Bright digital ink suitable for being fired at 800 DEG C and preparation method thereof

Abstract

The invention relates to the field of ceramic ink production, in particular to bright digital ink suitable for being fired at 800 DEG C and a preparation method of the bright digital ink. The bright digital ink comprises 25-50% of low-temperature frit powder, 2-10% of a hyperdispersant, 0.01-2% of a defoaming agent and 40-60% of a solvent. Wherein the low-temperature frit powder comprises the following components in percentage by weight: 40 to 65 percent of SiO2, 0.01 to 5 percent of Al2O3, 0.01 to 5 percent of CaO, 0.01 to 5 percent of MgO, 0.01 to 5 percent of K2O, 10 to 25 percent of Na2O, 1 to 10 percent of TiO2, 1 to 10 percent of BaO, 0.01 to 15 percent of ZnO and 5 to 25 percent of B2O3. The bright digital ink prepared by the invention can be used for secondary firing of 800 DEG C ceramic tile products, the prepared ceramic tile products have brighter color patterns and better decorative effect, and the additional value of the products can be better improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of ceramic ink production, in particular to a bright digital ink suitable for 800 DEG C firing and a preparation method thereof. BACKGROUND

[0002] Ceramic inkjet printing technology has been developed for many years in China, and the technology has been popularized. With the serious homogenization of ceramic tiles, it is more and more difficult to innovate the decoration of ceramic tiles. The needs of young consumers are also more and more personalized. In order to better meet the needs of consumers, the secondary firing of ceramic tiles is more and more loved by consumers due to its more vivid color patterns, more rich decoration effects, and the ability to meet the needs of various private customization. However, the current secondary firing decoration surface glaze mostly uses low-temperature dry particles to achieve this, which is very disadvantageous to version conversion and dry particle waste for the increasingly customized products, resulting in high cost. To solve these problems and realize inkjet digital printing, quick customization and version conversion are the best solutions.

[0003] In Chinese patent CN103642317A, a low-temperature ceramic inkjet ink is introduced. The patent is a method of adding some low-temperature colored frits and mineral raw materials to conventional ink. The above patent uses ordinary grinding process, and the general frit cannot meet the printing performance requirements and cannot be suitable for 800 DEG C firing. In addition, most of the low-temperature frits on the market contain a large amount of lead element, which plays a role of dissolving agent in the frit, but it is a heavy metal and is highly toxic, which is not conducive to the environmental protection production and use of ceramic tiles, and cannot well meet the current requirements of ceramic enterprises for secondary firing production decoration. SUMMARY

[0004] The present application is aimed at the current needs of ceramic enterprises to enrich the design style and decoration effect of ceramic tiles by using low-temperature secondary firing, and a bright digital ink suitable for 800 DEG C firing is prepared to better serve ceramic enterprises.

[0005] A bright digital ink suitable for 800 DEG C firing is composed of the following components by weight percentage: low-temperature frit powder 25-50%, super dispersant 2-10%, defoaming agent 0-2%, solvent 40-60%; wherein the low-temperature frit powder component is: SiO2 40-65%, Al2O3 0-5%, CaO 0-5%, MgO 0-5%, K2O 0-5%, Na2O 10-25%, TiO2 1-10%, BaO 1-10%, ZnO 0-15%, B2O3 5-25%.

[0006] Preferably, the low-melting frit powder needs to be prepared according to the ingredient ratio of SiO2 40-65%, Al2O3 0-5%, CaO 0-5%, MgO 0-5%, K2O 0-5%, Na2O 10-25%, TiO2 1-10%, BaO 1-10%, ZnO 0-15%, B2O3 5-25%, and then the frit is sintered at 1300-1600°C to form a glass frit, and then the glass frit is cooled by water quenching and ground to a fineness of 1250 mesh or less.

[0007] Preferably, the hyperdispersant is one or a mixture of several of polyester hyperdispersants, polyurethane hyperdispersants, polyamide hyperdispersants, and polyacrylate hyperdispersants.

[0008] Preferably, the defoaming agent is one or a mixture of several of silicone defoaming agents or polyether defoaming agents.

[0009] Preferably, the solvent is one or a mixture of several of isopropyl laurate, isooctyl cocoate, isooctyl palmitate, myristate, methyl oleate, butyl oleate, methyl laurate, low-polarity alkane solvents ToTal 25-28H, 30-36H, 30-38H, 35-40H, n-undecane, n-dodecane, n-decane, and 5-methyl decane.

