CN110764379A - Blue ceramic toner prepared by suspension polymerization method and preparation method thereof - Google Patents
Blue ceramic toner prepared by suspension polymerization method and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a blue ceramic ink powder prepared by a suspension polymerization method and a preparation method thereof. The invention adopts the ball milling dispersion technology and the suspension polymerization method to prepare the ceramic ink powder, effectively solves the problems of uneven components and easy leakage of the ceramic ink powder prepared by the traditional melting and crushing method, and has the advantages of uniform dispersion of the components, regular appearance, smooth surface, controllable particle size, narrow particle size distribution and the like.
Description
Technical Field
The invention relates to a blue ceramic toner and a preparation method thereof, in particular to a blue ceramic toner for ceramic laser printing and a preparation method thereof.
Background
The decoration means of the ceramic material mainly comprises three processes of applique, roller printing and ink-jet printing at present, the three decoration processes can basically meet the large-scale decoration requirements of various ceramic products, but the existing decoration means gradually becomes insufficient along with the improvement of the requirements of people on the appearance quality of the ceramic products and the expansion of the personalized market demand. Recently, a ceramic laser printing process has better, finer and more real decoration effect and can design decoration patterns for customers, so that the ceramic laser printing process is more and more popular with enterprises and customers. Therefore, the technology will be the next technical revolution in the field of ceramic decoration.
At present, the preparation method of the ceramic toner is mainly a melting and crushing method. The melt crushing method is still the mainstream technology for industrially preparing the ceramic ink powder at present because of the advantages of mature technology, easy and safe operation, stable production quality, lower production cost and the like. For example, Zhongtianjia electronics Co., Ltd. in Tianjin City (patent CN 20101010413.3), black ceramic pigment, styrene acrylic resin, charge regulator, polypropylene wax and other components are mixed by mixing equipment, and then coarse crushing, micro crushing and grading are carried out to remove large and small particles, and particles with the particle size of 6-10 μm are reserved. Wuxi Jiateng magnetic powder Co., Ltd (patent CN 201110327960.5) pours blue inorganic ceramic pigment, styrene-acrylic resin, polypropylene wax and charge regulator into a mixing roll, mixes them evenly to prepare a mixture, puts into an extruding machine, tabletting at high temperature, cooling and crushing, and grading to obtain particles with average particle size of 6-8 μm. In a similar patent CN201510302129.1, a high-temperature resistant color toner is prepared by a melting and crushing method, and the diameter of the screened toner is 8-20 μm. However, the toner particles prepared by the fusion method have irregular shapes, rough particle appearance, wide particle size distribution and uneven distribution of all components, and the ceramic pigment is easy to fall off, so that high-resolution and high-quality color patterns cannot be printed.
Disclosure of Invention
The invention provides a method for preparing blue ceramic ink powder for ceramic printing by ball milling and suspension polymerization, which has the advantages of uniform distribution of components, regular appearance, controllable particle size, narrow particle size distribution, simple process, energy conservation, environmental protection and low cost, and aims to overcome the technical defects of irregular shape, rough particle appearance, wide particle size distribution, non-uniform distribution of the components, easiness in falling off, incapability of printing high-resolution high-quality color images and high cost of the ink powder prepared by the prior art.
The technical scheme for realizing the purpose of the invention is as follows:
the blue ceramic toner provided by the invention comprises the following components in parts by weight:
10-40 parts of blue ceramic pigment
65-80 parts of styrene
10-20 parts of butyl acrylate
1-3 parts of charge regulator
3-6 parts of wax
1.5-3 parts of initiator
10-20 parts of dispersant
1-2 parts of surfactant
3-5 parts of hydrophobic silicon dioxide
750 portions of deionized water and 1000 portions of deionized water.
Furthermore, the blue ceramic pigment adopts any one of cobalt blue PB-28, chromium cobalt blue PB-36 and vanadium zirconium blue.
Further, the charge regulator is a metal complex produced by Hubeidinglong chemical industry Co.
Further, the wax is one of slice paraffin and polyethylene wax.
Further, the initiator is one of Azobisisobutyronitrile (AIBN), azobisisoheptonitrile, Benzoyl Peroxide (BPO) and lauroyl peroxide.
Further, the dispersing agent is one of polyvinyl alcohol 1788, polyvinyl alcohol 1750 +/-50, gelatin and methyl cellulose.
Further, the surfactant is one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, tween-60 and tween-80.
