives images and texts can be obviously improved.
Detailed Description
Example 1
A preparation method of color carbon powder comprises the following steps:
(1) respectively preparing reaction components:
preparing a high-molecular emulsion, wherein the high-molecular emulsion is formed by mixing styrene-acrylic polymer emulsion and polyacrylate emulsion according to a mass ratio of 5: 1;
adding polypropylene wax and activated nano diatomite particles into deionized water to prepare 5% by mass of polypropylene wax dispersion liquid, wherein the mass percent of the activated nano diatomite in the polypropylene wax dispersion liquid is 0.2%;
adding a coloring agent and bismuth oxide coated nano silicon dioxide into deionized water to prepare a coloring agent dispersion liquid with the mass fraction of 1.2%, wherein the mass fraction of the bismuth oxide coated nano silicon dioxide in the coloring agent dispersion liquid is 0.3%;
(2) mixing the polymer emulsion, the wax dispersion liquid and the coloring agent dispersion liquid according to the weight ratio of 58: 6:3, adding the mixture into deionized water for dispersion according to the mass ratio, adjusting the pH value of the mixture to 4.2, stirring the mixture for 30min at the rotating speed of 300r/min to obtain a mixed solution, adding humic acid grafted acrylic acid with the mass of 0.25% of the mixed solution into the mixed solution, heating the mixed solution to 60 ℃, stirring the mixed solution for 2 hours at the rotating speed of 500r/min, and adjusting the pH value of the mixed solution to be neutral to obtain a pretreated material;
(3) adding 5% of polymerization reaction monomer and 0.01% of initiator into the pretreated material for polymerization reaction, controlling the reaction temperature between 80 ℃ and the reaction time to be 3 hours, then carrying out ultrasonic treatment for 3min, and then carrying out cooling, separation and drying to obtain the colored carbon powder.
Further, the preparation method of the activated nano diatomite particles comprises the following steps: mixing a certain amount of nano kieselguhr and deionized water to prepare a nano kieselguhr water suspension with the mass fraction of 5.5%, then adopting hydrochloric acid with the mass fraction of 0.2% to adjust the pH value of the suspension to 4.5, heating to 60 ℃, stirring for 10min at the rotating speed of 500r/min, then adding ammonium persulfate with the mass fraction of 0.08% of the suspension, stirring uniformly, keeping the temperature at 80 ℃ for 12min, then carrying out vacuum filtration, and drying by adopting a vacuum drying oven to obtain the nano kieselguhr water suspension.
Further, the preparation method of the bismuth oxide coated nano silicon dioxide comprises the following steps: according to the following steps of 100: 3.5, putting the nano silicon dioxide and the bismuth nitrate into a ball milling tank in a mass ratio of 50: 1, adding absolute ethyl alcohol with the mass 3 times of that of the nano silicon dioxide, performing ball milling for 1 hour, and drying to remove the absolute ethyl alcohol to obtain a solid mixture; adding sodium carbonate accounting for 0.25% of the mass of the solid mixture into the solid mixture, then adding deionized water accounting for 0.25% of the mass of the solid mixture into the solid mixture, uniformly stirring the mixture, and continuing to perform ball milling for 30min to obtain a mixed material; placing the mixed material in a muffle furnace, calcining for 30min at 400 ℃, naturally cooling to room temperature to obtain solid powder, and mixing the solid powder according to the weight ratio of 1: 5, adding the mixture into absolute ethyl alcohol, stirring the mixture for 1 hour at the rotating speed of 2500r/min, grinding the mixture for 2 hours, and then drying the mixture to room temperature in vacuum to obtain the catalyst.
Further, the colorant is an azo pigment.
Further, the initiator is diacyl peroxide.
Further, the ultrasonic power is 500W, and the frequency is 30 kHz.