[0010] A preparation method of a bright digital ink suitable for firing at 800°C, comprising the following steps:

[0011] Step one: mixing the solvent, hyperdispersant, and defoaming agent to prepare a dispersion liquid;

[0012] Step two: adding the low-melting frit powder to the dispersion liquid and performing stage grinding with a horizontal sand mill;

[0013] Step three: performing grinding with 0.35-0.45 mm zirconium beads at a speed of 50-90% of the highest speed of the sand mill and a zirconium bead filling rate of 70-90%, and grinding to a certain particle size and viscosity of the ink;

[0014] Step four: performing grinding with 0.2-0.25 mm zirconium beads at a speed of 50-90% of the highest speed of the sand mill and a zirconium bead filling rate of 70-90%, and grinding to a certain particle size and viscosity of the ink;

[0015] Step five: performing grinding with 0.1-0.15 mm zirconium beads at a speed of 50-90% of the highest speed of the sand mill and a zirconium bead filling rate of 70-90%, and grinding to a certain particle size and viscosity of the ink and a certain requirement for filtration performance;

[0016] Step six: the prepared ink slurry is added with a certain proportion of solvent, defoaming agent, etc., to be mixed into the required solid content and viscosity, and is filtered through multiple stages to obtain the bright digital ink suitable for 800 DEG C firing.

[0017] Preferably, in step three, the sand mill is used for grinding to an ink particle size D50 < 700 nm, the particle size instrument is Eurofuge, and the 40 DEG C viscosity is < 500 cp, and the viscometer is Brookfield.

[0018] Preferably, in step four, the sand mill is used for grinding to an ink particle size D50 < 650 nm, the particle size instrument is Eurofuge, and the 40 DEG C viscosity is < 500 cp, and the viscometer is Brookfield.

[0019] Preferably, in step five, the sand mill is used for grinding to an ink particle size D50 < 650 nm, the particle size instrument is Eurofuge, and the 40 DEG C viscosity is < 500 cp, and the viscometer is Brookfield, and the Celite glass fiber filter is used for suction filtration, and the suction filtration is greater than 200 g.

[0020] Preferably, in step six, after the prepared ink is mixed, it is filtered through multiple stages of 1 mu m filter element, and is packaged after filtration to obtain the bright digital ink suitable for 800 DEG C firing.

[0021] Compared with the prior art, the present application has the following advantages:

[0022] The bright digital ink suitable for 800 DEG C firing has the characteristics that a low-temperature frit powder prepared by a suitable process is selected, and does not contain lead element, and belongs to a green and environmentally-friendly material. The ordinary ceramic ink preparation process is difficult to grind the frit powder to a suitable printing effect, one is the influence of the powder formula and the firing process, and the other is the influence of the grinding preparation process. Through a large number of experiments, the present application selects a suitable inorganic powder preparation process of low-temperature frit powder, needs to be fired at a suitable temperature, and needs to be water-milled to a sufficient fineness, and a suitable ink grinding preparation process, and successfully prepares a low-temperature bright ink with good printing performance and excellent decoration effect. The low-temperature bright ink prepared by the present application can better serve the secondary firing of 800 DEG C for the ceramic enterprise.

CONCRETE EMBODIMENT

[0023] The present application provides a bright digital ink suitable for 800 DEG C firing, in order to make the technical scheme and preparation method of the present application more clear and clear, the present application is further described in detail as follows.

[0024] A bright light digital ink suitable for 800℃ firing, the bright light digital ink is composed of the following components by weight percentage: low temperature frit powder 25-50%, super dispersant 2-10%, defoaming agent 0-2%, solvent 40-60%; wherein the low temperature frit powder composition is: SiO2 40-65%, Al2O3 0-5%, CaO 0-5%, MgO 0-5%, K2O 0-5%, Na2O 10-25%, TiO2 1-10%, BaO 1-10%, ZnO 0-15%, B2O3 5-25%.

[0025] The low temperature frit powder needs to be prepared according to the ingredient ratio: SiO2 40-65%, Al2O3 0-5%, CaO 0-5%, MgO 0-5%, K2O 0-5%, Na2O 10-25%, TiO2 1-10%, BaO 1-10%, ZnO 0-15%, B2O3 5-25%, first fired into a glass frit at 1300-1600℃, then cooled by water quenching, ground and refined to 1250 mesh or less with water, dried, and treated by air flow grinding for standby.

[0026] The super dispersant is one or a mixture of several of polyester type super dispersant, polyamide type super dispersant, polyacrylate type super dispersant, and polyurethane type dispersant. Such as Lubrizol-13940, Lubrizol-J980, Lubrizol-J1280, S35, Nippon Shokubai 1028, 1087, CH-6, CH-30, AD1310, HP1068, HP1064, HP1062, 905, 914, 926C, etc.

[0027] The defoaming agent is one or several of polyether modified silicone defoaming agent or silicone defoaming agent. Such as BYK-066N, BYK-019, BYK-1719, BYK-1770, BYK-067, 3017, 3206, IC-20, etc.

