CN109852142B - Preparation method of coating ink for small-particle-size ceramic ink-jet printing - Google Patents
Preparation method of coating ink for small-particle-size ceramic ink-jet printing Download PDFInfo
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Abstract
The invention discloses a preparation method of coating ink for small-particle-size ceramic ink-jet printing. By using grinding media with different particle sizes for graded grinding, the coating pigment suitable for ceramic ink-jet printing is successfully prepared. The method is simple and efficient to operate and is suitable for preparing various coating inks. The prepared ceramic ink has uniform pigment particles, narrow particle size distribution, average particle size of 500-600 nm and maximum particle size of no more than 1 mu m, and the wrapped ink is full and bright in color after being sintered at the high temperature of 1000-1300 ℃, so that the ceramic ink can be used for ceramic chip production and can also be used in the field of archaized bricks. The problems that the ink is easy to precipitate and block a nozzle when the ink is too large in fineness and the color difference is caused when the ink is too small in fineness are solved. The ink particles are distributed in a centralized manner, so that the storage stability and printing smoothness of the wrapped ink are improved, the pigment is prevented from being damaged irregularly, and the color development stability is improved. The use of the wrapping ink enriches the pattern design of the ceramic tile product, greatly simplifies the production process of the ceramic tile and saves the production cost of enterprises.
Description
Technical Field
The invention relates to a preparation method of ceramic ink, in particular to a preparation method of coating ink for ceramic ink-jet printing.
Background
In recent years, the ceramic ink-jet printing technology rapidly replaces the silk screen and roller printing technology with extremely high automation degree and production stability, becomes the most popular surface decoration technology, and is praised as the third decoration technical revolution of the ceramic industry. With the comprehensive popularization and application of ceramic ink-jet printing technology, the demand of ceramic ink as a ceramic surface decorative material is increasing day by day.
Ceramic inks are generally composed of colorants, resins, dispersants, leveling agents, defoamers, anti-settling agents, and solvents. The ink for ink-jet printing needs to be prepared by grinding and dispersing the pigment into ink, the pigment in the ink must be superfine to submicron and nanometer levels to realize ink-jet printing, otherwise the smoothness of ink-jet printing cannot be ensured, and even a nozzle can be blocked. In the case of a conventional non-encapsulated coloring material, the coloring effect can be ensured by grinding and crushing the coloring material to a predetermined particle diameter. The form of the pulverized and crushed particles of the coloring material is not particularly limited, and may be any form. As in the prior art, praseodymium yellow, red brown, cobalt blue, cobalt black and other inks are generally prepared by first-stage grinding dispersion.
At present, red ceramic ink mainly takes pink and red brown as main materials, particularly red brown, but the red brown ink has lighter and darker color, the produced ceramic tile product has insufficient color, rigid pattern and easy distortion, a silk screen printing procedure is usually required to be added after ink-jet printing, and the problem is solved by using fancy glaze containing wrapped scarlet pigment to complement color of the product. This, however, not only increases the complexity of the production operation, but also increases the labor and equipment costs.
The wrapped scarlet and the wrapped rhubarb ink have bright and pure colors, full colors and high saturation, can be superposed with other color inks to form a wider color gamut range, greatly enriches the types of color systems of the ceramic inks, and enables the color patterns and patterns of ceramic tile products to be more colorful. As shown in fig. 1, a transmission electron micrograph of a typical encapsulated colorant in a ceramic ink shows, in the encapsulated colorant, a color former is encapsulated in the pigment. If the shell outside the color body (such as zirconium silicate shell) is damaged, the color body can be completely exposed in the air and oxidized and decomposed at high temperature, so that the color body cannot be developed or is dull, and the color development effect is greatly influenced. However, their particles are generally large and require further refinement to be useful in ceramic ink jet printing.
In general, the more uniform the particles in the ceramic ink, the narrower the particle size distribution, and the more favorable the color development of the encapsulated ink. However, due to the special coating structure of the coating type pigment, the grinding and refining process has a dilemma, on one hand, in order to ensure the color development effect, the coating type pigment cannot be ground too finely so as to avoid damaging the coating type structure, but if the particles of the pigment are too large, the storage stability of the ink is poor, and the precipitation is very easy to generate; on the other hand, the fine particles are required to ensure the printing smoothness and the ink stability, but the coating structure is possibly damaged and the color development is difficult.