The preparation method of the blue ceramic toner comprises the following steps:
(1) surface modification of ceramic pigment, namely adding blue ceramic pigment into toluene solution and carrying out ultrasonic treatment for 30 minutes, adding silane coupling agent into the toluene solution and carrying out ultrasonic treatment for 30 minutes, heating the mixture to 80 ℃ and stirring for 5 hours, finally washing with ethanol for several times, drying at 60 ℃ for 12 hours, and grinding for later use;
(2) preparing an oil phase: adding wax into a monomer mixed by styrene and butyl acrylate, heating to dissolve the wax, then adding the modified blue ceramic pigment, the charge regulator and the initiator into the monomer, ultrasonically dispersing for 5min, transferring the mixed solution into a ball milling tank containing zirconium dioxide microspheres, and performing ball milling for 4-6h to obtain uniform and stable dispersion liquid;
(3) preparing an aqueous phase: adding a dispersing agent and a surfactant into deionized water, and heating to dissolve the dispersing agent and the surfactant;
(4) preparing a mixed phase: slowly dropping the oil phase liquid into the water phase and shearing at high speed under the action of a high-shear emulsifying machine;
(5) polymerization: transferring the sheared mixed solution into a container, heating to 75-85 ℃ under the protection of nitrogen, and stirring for reacting for 6-10 h;
(6) and (3) separation and drying: filtering and separating the product obtained in the step (5), washing with deionized water for 1-3 times to remove redundant dispersing agent and surfactant, washing with absolute ethyl alcohol for 1-3 times to remove a small amount of unreacted monomer, transferring the product to a vacuum oven, and drying in vacuum at 35-50 ℃ for 6-10h to obtain dry and pure quasi-ceramic powdered ink particles;
(7) adding externally: and adding hydrophobic silicon dioxide, and carrying out modification treatment on the dried quasi-ceramic toner particles to obtain the ceramic toner for the ceramic laser printer.
Further, in the step (1), the silane coupling agent accounts for 5wt% of the ceramic pigment, and the stirring speed is 400-500 r/min.
Further, in the step (2), zirconium dioxide microspheres with the diameter of 1.2-1.6mm are adopted for ball milling, the mass ratio of the zirconium dioxide microspheres to the ceramic pigment is 50:1-100:1, and the rotating speed of the ball mill is 500-.
Further, in the step (4), the rotation speed of the high shear emulsifying machine is 4000-.
Further, in the step (5), the stirring speed is 300-500 r/min.
Compared with the prior art, the invention has the advantages and beneficial effects that:
(1) the invention is favorable for solving the problem of uniform dispersion of each functional component by a ball milling dispersion technology.
(2) The invention uses the styrene-acrylic resin to coat the pigment, the wax and the charge agent, and can effectively solve the problem of leakage of the pigment and the wax particles.
(3) The invention prepares the composite particles with the particle size of 6-10 microns through suspension polymerization, so that the blue ceramic toner which is spherical in shape, smooth in surface, uniform in particle size and narrow in distribution is finally obtained.
(4) The ceramic ink powder is prepared by suspension polymerization, and the preparation method has the advantages of simple process, energy conservation, environmental protection and low cost.
Drawings
FIG. 1 is a block diagram of the process flow of the present invention.
FIG. 2 is an SEM image of a ceramic toner prepared by suspension polymerization in example 1 of the present invention, in which a: overall view, b: individual ink particle patterns.
FIG. 3 is a graph showing the particle size distribution of the ceramic toner prepared in example 1 of the present invention.
FIG. 4 is a DSC chart of the ceramic toner prepared in example 2 of the present invention.
FIG. 5 is an XRD pattern of the calcined and cobalt blue pigment of the ceramic toner of example 3 of the present invention at 1000 ℃.
Detailed Description
Example 1
The technological process of the preparation method of the blue ceramic toner is shown in figure 1.
(1) Surface modification of ceramic pigment 10 parts of ceramic pigment cobalt blue PB-28 are added into 100 parts of toluene solution and subjected to ultrasonic treatment for 30 minutes, 0.5 part of silane coupling agent is added into the toluene solution and subjected to ultrasonic treatment for 30 minutes, and then the mixture is heated to 80 ℃ and stirred for 5 hours at the rotating speed of 400 r/min. Finally, washing with ethanol for several times, drying at 60 ℃ for 12h, and grinding for later use.