[0028] The solvent is one or several of isooctyl cocoate, isopropyl laurate, isooctyl palmitate, (2-ethylhexyl) palmitate, myristate, methyl oleate, butyl oleate, methyl laurate, low polarity alkane solvent (such as TOTAL 25-28H, 30-35H, 30-36H, 30-38H, 35-40H), n-undecane, n-dodecane, n-decane, 5-methyl decane.

[0029] The preparation method of the bright light digital ink includes the following steps:

[0030] Step one: mix the solvent, super dispersant, and defoaming agent to prepare a dispersion liquid;

[0031] Step two: add low-temperature frit powder (mass ratio 50-60%) into the dispersion (mass ratio 40-50%), and use a horizontal sand mill to grind in stages.

[0032] Step three: use 0.35-0.45 mm zirconium beads to grind in the first stage, the rotation speed is 50-90% of the highest rotation speed of the sand mill, the zirconium bead filling rate is 70-90%, and the ink is ground to a certain particle size and viscosity.

[0033] Step four: use 0.2-0.25 mm zirconium beads to grind in the second stage, the rotation speed is 50-90% of the highest rotation speed of the sand mill, the zirconium bead filling rate is 70-90%, and the ink is ground to a certain particle size and viscosity.

[0034] Step five: use 0.1-0.15 mm zirconium beads to grind in the third stage, the rotation speed is 50-90% of the highest rotation speed of the sand mill, the zirconium bead filling rate is 70-90%, and the ink is ground to a certain particle size and viscosity, and the filtration performance meets certain requirements.

[0035] Step six: add a certain proportion of solvent, defoaming agent, etc. to the ground ink slurry to adjust the required solid content and viscosity, and then filter through multiple stages to obtain a bright digital ink suitable for 800°C firing.

[0036] In step three, the sand mill is used to grind the ink to a particle size D50 < 700 nm, the particle size instrument is Eurofina, the 40°C viscosity is < 500 cp, and the viscometer is Brookfield.

[0037] In step four, the sand mill is used to grind the ink to a particle size D50 < 650 nm, the particle size instrument is Eurofina, the 40°C viscosity is < 500 cp, and the viscometer is Brookfield.

[0038] In step five, the sand mill is used to grind the ink to a particle size D50 < 650 nm, the particle size instrument is Eurofina, the 40°C viscosity is < 500 cp, and the viscometer is Brookfield. The filter is a Kelvitan glass fiber filter, and the filtration is greater than 200 grams.

[0039] In step six, after the prepared ink is adjusted, it is filtered through multiple 1 μm filter cartridges, and then packaged to obtain a bright digital ink suitable for 800°C firing.

[0040] The preparation process of the present application will be further illustrated by the following examples and comparative examples:

[0041] Example 1:

[0042] A bright light digital ink suitable for firing at 800°C was prepared according to the following formulation, which consisted of the following components in weight percentage: low temperature frit powder 50%, AD1310 5%, BYK067 0.1%, n-decane 30.9%, 5-methyl decane 14%.

[0043] The low temperature frit powder component was as follows: SiO2 55%, Al2O3 1.8%, CaO 0.8%, MgO 0.3%, K2O 1%, Na2O 19%, TiO2 5%, BaO 3.6%, ZnO 1%, B2O3 12.5%; after mixing the ingredients, the mixture was first fired at 1500°C to form a glass frit, then cooled by water quenching, ground to 1250 mesh or less, dried, and used after treatment.

[0044] A low temperature bright light digital ink was prepared according to the above formulation. First, the ultradispersant AD1310 5%, the defoaming agent BYK067 0.1%, n-decane 30.9%, and 5-methyl decane 14% were mixed and stirred uniformly, and then added to a grinding device. While stirring, the sand mill was started.

[0045] First stage grinding: the sand mill was a Netzsch Labstar horizontal sand mill, which used 0.35-0.45 mm zirconium beads for grinding, with a zirconium bead filling rate of 85%, and the grinding speed was set to 3000 r / min. After starting the sand mill, the prepared low temperature glass frit powder was slowly added to the stirring cylinder for cyclic grinding. When the sand mill ground the ink to a particle size D50 < 800 nm, the particle size instrument was a Malvern, and the viscosity was < 500 cp at 40°C, the viscosity meter was a Brookfield, and the second stage grinding was started.

[0046] Second stage grinding: the sand mill was a Netzsch Labstar horizontal sand mill, which used 0.2-0.25 mm zirconium beads for grinding, with a zirconium bead filling rate of 85%, and the grinding speed was set to 3000 r / min. When the sand mill ground the ink to a particle size D50 < 700 nm, the particle size instrument was a Malvern, and the viscosity was < 500 cp at 40°C, the viscosity meter was a Brookfield, and the third stage grinding was started.