The prepared coated ceramic ink for ink-jet printing is the key for simplifying the ceramic printing production process and reducing the production cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of the coating ink which has a good color development effect and is suitable for small-particle-size ceramic ink-jet printing for ceramic ink-jet printing.
The technical scheme adopted by the invention is as follows:
a preparation method of coating ink for ceramic ink-jet printing comprises the following steps:
1) mixing the coating pigment and the solvent, and uniformly dispersing to obtain the material to be ground;
2) carrying out primary grinding on the material to be ground, wherein the size of a grinding medium is 1.0-1.5 mm, and grinding until the average particle size of a pigment is 1.0-1.3 mu m to obtain a primary grinding material;
3) performing secondary grinding on the primary grinding material, wherein the size of a grinding medium is 0.7-1.0 mm and is smaller than that of the primary grinding medium, and grinding until the average particle size of the pigment is 0.7-0.9 mu m to obtain a secondary grinding material;
4) carrying out three-stage grinding on the secondary grinding material, wherein the size of a grinding medium is 0.5-0.7 mm and is smaller than that of the grinding medium of the secondary grinding, and grinding until the average particle size of the pigment is 0.5-0.6 mu m to obtain pigment slurry for ceramic ink-jet printing;
5) and mixing the pigment slurry with other additives to obtain the coating ink for ceramic ink-jet printing.
As a further improvement of the preparation method, the size of the grinding medium used in the primary grinding is 1.1-1.3 mm.
As a further improvement of the preparation method, the size of the grinding medium used in the secondary grinding is 0.7-0.9 mm.
As a further improvement of the preparation method, the size of the grinding medium used in the third-stage grinding is 0.5-0.6 mm.
As a further improvement of the preparation method, the initial particle size of the coating pigment is 1-5 μm.
As a further improvement of the preparation method, the coating pigment is selected from at least one of zirconium silicate coated cadmium sulfoselenide scarlet and zirconium silicate coated cadmium sulfide rhubarb.
As a further improvement of the preparation method, the coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 30-60% of coating pigment, 1-5% of resin, 3-8% of dispersing agent, 0-0.5% of flatting agent, 0-0.6% of defoaming agent, 0-0.5% of anti-settling agent and the balance of solvent.
As a further improvement of the above production method, the resin includes at least one of an alkyd resin, an acrylic resin, and a polyester resin.
As a further improvement of the preparation method, the coating pigment, the resin, the dispersant, the anti-settling agent and part of the solvent are mixed and dispersed uniformly to obtain the material to be ground.
As a further improvement of the above preparation process, the dispersant is independently a polyurethane-type dispersant.
As a further improvement of the preparation method, the leveling agent is Levaslip8629 independently.
As a further improvement of the preparation method, the anti-settling agent is Disparlon NS-5501 or Haimines SD-1 independently.
As a further improvement of the above production method, the solvent independently comprises at least one of diethylene glycol methyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether acetate and an alicyclic hydrocarbon organic solvent.
The invention has the beneficial effects that:
the method is simple and efficient to operate and is suitable for preparing various coating inks. The prepared ceramic ink has uniform pigment particles, narrow particle size distribution, average particle size of 500-600 nm and maximum particle size of no more than 1 mu m, and the wrapped ink is full and bright in color after being sintered at the high temperature of 1000-1300 ℃, so that the ceramic ink can be used for ceramic chip production and can also be used in the field of archaized bricks. The problems that the ink is easy to precipitate and block a nozzle when the ink is too large in fineness and the color difference is caused when the ink is too small in fineness are solved. The ink particles are distributed in a centralized manner, so that the storage stability and printing smoothness of the wrapped ink are improved, the pigment is prevented from being damaged irregularly, and the color development stability is improved. The use of the wrapping ink enriches the pattern design of the ceramic tile product, greatly simplifies the production process of the ceramic tile and saves the production cost of enterprises.