Example 2
A preparation method of color carbon powder comprises the following steps:
(1) respectively preparing reaction components:
preparing a high-molecular emulsion, wherein the high-molecular emulsion is formed by mixing styrene-acrylic polymer emulsion and polyacrylate emulsion according to a mass ratio of 8: 1;
adding polypropylene wax and activated nano diatomite particles into deionized water to prepare 7% by mass of polypropylene wax dispersion liquid, wherein the mass percent of the activated nano diatomite in the polypropylene wax dispersion liquid is 0.4%;
adding a coloring agent and bismuth oxide coated nano silicon dioxide into deionized water to prepare a coloring agent dispersion liquid with the mass fraction of 1.5%, wherein the mass fraction of the bismuth oxide coated nano silicon dioxide in the coloring agent dispersion liquid is 0.5%;
(2) mixing the polymer emulsion, the wax dispersion liquid and the coloring agent dispersion liquid according to the weight ratio of 60: adding the mixture into deionized water according to the mass ratio of 8: 5 for dispersion, adjusting the pH value of the mixture to 4.5, stirring at the rotating speed of 300r/min for 35min to obtain a mixed solution, adding humic acid grafted acrylic acid with the mass of 0.30% of the mixed solution into the mixed solution, heating to 80 ℃, stirring at the rotating speed of 500r/min for 2 hours, and adjusting the pH value of the mixed solution to be neutral to obtain a pretreated material;
(3) adding 8% of polymerization reaction monomer and 0.03% of initiator into the pretreated material for polymerization reaction, controlling the reaction temperature between 90 ℃ and the reaction time to be 5 hours, then carrying out ultrasonic treatment for 5min, and then carrying out cooling, separation and drying to obtain the colored carbon powder.
Further, the preparation method of the activated nano diatomite particles comprises the following steps: mixing a certain amount of nano kieselguhr and deionized water to prepare a nano kieselguhr water suspension with the mass fraction of 6.5%, then adopting hydrochloric acid with the mass fraction of 0.2% to adjust the pH value of the suspension to 4.5, heating to 60 ℃, stirring for 10min at the rotating speed of 500r/min, then adding ammonium persulfate with the mass fraction of 0.08% of the suspension, stirring uniformly, keeping the temperature at 80 ℃ for 12min, then carrying out vacuum filtration, and drying by adopting a vacuum drying oven to obtain the nano kieselguhr water suspension.
Further, the preparation method of the bismuth oxide coated nano silicon dioxide comprises the following steps: according to the following steps of 100: 3.8, putting the nano silicon dioxide and the bismuth nitrate into a ball milling tank according to the mass ratio of 50: 1, adding absolute ethyl alcohol with the mass 3 times of that of the nano silicon dioxide, performing ball milling for 1 hour, and drying to remove the absolute ethyl alcohol to obtain a solid mixture; adding sodium carbonate accounting for 0.28% of the mass of the solid mixture into the solid mixture, then adding deionized water accounting for 0.25% of the mass of the solid mixture into the solid mixture, uniformly stirring the mixture, and continuing to perform ball milling for 30min to obtain a mixed material; placing the mixed material in a muffle furnace, calcining for 30min at 450 ℃, naturally cooling to room temperature to obtain solid powder, and mixing the solid powder according to the weight ratio of 1: 5, adding the mixture into absolute ethyl alcohol, stirring the mixture for 1 hour at the rotating speed of 2500r/min, grinding the mixture for 2 hours, and then drying the mixture to room temperature in vacuum to obtain the catalyst.
Further, the colorant is an azo pigment.
Further, the initiator is diacyl peroxide.
Further, the ultrasonic power is 500W, and the frequency is 30 kHz.
Example 3
A preparation method of color carbon powder comprises the following steps:
(1) respectively preparing reaction components:
preparing a high-molecular emulsion, wherein the high-molecular emulsion is formed by mixing styrene-acrylic polymer emulsion and polyacrylate emulsion according to the mass ratio of 6: 1;
adding polypropylene wax and activated nano diatomite particles into deionized water to prepare polypropylene wax dispersion liquid with the mass fraction of 6%, wherein the mass percent of the activated nano diatomite in the polypropylene wax dispersion liquid is 0.3%;
adding a coloring agent and bismuth oxide coated nano silicon dioxide into deionized water to prepare a coloring agent dispersion liquid with the mass fraction of 1.4%, wherein the mass fraction of the bismuth oxide coated nano silicon dioxide in the coloring agent dispersion liquid is 0.4%;
(2) mixing the polymer emulsion, the wax dispersion liquid and the coloring agent dispersion liquid according to the proportion of 59: adding the mixture into deionized water at a mass ratio of 7:4 for dispersion, adjusting the pH value of the mixture to 4.3, stirring at a rotating speed of 300r/min for 32min to obtain a mixed solution, adding humic acid grafted acrylic acid with the mass of 0.28% of the mixed solution into the mixed solution, heating to 70 ℃, stirring at a rotating speed of 500r/min for 2 hours, and adjusting the pH value of the mixed solution to be neutral to obtain a pretreated material;
(3) adding 6% of polymerization reaction monomer and 0.02% of initiator into the pretreated material for polymerization reaction, controlling the reaction temperature to be 85 ℃, controlling the reaction time to be 4 hours, then carrying out ultrasonic treatment for 4min, and then carrying out cooling, separation and drying to obtain the colored carbon powder.