[0047] Third stage grinding: the sand mill was a Netzsch Labstar horizontal sand mill, which used 0.1-0.15 mm zirconium beads for grinding, with a zirconium bead filling rate of 85%, and the grinding speed was set to 3000 r / min. When the sand mill ground the ink to a particle size D50 < 630 nm, the particle size instrument was a Malvern, and the viscosity was < 500 cp at 40°C, the viscosity meter was a Brookfield, and the filter was a Whatman 1 μm glass fiber filter. When the filter was used to filter more than 200 grams, the grinding was completed.

[0048] After the ink is ground, the performance parameters of the ink are controlled by adding an appropriate amount of solvent isooctyl cocoate, the solid content of the ink is controlled between 20-40%, the 40°C viscosity is controlled between 10-18 cp, the surface tension is controlled between 25-40 mN / m, and the density is 1.0-1.28 g / cm 3 .

[0049] The prepared ink is filtered through multi-stage 1 μm filter cartridges, and after filtration, the low-temperature bright digital ink product is obtained.

[0050] Example 2

[0051] A bright digital ink suitable for firing at 800°C is prepared according to the following formulation, which is composed of the following components by weight percentage: low-temperature frit powder 50%, 914 6%, BYK067 0.1%, n-undecane 26.9%, isooctyl palmitate 17%.

[0052] The low-temperature frit powder component is: SiO2 50%, Al2O3 1.93%, CaO 0.62%, MgO 0.26%, K2O 1%, Na2O 18.3%, TiO2 5%, BaO 3.6%, ZnO 0.86%, B2O3 18.43%. The ingredients are first prepared into a glass frit by firing at 1550°C, then cooled by water quenching, ground to 1250 mesh or less by water grinding, dried, and used after treatment.

[0053] The low-temperature bright digital ink is prepared according to the above formulation, and the first part: the super dispersant 914 6%, the defoaming agent BYK067 0.1%, the n-undecane 26.9%, and the isooctyl palmitate 17% are mixed and stirred uniformly, and added to the grinding equipment. While stirring, the sand mill is started.

[0054] The first stage of grinding, the sand mill is a Nanjing Labstar horizontal sand mill, which uses 0.35-0.45 mm zirconium beads for grinding, with a zirconium bead filling rate of 85%, and the grinding speed is set to 3000 r / min. After starting the sand mill, the prepared low-temperature glass frit powder is slowly added to the stirring cylinder for circulation grinding. When the sand mill is ground to a particle size D50 < 800 nm, the particle size instrument is Eurotek, and the 40°C viscosity is < 500 cp, the viscometer is Brookfield, and the second stage of grinding is started.

[0055] The second stage grinding, sand mill is a Labstar horizontal sand mill, using 0.2-0.25mm zirconium beads for grinding, zirconium beads filling rate of 85%, set grinding speed 2000r / min. When the sand mill grinding to ink particle size D50 <700nm, particle size instrument using Europe and the United States, 40℃ viscosity <500cp, viscosity meter using Brookfield, into the third stage grinding.

[0056] The third stage grinding, sand mill is a Labstar horizontal sand mill, using 0.1-0.15mm zirconium beads for grinding, zirconium beads filling rate of 85%, set grinding speed 2000r / min. When the sand mill grinding to ink particle size D50 <630nm, particle size instrument using Europe and the United States, 40℃ viscosity <500cp, viscosity meter using Brookfield, using Corbat 1μm glass fiber filter filter, filter greater than 300 grams, complete grinding.

[0057] After the ink grinding qualified, add appropriate amount of solvent isocetyl palmitate to control the performance parameters of the ink, the solid content of the ink is controlled between 20-40%, the 40℃ viscosity is controlled between 10-18cp, the surface tension is controlled between 25-40mN / m, the density is 1.0-1.28g / cm 3 .

[0058] The prepared ink is filtered through multiple 1μm filter cartridges, and the low-temperature bright digital ink product is obtained after packaging.

[0059] Example 3

[0060] The bright digital ink suitable for 800℃ firing is prepared according to the following formula, which is composed of the following components by weight percentage: low-temperature frit powder 50%, CH-6 2%, J9804%, isopropyl laurate 7%, isooctyl cocoate 37%.

[0061] Among them, the low-temperature frit powder component is:

[0062] SiO246%, Al2O32.5%, CaO 3.24%, MgO 2.26%, K2O 5%, Na2O 16.3%, TiO21%, BaO 8.6%, ZnO 4.66%, B2O310.44%, the proportion of ingredients is first prepared into a glass frit by firing at 1550℃, then cooled by water quenching, ground to 1250 mesh or less with water, dried, and used after treatment.

[0063] The low-temperature bright digital ink is prepared according to the above formula, and the first part is prepared by mixing and stirring the dispersant CH-62%, the dispersant J9804%, isopropyl laurate 7%, and isooctyl cocoate 37% uniformly, and then adding them into a grinding device.