Drawings
FIG. 1 is a transmission electron micrograph of a typical encapsulated colorant;
FIG. 2 is a photograph of a finished product after firing of a covered scarlet and yellow ink for ceramic ink-jet printing prepared in comparative examples 1 to 3 and examples 1 to 4;
Detailed Description
A preparation method of coating ink for ceramic ink-jet printing comprises the following steps:
1) mixing the coating pigment and the solvent, and uniformly dispersing to obtain the material to be ground;
2) carrying out primary grinding on the material to be ground, wherein the size of a grinding medium is 1.0-1.5 mm, and grinding until the average particle size of a pigment is 1.0-1.3 mu m to obtain a primary grinding material;
3) performing secondary grinding on the primary grinding material, wherein the size of a grinding medium is 0.7-1.0 mm and is smaller than that of the primary grinding medium, and grinding until the average particle size of the pigment is 0.7-0.9 mu m to obtain a secondary grinding material;
4) carrying out three-stage grinding on the secondary grinding material, wherein the size of a grinding medium is 0.5-0.7 mm and is smaller than that of the grinding medium of the secondary grinding, and grinding until the average particle size of the pigment is 0.5-0.6 mu m to obtain pigment slurry for ceramic ink-jet printing;
5) and mixing the pigment slurry with other additives to obtain the coating ink for ceramic ink-jet printing.
As a further improvement of the preparation method, the size of the grinding medium used in the primary grinding is 1.1-1.3 mm.
As a further improvement of the preparation method, the size of the grinding medium used in the secondary grinding is 0.7-0.9 mm.
As a further improvement of the preparation method, the size of the grinding medium used in the third-stage grinding is 0.5-0.6 mm.
Particularly, the size of the grinding medium used in the primary grinding is 1.1-1.3 mm; the size of the grinding medium used for the secondary grinding is 0.7-0.9 mm; the size of the grinding medium used in the third-stage grinding is 0.5-0.6 mm.
As a further improvement of the preparation method, the initial particle size of the coating pigment is 1-5 μm.
As a further improvement of the preparation method, the coating pigment is selected from at least one of zirconium silicate coated cadmium sulfoselenide scarlet and zirconium silicate coated cadmium sulfide rhubarb.
The coating ink for ceramic ink-jet printing can be obtained by compounding according to the actual production requirements and the composition of the existing ceramic ink-jet printing ink. As a further improvement of the preparation method, the coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 30-60% of coating pigment, 1-5% of resin, 3-8% of dispersing agent, 0-0.5% of flatting agent, 0-0.6% of defoaming agent, 0-0.5% of anti-settling agent and the balance of solvent.
As a further improvement of the above production method, the resin includes at least one of an alkyd resin, an acrylic resin, and a polyester resin.
In order to simplify the production process and improve the mixing effect, as a further improvement of the preparation method, the coating pigment, the resin, the dispersing agent, the anti-settling agent and part of the solvent are mixed and dispersed uniformly to obtain the material to be ground. And then grinding together, and the grinding process can fully and uniformly mix the components.
As a further improvement of the above preparation process, the dispersant is independently a polyurethane-type dispersant.
As a further improvement of the preparation method, the leveling agent is Levaslip8629 independently.
As a further improvement of the preparation method, the anti-settling agent is Disparlon NS-5501 or Haimines SD-1 independently.
As a further improvement of the above production method, the solvent independently comprises at least one of diethylene glycol methyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether acetate and an alicyclic hydrocarbon organic solvent.
The technical scheme of the invention is further explained by combining the embodiment.
For convenience of comparison, in the following examples and comparative examples, the resin was YL-885 polyester resin, the dispersant was a polyurethane type dispersant TR-7010, the leveling agent was Levaslip8629, the defoaming agent was an organosilicon defoaming agent AT-99, the anti-settling agent was Hamming SD-1, and the solvent was an alicyclic hydrocarbon organic solvent.
Example 1
The coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 50% of coating pigment (zirconium silicate coated cadmium sulfoselenide red), 2% of resin, 6% of dispersing agent, 0.1% of flatting agent, 0.1% of defoaming agent, 0.2% of anti-settling agent and the balance of solvent.
Example 2
The coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 50% of coating pigment (zirconium silicate coated cadmium sulfoselenide red), 2.5% of resin, 5.5% of dispersing agent, 0.1% of flatting agent, 0.1% of defoaming agent, 0.25% of anti-settling agent and the balance of solvent.