(2) Preparing an oil phase: adding 3 parts of sliced paraffin into a monomer mixed with 65 parts of styrene and 10 parts of butyl acrylate, heating to dissolve the sliced paraffin, then adding the treated blue ceramic pigment (1), 1 part of charge regulator and 1.5 parts of initiator BPO into the monomer, performing ultrasonic dispersion for 5min, transferring the mixed solution into a ball-milling tank containing zirconium dioxide microspheres with the particle size of 1.2-1.6mm, performing ball-milling dispersion for 4h, wherein the mass ratio of the zirconium dioxide microspheres to the ceramic pigment is 50:1, and the rotating speed of the ball mill is 500 r/min.
(3) Preparing an aqueous phase: 10 parts of polyvinyl alcohol 1788 and 1 part of sodium lauryl sulfate were added to 750 parts of deionized water and heated to dissolve them.
(4) Preparing a mixed phase: slowly dripping the oil phase liquid (2) into the water phase (3) and shearing at high speed under the action of a high-shear emulsifying machine, wherein the rotating speed is 6000 r/min.
(5) Polymerization: transferring the sheared mixed solution into a four-neck flask, heating to 75 ℃ under the protection of nitrogen, and reacting for 10 hours at the stirring speed of 300 r/min.
(6) And (3) separation and drying: and (3) filtering and separating the product in the step (5), washing the product with deionized water for three times to remove redundant dispersing agent and surfactant, and then washing the product with absolute ethyl alcohol for three times to remove a small amount of unreacted monomer. And transferring the product to a vacuum oven, and carrying out vacuum drying for 6h at 50 ℃ to obtain the dry pure quasi-ceramic ink powder particles.
(7) Adding externally: and adding 3 parts of modified silicon dioxide, and carrying out modification treatment on the dried quasi-ceramic toner particles to obtain the ceramic toner for the ceramic laser printer.
FIG. 2 is an SEM image of a ceramic toner prepared by suspension polymerization in example 1 of the present invention, in which a: overall view, 2 b: individual ink particle patterns. From FIG. 2a, it is clear that the ceramic toner is uniform microspheres and has a uniform particle size distribution, wherein the particle size ranges from 6 μm to 10 μm, and from FIG. 2b, it is clear that the surface of the single ceramic toner is smooth and the particle size is about 8 μm.
Fig. 3 is a graph showing the particle size distribution of the ceramic toner prepared in example 1 of the present invention, and it can be seen from the graph that the average particle size d50=8.43 μm and the distribution curve is narrow, which corresponds to the particle size in fig. 2.
Example 2
(1) Surface modification of ceramic pigment is carried out by adding 20 portions of ceramic pigment cobalt blue PB-28 into 200 portions of toluene solution, carrying out ultrasonic treatment for 30 minutes, adding 1.0 portion of silane coupling agent into the toluene solution, carrying out ultrasonic treatment for 30 minutes, heating the mixture to 80 ℃ and stirring the mixture for 5 hours at a rotation speed of 450 r/min. Finally, washing with ethanol for several times, drying at 60 ℃ for 12h, and grinding for later use.
(2) Preparing an oil phase: adding 4.5 parts of sliced paraffin into a monomer mixed with 70 parts of styrene and 15 parts of butyl acrylate, heating to dissolve the sliced paraffin, then adding the treated blue ceramic pigment (1), 1.5 parts of charge regulator and 2 parts of initiator BPO into the monomer, ultrasonically dispersing for 5min, transferring the mixed solution into a ball-milling tank containing zirconium dioxide microspheres with the particle size of 1.2-1.6mm, and carrying out ball-milling dispersion for 5h, wherein the mass ratio of the zirconium dioxide microspheres to the ceramic pigment is 75:1, and the rotating speed of the ball mill is 600 r/min.
(3) Preparing an aqueous phase: 15 parts of polyvinyl alcohol 1788 and 1.5 parts of sodium lauryl sulfate were added to 850 parts of deionized water and heated to dissolve them.
(4) Preparing a mixed phase: slowly dripping the oil phase liquid in the step (2) into the water phase in the step (3) and shearing at high speed under the action of a high-shear emulsifying machine, wherein the rotating speed is 5000 r/min.
(5) Polymerization: transferring the sheared mixed solution into a four-neck flask, heating to 80 ℃ under the protection of nitrogen, and reacting for 8 hours at the stirring speed of 400 r/min.
(6) And (3) separation and drying: and (3) filtering and separating the product in the step (5), washing the product with deionized water for three times to remove redundant dispersing agent and surfactant, and then washing the product with absolute ethyl alcohol for three times to remove a small amount of unreacted monomer. And transferring the product to a vacuum oven, and carrying out vacuum drying for 10h at 35 ℃ to obtain the dry pure quasi-ceramic ink powder particles.