[0064] The first stage grinding is performed by using a Netzsch Labstar horizontal sand mill, 0.35-0.45 mm zirconium beads are used for grinding, the filling rate of the zirconium beads is 85%, and the grinding speed is set to 3000 r / min. After the sand mill is started, the prepared low-temperature glass frit powder is slowly added into the stirring cylinder for circulation grinding. When the particle size D50 of the ink is less than 800 nm, the particle size instrument is Malvern, the viscosity at 40°C is less than 500 cp, and the viscometer is Brookfield, the second stage grinding is performed.

[0065] The second stage grinding is performed by using a Netzsch Labstar horizontal sand mill, 0.2-0.25 mm zirconium beads are used for grinding, the filling rate of the zirconium beads is 85%, and the grinding speed is set to 2000 r / min. When the particle size D50 of the ink is less than 700 nm, the particle size instrument is Malvern, the viscosity at 40°C is less than 500 cp, and the viscometer is Brookfield, the third stage grinding is performed.

[0066] The third stage grinding is performed by using a Netzsch Labstar horizontal sand mill, 0.1-0.15 mm zirconium beads are used for grinding, the filling rate of the zirconium beads is 85%, and the grinding speed is set to 2000 r / min. When the particle size D50 of the ink is less than 630 nm, the particle size instrument is Malvern, the viscosity at 40°C is less than 500 cp, the viscometer is Brookfield, and the filter is 1 μm glass fiber filter of Cole-Parmer, the grinding is completed when the filtration is greater than 300 g.

[0067] After the ink grinding is qualified, an appropriate amount of solvent isooctyl cocoate is added to control the performance parameters of the ink. The solid content of the ink is controlled to be between 20-40%, the viscosity at 40°C is controlled to be between 10-18 cp, the surface tension is controlled to be between 25-40 mN / m, and the density is controlled to be between 1.0-1.28 g / cm 3 .

[0068] The prepared ink is filtered through a multi-stage 1 μm filter, and the low-temperature bright digital ink product is obtained after packaging.

[0069] To better illustrate the patent, the following comparative example, because the low temperature clinker powder contains a large amount of B2O3 5-25%, and B2O3 is not able to be prepared by grinding into ink, therefore, it is not advisable to adopt direct grinding after mixing the above raw materials of SiO2 40-65%, Al2O3 0-5%, CaO 0-5%, MgO 0-5%, K2O 0-5%, Na2O 10-25%, TiO2 1-10%, BaO 1-10%, ZnO 0-15%, B2O3 5-25%, which cannot be compared.

[0070] The following comparative example adopts the raw materials of the example to be fired according to the low temperature method for comparison.

[0071] Comparative Example 1

[0072] The ink is prepared according to the following formula of Comparative Example 1:

[0073] Low temperature clinker powder 50%, AD1310 5%, BYK067 0.1%, n-decane 30.9%, 5-methyl decane 14%.

[0074] The composition of the low temperature clinker powder is: SiO2 55%, Al2O3 1.8%, CaO 0.8%, MgO 0.3%, K2O 1%, Na2O 19%, TiO2 5%, BaO 3.6%, ZnO 1%, B2O3 12.5%. The ingredients are first fired at 1150 DEG C, then cooled by water quenching, and then refined by water grinding to 1250 mesh or less, and then dried for standby.

[0075] Comparative Example 1 is prepared according to the above formula, and the ultradispersed agent AD1310 5%, the defoaming agent BYK067 0.1%, the n-decane 30.9%, and the 5-methyl decane 14% are mixed and stirred uniformly, and then added to the grinding equipment. While stirring, the sand mill is started.

[0076] The first stage grinding, the sand mill is Netzsch Labstar horizontal sand mill, and 0.35-0.45 mm zirconium beads are used for grinding. The zirconium bead filling rate is 85%, and the grinding speed is set to 3000 r / min. After starting the sand mill, the prepared powder of Comparative Example 1 is slowly added to the stirring cylinder, and the cycle grinding is carried out. When the sand mill is ground to the ink particle size D50 < 800 nm and the 40 DEG C viscosity < 500 cp, the second stage grinding is entered.

[0077] The second stage grinding, the sand mill is Netzsch Labstar horizontal sand mill, and 0.2-0.25 mm zirconium beads are used for grinding. The zirconium bead filling rate is 85%, and the grinding speed is set to 3000 r / min. When the sand mill is ground to the ink particle size D50 < 700 nm and the 40 DEG C viscosity < 500 cp, the third stage grinding is entered.

[0078] The third stage grinding, the sand mill is Netzsch Labstar horizontal sand mill, using 0.1-0.15mm zirconium beads for grinding, the zirconium beads filling rate is 85%, the grinding speed is set to 3000r / min. When the sand mill grinds to ink particle size D50<630nm, 40℃ viscosity <500cp, using the Corbat 1μm glass fiber filter to filter, the filter is greater than 200g, the grinding is completed.