Further, the preparation method of the activated nano diatomite particles comprises the following steps: mixing a certain amount of nano kieselguhr and deionized water to prepare a nano kieselguhr water suspension with the mass fraction of 5.8%, then adopting hydrochloric acid with the mass fraction of 0.2% to adjust the pH value of the suspension to 4.5, heating to 60 ℃, stirring for 10min at the rotating speed of 500r/min, then adding ammonium persulfate with the mass fraction of 0.08% of the suspension, stirring uniformly, keeping the temperature at 80 ℃ for 12min, then carrying out vacuum filtration, and drying by adopting a vacuum drying oven to obtain the nano kieselguhr water suspension.
Further, the preparation method of the bismuth oxide coated nano silicon dioxide comprises the following steps: according to the following steps of 100: 3.6, putting the nano silicon dioxide and the bismuth nitrate into a ball milling tank according to the mass ratio of 50: 1, adding absolute ethyl alcohol with the mass 3 times of that of the nano silicon dioxide, performing ball milling for 1 hour, and drying to remove the absolute ethyl alcohol to obtain a solid mixture; adding sodium carbonate accounting for 0.26% of the mass of the solid mixture into the solid mixture, then adding deionized water accounting for 0.25% of the mass of the solid mixture into the solid mixture, uniformly stirring the mixture, and continuing to perform ball milling for 30min to obtain a mixed material; placing the mixed material in a muffle furnace, calcining for 30min at 420 ℃, naturally cooling to room temperature to obtain solid powder, and mixing the solid powder according to the weight ratio of 1: 5, adding the mixture into absolute ethyl alcohol, stirring the mixture for 1 hour at the rotating speed of 2500r/min, grinding the mixture for 2 hours, and then drying the mixture to room temperature in vacuum to obtain the catalyst.
Further, the colorant is an azo pigment.
Further, the initiator is diacyl peroxide.
Further, the ultrasonic power is 500W, and the frequency is 30 kHz.
Comparative example 1: only differs from example 1 in that no activated nano-diatomaceous earth particles are added.
Comparative example 2: only the same amount of untreated nano-diatomaceous earth particles was added as in example 1.
Comparative example 3: only differs from example 1 in that no bismuth oxide coated nanosilica is added.
Comparative example 4: the only difference from example 1 is that an equal amount of nanosilica was added instead of the bismuth oxide coated nanosilica.
The respective Color toners prepared in the above examples and comparative examples were evaluated for fixability (roll tack) as represented by Color L aserJet 2600, a printer of hewlett packard co.
1. Evaluation of fixability:
placing a printer filled with color carbon powder in a low-temperature and low-humidity (10 ℃/RH 10%) environment for 12h, then printing E-shaped plate samples with 5% coverage, continuously printing 3000 sheets, observing whether carbon powder is adhered to a roller at a fixing part by eye, sampling and testing bottom ash, respectively testing azo black E and azo yellow by using coloring agents, and taking an average value; the results are shown in Table 1:
TABLE 1 evaluation results of color toner fixability
Figure DEST_PATH_IMAGE002
As can be seen from Table 1, the color carbon powder prepared by the invention can solve the problem that the carbon powder is easy to stick to a roller during printing and copying.
The red carbon powder prepared in the embodiment and the comparative examples 3 and 4 is subjected to laser printing, and the printed pictures and texts are respectively placed and processed for 30min at high temperature and low temperature, and observed:
TABLE 2
Figure DEST_PATH_IMAGE004
As can be seen from Table 2, the carbon powder prepared by the invention has good temperature resistance and can be stored for a long time without fading.