(7) Adding externally: and adding 4 parts of modified silicon dioxide, and carrying out modification treatment on the dried quasi-ceramic toner particles to obtain the ceramic toner for the ceramic laser printer.
FIG. 4 is a DSC of the ceramic toner prepared in example 2 of the present invention, and we can see that the glass transition temperature (Tg) of the ceramic toner is 62.5 ℃ which is in the range of 50-70 ℃ in conformity with the glass transition temperature of the conventional toner, ensuring better adhesion of the resin to the ceramic substrate.
Example 3
(1) Surface modification of ceramic pigment 40 parts of ceramic pigment cobalt blue PB-28 are added into 400 parts of toluene solution and subjected to ultrasonic treatment for 30 minutes, 2 parts of silane coupling agent are added into the toluene solution and subjected to ultrasonic treatment for 30 minutes, and then the mixture is heated to 80 ℃ and stirred for 5 hours at the rotating speed of 500 r/min. Finally, washing with ethanol for several times, drying at 60 ℃ for 12h, and grinding for later use.
(2) Preparing an oil phase: adding 6 parts of sliced paraffin into a monomer mixed by 80 parts of styrene and 20 parts of butyl acrylate, heating to dissolve the sliced paraffin, then adding the treated blue ceramic pigment (1), 3 parts of charge regulator and 3 parts of initiator BPO into the monomer, performing ultrasonic dispersion for 5min, transferring the mixed solution into a ball-milling tank containing zirconium dioxide microspheres with the particle size of 1.2-1.6mm, performing ball-milling dispersion for 6h, wherein the mass ratio of the zirconium dioxide microspheres to the ceramic pigment is 100:1, and the rotating speed of the ball mill is 700 r/min.
(3) Preparing an aqueous phase: 20 parts of polyvinyl alcohol 1788 and 2 parts of sodium lauryl sulfate are added to 1000 parts of deionized water and heated to dissolve them.
(4) Preparing a mixed phase: slowly dripping the oil phase liquid in the step (2) into the water phase in the step (3) and shearing at high speed under the action of a high-shear emulsifying machine, wherein the rotating speed is 4000 r/min.
(5) Polymerization: transferring the sheared mixed solution into a four-neck flask, heating to 85 ℃ under the protection of nitrogen, and reacting for 7 hours at the stirring speed of 500 r/min.
(6) And (3) separation and drying: and (3) filtering and separating the product in the step (5), washing the product with deionized water for three times to remove redundant dispersing agent and surfactant, and then washing the product with absolute ethyl alcohol for three times to remove a small amount of unreacted monomer. And transferring the product to a vacuum oven, and carrying out vacuum drying at 40 ℃ for 8h to obtain the dry and pure quasi-ceramic toner particles.
(7) Adding externally: and 5 parts of modified silicon dioxide is added, and the dried quasi-ceramic powdered ink particles are modified to obtain the ceramic powdered ink for the ceramic laser printer.
The color properties of the ceramic toner samples with different pigment contents were tested, and the results are shown in table 1:
TABLE 1 color Properties of ceramic toners with different cobalt blue pigment contents
| Examples | Content of cobalt blue | L* | a* | b* | C* | |
| 1 | 10 | 55.22 | 6.22 | -39.59 | 40. 07 | 278.20 |
| 2 | 20 | 53.51 | 7.06 | -40.14 | 40.90 | 281.06 |
| 3 | 40 | 50.88 | 8.82 | -40.34 | 41.04 | 282.44 |
As can be seen from table 1, the ceramic toner hue is reddish blue, the brightness value (L) of the ceramic toner decreases as the cobalt blue pigment content increases, while both the red phase value (a) and the blue phase value (b) show an increasing tendency, and the overall color saturation (C) also increases. From the chromaticity angle h0It can also be seen that the chroma angle of the pigment is approximately 2800To the left and right, the sample color is in the blue region, which is a blue ceramic pigment.
FIG. 5 is an XRD pattern of the calcined ceramic toner of example 3 of the present invention at 1000 ℃ and the cobalt blue pigment, and it can be seen from the XRD pattern that the characteristic diffraction peak of the calcined ceramic toner at 1000 ℃ in curve 2 is consistent with the characteristic diffraction peak of the cobalt blue pigment in curve 1, which indicates that the cobalt blue pigment has good thermal stability and can be used as a ceramic pigment.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The blue ceramic toner is characterized by comprising the following components in parts by weight:
10-40 parts of blue ceramic pigment
65-80 parts of styrene
10-20 parts of butyl acrylate
1-3 parts of charge regulator
3-6 parts of wax
1.5-3 parts of initiator
10-20 parts of dispersant
1-2 parts of surfactant
3-5 parts of hydrophobic silicon dioxide
750 portions of deionized water and 1000 portions of deionized water.