[0079] After the ink grinding is qualified, add appropriate amount of solvent isooctyl cocoate to control the performance parameters of the ink, the solid content of the ink is controlled between 20-40%, the 40℃ viscosity is controlled between 10-18cp, the surface tension is controlled between 25-40mN / m, and the density is 1.0-1.28g / cm 3 .

[0080] The prepared ink is filtered through multiple 1μm filter cartridges to obtain the ink of Comparative Example 1.

[0081] Comparative Example 2

[0082] Comparative Example 2 is prepared according to the following formula:

[0083] Low temperature frit powder 50%,

[0084] 9146%, BYK067 0.1%, n-undecane 26.9%, isooctyl palmitate 17%.

[0085] The low temperature frit powder needs to be proportioned according to the composition: SiO2 50%, Al2O3 1.93%, CaO 0.62%, MgO 0.26%, K2O 1%, Na2O 18.3%, TiO2 5%, BaO 3.6%, ZnO 0.86%, B2O3 18.43%. First, the glass frit is prepared by firing at 1200℃, then cooled by water quenching, ground to 1250 mesh or less by water grinding, and dried for standby use.

[0086] Comparative Example 2 is prepared according to the above formula, the hyperdispersant 9146%, the defoamer BYK067 0.1%, the n-undecane 26.9%, and the isooctyl palmitate 17% are mixed and stirred uniformly, and added to the grinding equipment. While stirring, the sand mill is started.

[0087] The first stage grinding, the sand mill is Netzsch Labstar horizontal sand mill, using 0.35-0.45mm zirconium beads for grinding, the zirconium beads filling rate is 85%, the grinding speed is set to 3000r / min. After starting the sand mill, the prepared low temperature glass frit powder is slowly added to the stirring cylinder for circulating grinding. When the sand mill grinds to ink particle size D50<800nm, 40℃ viscosity <500cp, the second stage grinding is entered.

[0088] The second stage grinding, sand mill is Nanqi Labstar horizontal sand mill, using 0.2-0.25mm zirconium beads for grinding, zirconium beads filling rate is 85%, set grinding speed 2000r / min. When the sand mill grinding to ink particle size D50 <700nm, 40℃ viscosity <500cp, into the third stage grinding.

[0089] The third stage grinding, sand mill is Nanqi Labstar horizontal sand mill, using 0.1-0.15mm zirconium beads for grinding, zirconium beads filling rate is 85%, set grinding speed 2000r / min. When the sand mill grinding to ink particle size D50 <630nm, 40℃ viscosity <500cp, using Kobleite 1μm glass fiber filter to filter, filter more than 300 grams, complete grinding.

[0090] After the ink grinding qualified, add appropriate amount of solvent hexadecyl isooctyl to control the performance parameters of the ink, the solid content of the ink is controlled between 20-40%, the 40℃ viscosity is controlled between 10-18cp, the surface tension is controlled between 25-40mN / m, the density is 1.0-1.28g / cm 3 .

[0091] The prepared ink is filtered through multiple 1μm filter cartridges to obtain the ink of Comparative Example 2.

[0092] Comparative Example 3

[0093] Comparative Example 3 is prepared according to the following formula:

[0094] Low temperature frit powder 50%, CH-6 62%, J980 4%, isopropyl laurate 7%, isooctyl cocoate 37%.

[0095] The low temperature frit powder needs to be mixed according to the composition: SiO2 46%, Al2O3 2.5%, CaO 3.24%, MgO 2.26%, K2O 5%, Na2O 16.3%, TiO2 1%, BaO 8.6%, ZnO 4.66%, B2O3 10.44%, after batching, first fired at 1200℃, then water quenching, grinding to 1250 mesh or less with water, and drying for standby.

[0096] Comparative Example 3 is prepared according to the above formula, the hyperdispersant CH-6 62%, the hyperdispersant J980 4%, isopropyl laurate 7%, isooctyl cocoate 37% are mixed and stirred uniformly, and added to the grinding equipment. While stirring, the sand mill is started.

[0097] The first stage grinding, sand mill is Labstar horizontal sand mill, using 0.35-0.45mm zirconium beads for grinding, zirconium beads filling rate is 85%, set grinding speed 3000r / min. After starting the sand mill, the prepared low temperature glass frit powder is slowly added to the stirring cylinder, and the cycle grinding is carried out. When the sand mill is ground to ink particle size D50<800nm, 40℃ viscosity <500cp, the second stage grinding is entered.

[0098] The second stage grinding, sand mill is Labstar horizontal sand mill, using 0.2-0.25mm zirconium beads for grinding, zirconium beads filling rate is 85%, set grinding speed 2000r / min. When the sand mill is ground to ink particle size D50<700nm, 40℃ viscosity <500cp, the third stage grinding is entered.