Example 3
The coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 50% of coating pigment (zirconium silicate coated cadmium sulfide rhubarb), 3% of resin, 6% of dispersing agent, 0.1% of flatting agent, 0.2% of defoaming agent, 0.3% of anti-settling agent and the balance of solvent.
Example 4
The coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 50% of coating pigment (zirconium silicate coated cadmium sulfide rhubarb), 2% of resin, 4.5% of dispersing agent, 0.2% of flatting agent, 0.2% of defoaming agent, 0.15% of anti-settling agent and the balance of solvent.
Comparative example 1
The coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 50% of coating pigment (zirconium silicate coated cadmium sulfoselenide red), 2% of resin, 6% of dispersing agent, 0.1% of flatting agent, 0.1% of defoaming agent, 0.2% of anti-settling agent and the balance of solvent.
Comparative example 2
The coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 50% of coating pigment (zirconium silicate coated cadmium sulfide rhubarb), 2.5% of resin, 5% of dispersing agent, 0.1% of flatting agent, 0.2% of defoaming agent, 0.3% of anti-settling agent and the balance of solvent.
Comparative example 3
The coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 50% of coating pigment (zirconium silicate coated cadmium sulfide red), 3% of resin, 6% of dispersing agent, 0.1% of flatting agent, 0.2% of defoaming agent, 0.3% of anti-settling agent and the balance of solvent.
The preparation process of the coating ink for different ceramic ink-jet printing is shown in table 1, and the average particle size of the pigment obtained by final grinding is controlled to be 400-600 nm.
TABLE 1 preparation Process parameters of wrapping ink for ceramic ink-jet printing
And (3) performance detection:
the prepared wrapping ink for ceramic ink-jet printing is subjected to performance detection, and the test results are shown in table 2.
TABLE 2 results of performance testing of the wrapping inks for ceramic ink-jet printing
Note: the viscosity was measured at 40 ℃ using a rotary viscometer; the surface tension was measured at a temperature of 40 ℃ using a dynamic surface tensiometer.
According to analysis results, the ink prepared by the first-stage grinding in the comparative examples 1-2 is uneven in particle size distribution, the size of the ratio (D90-D10)/D50 represents the width of particle size distribution, the particle size distribution in the comparative examples 1-2 is obviously wider than that in the comparative examples 1-4, the particle size distribution is easy to show bimodal or multimodal distribution, the fineness of a plurality of pigment particles is too large, the suspension property of the ink is poor, and precipitates are easy to generate and block a spray head. Comparative example 3 the ink performance was improved by the two-stage milling compared to comparative examples 1-2, but the results were still not comparable to the three-stage milling results of examples 1-4.
The ink prepared in the embodiments 1 to 4 of the invention has the viscosity of 15.0 to 40.0mPa · s, the surface tension of 20 to 30mN/m, uniform particle size distribution, average particle size of 500 to 600nm, maximum particle size of not more than 1 μm, good stability and good ink-jet printing fluency. The phenomena of line breakage, streak and the like do not occur, the nozzle cannot be abraded and blocked, and the printed pattern is clear in detail and bright in color. The three-stage grinding adopts a regular step-by-step grinding mode, large grinding media are firstly used for grinding large-particle pigments to be controlled in a medium particle size range, then medium-particle pigments are ground again by using medium-particle grinding media, finally small grinding media are further ground and ground, the particle size of the final pigment particles is mainly concentrated in the range of 400-700 nm, and the proportion is up to 80%, so that the coated ink is good in color development and good in suspension stability. The three-stage grinding mode overcomes the defects that the red and yellow pigment coated on the market is ground too finely and the color development force is reduced. The particle size distribution of the wrapped ink subjected to three-stage grinding and dispersing treatment is very narrow, the defects of large particles and poor dispersibility of the wrapped red and yellow ink are overcome from the production technology, and the wrapped red and yellow ink has a great market prospect.
The process for manufacturing the ink-coated ceramic ink-jet printing product comprises the following steps:
pressing blank of a press → drying of a blank → spraying water on the blank for surface glaze (bell jar) → ceramic ink jet printing on the surface of the green brick → spraying and polishing the green brick for glaze (bell jar) → sintering of the semi-finished product in a kiln at 1200 deg.C → finished product.