2. The blue ceramic toner according to claim 1, wherein the blue ceramic pigment is any one of cobalt blue PB-28, chromium cobalt blue PB-36, and vanadium zirconium blue.
3. The blue ceramic toner according to claim 1, wherein the charge control agent is a metal complex produced by Hubeidinglong chemical Co.
4. The blue ceramic toner according to claim 1, wherein the wax is one of a sliced paraffin wax and a polyethylene wax.
5. The blue ceramic toner according to claim 1, wherein the initiator is one of azobisisobutyronitrile, azobisisoheptonitrile, benzoyl peroxide, and lauroyl peroxide.
6. The blue ceramic toner according to claim 1, wherein the dispersant is one of polyvinyl alcohol 1788, polyvinyl alcohol 1750 ± 50, gelatin, and methyl cellulose.
7. The blue ceramic toner according to claim 1, wherein the surfactant is one of sodium dodecylbenzenesulfonate, sodium dodecylsulfate, tween-60, and tween-80.
8. The method for producing a blue ceramic toner according to any one of claims 1 to 7, characterized by comprising the steps of:
(1) modified blue ceramic pigment: adding blue ceramic pigment into toluene solution for ultrasonic dispersion, adding silane coupling agent into the toluene solution, performing ultrasonic homogenization, heating the mixture to 80 +/-5 ℃, stirring for more than 5 hours, cleaning, drying and grinding for later use;
(2) preparing an oil phase: adding wax into a mixed monomer of styrene and butyl acrylate, heating to dissolve the wax, adding the modified blue ceramic pigment obtained in the step (1), a charge regulator and an initiator into the mixed monomer, performing ultrasonic dispersion uniformly, and performing ball milling for 4-6h to obtain a uniform and stable dispersion liquid;
(3) preparing an aqueous phase: adding a dispersing agent and a surfactant into deionized water, and heating to dissolve the dispersing agent and the surfactant;
(4) preparing a mixed phase: slowly dripping the oil phase in the step (2) into the water phase in the step (3) and carrying out high-speed shearing;
(5) polymerization: heating the mixed phase in the step (4) to 75-85 ℃ under the protection of nitrogen, and stirring for reacting for 6-10 h;
(6) and (3) separation and drying: filtering and washing the polymerization product obtained in the step (5), and then drying the polymerization product in vacuum for 6 to 10 hours at the temperature of between 35 and 50 ℃ to obtain dry and pure quasi-ceramic powdered ink particles;
(7) adding externally: and (4) adding hydrophobic silica, and carrying out modification treatment on the quasi-ceramic toner particles obtained in the step (6) to obtain the blue ceramic toner.
9. The method according to claim 8, wherein in the step (1), the silane coupling agent accounts for 5wt% of the weight of the blue ceramic pigment.
10. The method according to claim 8, wherein in the step (1), the stirring speed is 400-500 r/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090226837A1 (en) * | 2008-03-10 | 2009-09-10 | Yoshihiro Norikane | Toner manufacturing method, toner manufacturing apparatus, and toner manufactured by way of the toner manufacturing method thereof |
| CN103345133A (en) * | 2013-06-27 | 2013-10-09 | 金发科技股份有限公司 | Colour toner and preparation method thereof |
| CN105153803A (en) * | 2015-10-16 | 2015-12-16 | 佛山市明朝科技开发有限公司 | Colored ceramic ink powder for mass-polymerization architectural ceramic and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090226837A1 (en) * | 2008-03-10 | 2009-09-10 | Yoshihiro Norikane | Toner manufacturing method, toner manufacturing apparatus, and toner manufactured by way of the toner manufacturing method thereof |
| CN103345133A (en) * | 2013-06-27 | 2013-10-09 | 金发科技股份有限公司 | Colour toner and preparation method thereof |
| CN105153803A (en) * | 2015-10-16 | 2015-12-16 | 佛山市明朝科技开发有限公司 | Colored ceramic ink powder for mass-polymerization architectural ceramic and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 佘晓晓等: "陶瓷墨水分散剂的制备与性能研究", 《广东化工》 * |
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