[0099] The third stage grinding, sand mill is Labstar horizontal sand mill, using 0.1-0.15mm zirconium beads for grinding, zirconium beads filling rate is 85%, set grinding speed 2000r / min. When the sand mill is ground to ink particle size D50<630nm, 40℃ viscosity <500cp, using 1μm glass fiber filter of Koble filter to filter, when the filter is greater than 300g, the grinding is completed.

[0100] After the ink grinding is qualified, a proper amount of solvent isopropyl myristate is added to control the performance parameters of the ink, the solid content of the ink is controlled between 20-40%, the 40℃ viscosity is controlled between 10-18cp, the surface tension is controlled between 25-40mN / m, and the density is controlled between 1.0-1.28g / cm 3 .

[0101] Comparative Example 4

[0102] Comparative Example 4 is prepared according to the following formula:

[0103] Frit powder 50%, AD1310 5%, BYK067 0.1%, n-decane 30.9%, 5-methyl decane 14%.

[0104] The frit powder of the comparative example needs to be prepared according to the following composition: SiO222%, Al2O38%, CaO 3%, MgO 6%, K2O 8%, Na2O 19%, TiO25%, BaO 15%, ZnO 10%, B2O34%. The ingredients are first fired at 1150℃, then cooled by water quenching, and then ground to 1250 mesh or less with water, and then dried for standby use.

[0105] Comparative Example 1 is prepared according to the above formula, the hyperdispersant AD1310 5%, antifoam BYK067 0.1%, n-decane 30.9%, 5-methyl decane 14% are mixed and stirred uniformly, and are added to a grinding device. While stirring, the sand mill is started. The first stage grinding is performed using a Netzsch Labstar horizontal sand mill with 0.35-0.45 mm zirconium beads at a filling rate of 85% and a grinding speed of 3000 r / min. After starting the sand mill, the prepared frit powder is slowly added to the stirring cylinder for circulation grinding. When the ink particle size D50 is less than 800 nm and the 40℃ viscosity is less than 500 cp, the second stage grinding is started.

[0106] The second stage grinding is performed using a Netzsch Labstar horizontal sand mill with 0.2-0.25 mm zirconium beads at a filling rate of 85% and a grinding speed of 3000 r / min. When the ink particle size D50 is less than 700 nm and the 40℃ viscosity is less than 500 cp, the third stage grinding is started.

[0107] The third stage grinding is performed using a Netzsch Labstar horizontal sand mill with 0.1-0.15 mm zirconium beads at a filling rate of 85% and a grinding speed of 3000 r / min. When the ink particle size D50 is less than 630 nm and the 40℃ viscosity is less than 500 cp, and the filtration is greater than 300 g using a Whatman 1 μm glass fiber filter, the grinding is completed.

[0108] After the ink grinding is qualified, an appropriate amount of solvent isopropyl myristate is added to control the performance parameters of the ink. The solid content of the ink is controlled between 20-40%, the 40℃ viscosity is controlled between 10-18 cp, the surface tension is controlled between 25-40 mN / m, and the density is controlled between 1.0-1.28 g / cm 3 .

[0109] The prepared ink is filtered through multiple 1 μm filter cartridges to obtain the ink of Comparative Example 4.

[0110]

[0111] Table I

[0112] The low-temperature bright digital ink of Example 1 prepared by the present application is compared with Comparative Example 1 burned at 800℃. It is found that the gloss of Example 1 is 69.4 degrees, and is completely burned. The gloss of Comparative Example 1 is 1.5 degrees, and is completely matte, and is not completely burned.

[0113] The low-temperature bright digital ink prepared by the application is compared with the contrast sample 2 burned at 800 DEG C, the gloss of the example 2 is 76.4 degrees, and the example 2 is completely burned. The gloss of the contrast sample 2 is 1.4 degrees, and the contrast sample 2 is completely matte and not burned.

[0114] The low-temperature bright digital ink prepared by the application is compared with the contrast sample 3 burned at 800 DEG C, the gloss of the example 3 is 80.3 degrees, and the example 3 is completely burned. The gloss of the contrast sample 3 is 1.4 degrees, and the contrast sample 3 is completely matte and not burned.

[0115] The low-temperature bright digital ink prepared by the application is compared with the contrast sample 4 burned at 800 DEG C, the gloss of the example 1 is 82.1 degrees, and the example 1 is completely burned. The gloss of the contrast sample 4 is 1.4 degrees, and the contrast sample 4 is completely matte and not burned.

[0116] As shown in Table 1, the low-temperature bright digital ink prepared by the application can be applied to 800 DEG C burning.

[0117] The application provides a bright digital ink applied to 800 DEG C burning and a preparation method thereof, the bright digital ink prepared by the application can be well applied to 800 DEG C secondary burning of ceramic tiles, and the added value of the ceramic tiles can be better improved.