Claims (6)

1. A preparation method of color carbon powder is characterized by comprising the following steps:
(1) respectively preparing reaction components:
preparing a high-molecular emulsion, wherein the high-molecular emulsion is formed by mixing styrene-acrylic polymer emulsion and polyacrylate emulsion according to the mass ratio of 5-8: 1;
adding polypropylene wax and activated nano diatomite particles into deionized water to prepare 5-7% of polypropylene wax dispersion liquid, wherein the mass percent of the activated nano diatomite in the polypropylene wax dispersion liquid is 0.2-0.4%;
adding a colorant and bismuth oxide coated nano silicon dioxide into deionized water to prepare a colorant dispersion liquid with the mass fraction of 1.2-1.5%, wherein the mass fraction of the bismuth oxide coated nano silicon dioxide in the colorant dispersion liquid is 0.3-0.5%;
(2) mixing the polymer emulsion, the wax dispersion liquid and the coloring agent dispersion liquid according to the weight ratio of 58-60: adding 3-5 mass percent of the mixture into deionized water for dispersion, adjusting the pH value of the mixture to 4.2-4.5, stirring at the rotating speed of 300r/min for 30-35min to obtain a mixed solution, adding humic acid grafted acrylic acid with the mass fraction of 0.25-0.30% into the mixed solution, heating to 60-80 ℃, stirring at the rotating speed of 500r/min for 2 hours, and adjusting the pH value of the mixed solution to be neutral to obtain a pretreated material;
(3) adding 5-8% of polymerization reaction monomer and 0.01-0.03% of initiator into the pretreated material for polymerization reaction, controlling the reaction temperature between 80-90 ℃ and the reaction time between 3-5 hours, then carrying out ultrasonic treatment for 3-5min, cooling, separating and drying to obtain the colored carbon powder.
2. The method for preparing colored carbon powder according to claim 1, wherein the method for preparing the activated nano diatomite particles comprises the following steps: mixing a certain amount of nano kieselguhr and deionized water to prepare a nano kieselguhr water suspension with the mass fraction of 5.5-6.5%, then adopting hydrochloric acid with the mass fraction of 0.2% to adjust the pH value of the suspension to 4.5, heating to 60 ℃, stirring for 10min at the rotating speed of 500r/min, then adding ammonium persulfate with the mass fraction of 0.08% into the suspension, stirring uniformly, keeping the temperature at 80 ℃ for 12min, then carrying out vacuum filtration, and drying by adopting a vacuum drying oven to obtain the nano kieselguhr suspension.
3. The method for preparing colored carbon powder according to claim 1, wherein the method for preparing bismuth oxide coated nano-silica comprises: according to the following steps of 100: 3.5-3.8, putting the nano silicon dioxide and the bismuth nitrate into a ball milling tank, and controlling the ball-material ratio to be 50: 1, adding absolute ethyl alcohol with the mass 3 times of that of the nano silicon dioxide, performing ball milling for 1 hour, and drying to remove the absolute ethyl alcohol to obtain a solid mixture; adding sodium carbonate with the mass fraction of 0.25-0.28% into the solid mixture, then adding deionized water with the mass fraction of 0.25% into the solid mixture, uniformly stirring, and continuing ball milling for 30min to obtain a mixed material; placing the mixed material in a muffle furnace, calcining for 30min at the temperature of 400-450 ℃, naturally cooling to room temperature to obtain solid powder, and mixing the solid powder according to the weight ratio of 1: 5, adding the mixture into absolute ethyl alcohol, stirring the mixture for 1 hour at the rotating speed of 2500r/min, grinding the mixture for 2 hours, and then drying the mixture to room temperature in vacuum to obtain the catalyst.
4. The method for preparing colored carbon powder according to claim 1, wherein the colorant is azo pigment.
5. The method for preparing colored carbon powder according to claim 1, wherein the initiator is diacyl peroxide.
6. The method for preparing colored carbon powder according to claim 1, wherein the ultrasonic power is 500W and the frequency is 30 kHz.
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