FIG. 2 is a photograph of a fired product of a red and yellow ink for covering ceramic ink-jet printing prepared in comparative examples 1 to 3 and examples 1 to 4, in which comparative examples 1 to 3 correspond to numbers 1 to 3 on the figure and examples 1 to 4 correspond to numbers 4 to 7 on the figure. As can be seen from the figure, the wrapping ink prepared in comparative examples 1-3 is easy to block the nozzle, and the printed patterns have phenomena of wire drawing, wire breaking and the like, wherein No. 1 is the most serious, and No. 2 and No. 3 are the second; comparative example 2 through the first-stage grinding for a prolonged period of time, the prepared ink does not improve the printing fluency, and the coating pigment is damaged irregularly and seriously to cause the color development of the pattern to be poor; the ink prepared in the embodiment 1-4 is smooth in printing, the phenomena of line pulling and line breaking do not occur, and the No. 4-7 pattern is bright and full in color development.
Claims (7)
1. A preparation method of coating ink for ceramic ink-jet printing comprises the following steps:
1) mixing the coating pigment and the solvent, and uniformly dispersing to obtain the material to be ground;
2) performing primary grinding on the material to be ground, wherein the size of a grinding medium is 1.1-1.3 mm, and grinding until the average particle size of a pigment is 1.0-1.3 mu m to obtain a primary grinding material;
3) performing secondary grinding on the primary grinding material, wherein the size of a grinding medium is 0.7-0.9 mm and is smaller than that of the primary grinding medium, and grinding until the average particle size of the pigment is 0.7-0.9 mu m to obtain a secondary grinding material;
4) carrying out three-stage grinding on the secondary grinding material, wherein the size of a grinding medium is 0.5-0.6 mm and is smaller than that of the grinding medium of the secondary grinding, and grinding until the average particle size of the pigment is 0.5-0.6 mu m to obtain pigment slurry for ceramic ink-jet printing;
5) and mixing the pigment slurry with other additives to obtain the coating ink for ceramic ink-jet printing.
2. The method of claim 1, wherein: the initial particle size of the coating pigment is 1-5 μm.
3. The method of claim 1, wherein: the coating pigment is at least one of zirconium silicate coated cadmium sulfoselenide scarlet and zirconium silicate coated cadmium sulfide rhubarb.
4. The method of claim 1, wherein: the coating ink for ceramic ink-jet printing comprises the following components in percentage by mass: 30-60% of coating pigment, 1-5% of resin, 3-8% of dispersing agent, 0-0.5% of flatting agent, 0-0.6% of defoaming agent, 0-0.5% of anti-settling agent and the balance of solvent.
5. The method of claim 4, wherein: the resin includes at least one of alkyd resin, acrylic resin, and polyester resin.
6. The method of claim 4, wherein: and mixing and dispersing the coating pigment, the resin, the dispersing agent, the anti-settling agent and part of the solvent uniformly to obtain the material to be ground.
7. The method of claim 4, wherein: the dispersant is polyurethane dispersant; the leveling agent is Levaslip 8629; the anti-settling agent is Disparlon NS-5501 or Haimines SD-1; the solvent comprises at least one of diethylene glycol methyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether acetate and alicyclic hydrocarbon organic solvents.
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| CN111018543B (en) * | 2020-01-02 | 2022-04-01 | 杭州诺贝尔陶瓷有限公司 | Once-fired ultra-large specification thin porcelain plate and production method thereof |
| CN111004038B (en) * | 2020-01-02 | 2022-05-03 | 杭州诺贝尔陶瓷有限公司 | Super-large-specification thin porcelain plate with electrothermal function and production method thereof |
| CN113234357B (en) * | 2021-05-12 | 2023-05-05 | 闻涛 | Preparation method of environment-friendly high-performance digital inkjet red ink |
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Effective date of registration: 20221117 Address after: 529441 Room 102, 1st floor, Daoshi technology complex building, Sanlian fozai'ao, Shengtang Town, Enping City, Jiangmen City, Guangdong Province Patentee after: Guangdong Dow ceramic materials Co.,Ltd. Address before: 528031 Building 1, No. 131, Jihua West Road, Chancheng District, Foshan City, Guangdong Province Patentee before: FOSHAN DOWSTONG TECHNOLOGY Co.,Ltd. |
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