[0118] The above only describes the preferred embodiments of the application, and it should be noted that, for ordinary skilled in the art, the embodiments can be changed, modified, replaced and changed without departing from the technical principles of the application, and the changes, modifications, replacements and changes should be considered as the protection scope of the application.

Claims

1. A glossy digital ink suitable for firing at 800℃, characterized in that, It is composed of the following components by weight percentage: 25-50% low-temperature frit powder, 2-10% superdispersant, 0-2% defoamer, and 40-60% solvent; wherein the low-temperature frit powder composition is: 40-65% SiO2, 0-5% Al2O3, 0-5% CaO, 0-5% MgO, 0-5% K2O, 10-25% Na2O, 1-10% TiO2, 1-10% BaO, 0-15% ZnO, and 5-25% B2O3.

2. The glossy digital ink suitable for firing at 800℃ according to claim 1, characterized in that: The low-temperature frit powder needs to be prepared by firing at 1300-1600℃ to form a glass frit according to the following composition: SiO2 40-65%, Al2O3 0-5%, CaO 0-5%, MgO 0-5%, K2O 0-5%, Na2O 10-25%, TiO2 1-10%, BaO 1-10%, ZnO 0-15%, B2O3 5-25%. After being cooled by water quenching, it is ground to a fineness of less than 1250 mesh.

3. The glossy digital ink suitable for firing at 800℃ according to claim 1, characterized in that: The superdispersant is one or a mixture of several types of superdispersants, including polyester-type superdispersants, polyurethane-type superdispersants, polyamide-type superdispersants, and polyacrylate-type superdispersants.

4. The glossy digital ink suitable for firing at 800℃ according to claim 1, characterized in that, The defoamer is one or a mixture of several organosilicon defoamers or polyether defoamers.

5. The glossy digital ink suitable for firing at 800℃ according to claim 1, characterized in that, The solvent is one or a mixture of several of the following: isopropyl laurate, isooctyl cocoate, isooctyl palmitate, myristate, methyl oleate, butyl oleate, methyl laurate, low-polarity alkane solvents ToTal 25-28H, 30-36H, 30-38H, 35-40H, n-undecane, n-dodecane, n-decane, and 5-methyldecane.

6. The method for preparing glossy digital ink suitable for firing at 800°C according to any one of claims 1 to 5, characterized in that, Includes the following steps: Step 1: Mix the solvent, superdispersant, and defoamer to prepare a dispersion; Step 2: Add 50-60% of the low-temperature frit powder to 40-50% of the dispersion liquid, and grind it in stages using a horizontal sand mill; Step 3: In the first stage, 0.35-0.45mm zirconium beads are used for grinding. The speed is 50-90% of the maximum speed of the sand mill, the zirconium bead filling rate is 70-90%, and the ink is ground until it reaches a certain particle size and viscosity. Step 4: In the second stage, 0.2-0.25mm zirconium beads are used for grinding. The speed is 50-90% of the maximum speed of the sand mill, the zirconium bead filling rate is 70-90%, and the ink is ground until it reaches a certain particle size and viscosity. Step 5: In the third stage, 0.1-0.15mm zirconium beads are used for grinding. The speed is 50-90% of the maximum speed of the sand mill, the zirconium bead filling rate is 70-90%, and the grinding is continued until the ink reaches a certain particle size and viscosity, and the filtration performance meets certain requirements. Step Six: Add a certain proportion of solvent, defoamer, etc. to the ground ink slurry to adjust it to the required solid content and viscosity. After multi-stage filtration, a glossy digital ink suitable for firing at 800℃ is obtained.

7. The method for preparing glossy digital ink according to claim 6, characterized in that, In step three, the ink particles are ground using a sand mill until the particle size D50 is less than 700 nm. The particle size analyzer used is Omec, and the viscosity at 40°C is less than 500 cp. The viscometer used is Brookfield.

8. The method for preparing glossy digital ink according to claim 6, characterized in that, In step four, the ink particles are ground using a sand mill until the particle size D50 is less than 650 nm. The particle size analyzer used is Omec, and the viscosity at 40°C is less than 500 cp. The viscometer used is Brookfield.

9. The method for preparing glossy digital ink according to claim 6, characterized in that, In step five, the ink particles are ground using a sand mill until the particle size D50 is less than 650 nm. The particle size analyzer used is Omec. The viscosity at 40°C is less than 500 cp. The viscometer used is Brookfield. The ink is filtered using a Corbett glass fiber filter, and the filtered volume is greater than 200 grams.

10. The method for preparing glossy digital ink according to claim 6, characterized in that, In step six, after the prepared ink is mixed, it is filtered through multiple 1μm filter cartridges, and then packaged to obtain a glossy digital ink suitable for firing at 800℃.

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