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CN113735441A - Digital glaze for ceramic large plate or rock plate and preparation method thereof - Google Patents

Digital glaze for ceramic large plate or rock plate and preparation method thereof Download PDF

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Publication number
CN113735441A
CN113735441A CN202110975353.3A CN202110975353A CN113735441A CN 113735441 A CN113735441 A CN 113735441A CN 202110975353 A CN202110975353 A CN 202110975353A CN 113735441 A CN113735441 A CN 113735441A
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parts
digital glaze
powder
glaze
digital
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李杜鹃
张立
罗锡才
李助军
郑毅
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Guangzhou Railway Polytechnic
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Guangzhou Railway Polytechnic
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions

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Abstract

本发明涉及一种陶瓷大板或岩板的数码釉及其制备方法。该数码釉的组分及各组分的质量份数包括,长石10‑40份、高岭土5‑15份、硅灰粉2‑10份、二氧化锆2‑15份、溶剂40‑70份、分散剂2‑10份,以及助溶剂0‑15份。该数码釉具有白度高、遮盖力强、不滴墨、不拉线,稳定性极好、过滤性能更加优异的特点。该数码釉耐高温性能明显增强,固含量相较于传统的釉料具有显著的提高。该数码釉特别适用于陶瓷大板及岩板,不仅节省用料,而且能够更加突出陶瓷板或岩板优势的特点。

Figure 202110975353

The invention relates to a digital glaze of a large ceramic slab or a rock slab and a preparation method thereof. The components of the digital glaze and the parts by mass of each component include 10-40 parts of feldspar, 5-15 parts of kaolin, 2-10 parts of silica fume, 2-15 parts of zirconium dioxide, and 40-70 parts of solvent , 2-10 parts of dispersant, and 0-15 parts of co-solvent. The digital glaze has the characteristics of high whiteness, strong covering power, no ink dripping, no thread pulling, excellent stability and better filtering performance. The high temperature resistance of the digital glaze is obviously enhanced, and the solid content is significantly improved compared with the traditional glaze. The digital glaze is especially suitable for large ceramic slabs and slate slabs, which not only saves materials, but also highlights the advantages of ceramic slabs or slate slabs.

Figure 202110975353

Description

Digital glaze for ceramic large plate or rock plate and preparation method thereof
Technical Field
The invention relates to the technical field of ceramic digital ink-jet, in particular to digital glaze for a ceramic large plate or rock plate and a preparation method thereof.
Background
With the recent rise of ceramic ink-jet technology in the ceramic industry, a plurality of ceramic factories such as marcoboro, Mona Lisa and Xinming pearl introduce ceramic digital ink-jet printers, and high-end ceramic plates all adopt the digital ink-jet technology to replace the traditional printing process. In 2021, the hot tide of ceramic large plates and rock plates is raised in the industry, and dozens of large plate production lines are added in China during one year. At present, the definition of the rock plate in the industry is not unified, and no matter the blank, the glaze, the toughness, the process or the size, the unified standard does not exist at present, so that the rock plate is called by the existing enterprise, and the ceramic large plate is called by the existing enterprise.
The concept of the digital glaze is not released in the last year of exhibition, and is put forward in the international ceramic exhibition held in Guangzhou in 2017 for the first time, but the digital glaze is high in price at present, and only high-end ceramic plates can use the ink-jet printing technology, so that the ink-jet printing technology is required in the market, and the digital glaze which mainly has special functions in the market is high in price at present, and is only expected to play a role of adding flowers to the market, so that the digital glaze is difficult to have a huge market.
Returning to the nature of decoration, the future of the 'digital glaze' can be easily seen. The digital glaze as a solid-liquid mixture replaces pigments, printing oil, printing glaze and other additives, and can directly manufacture the required colors and patterns. The function and effect of the glaze, in contrast, determines that most glazes need to be covered with sufficient area and thickness, and the current glazing process can achieve these requirements precisely and with high adjustability.
However, no digital glaze suitable for ceramic slabs or rock slabs has been released in the market. The ink-jet thickness of the existing ceramic large plate and rock plate must reach 100g/m2Thus, a good covering power can be ensured and sufficient whiteness can be displayed. The current ink-jet printer nozzle aperture is generally 15-25um, the ink-jet quantity is small, and the thickness of the glaze spraying surface is very thin. Thus, for the traditional glaze, the whiteness and the covering power are difficult to have, and the problems of low coloring quality and poor pattern effect are caused.
Disclosure of Invention
The invention aims to provide a digital glaze for ceramic large plates or rock plates and a preparation method thereof.
The technical scheme for solving the technical problems is as follows:
the invention provides a digital glaze for a ceramic large plate or a rock plate, which comprises, by mass, 10-40 parts of feldspar, 5-15 parts of kaolin, 2-10 parts of silica fume powder, 2-15 parts of zirconium dioxide, 40-70 parts of a solvent, 2-10 parts of a dispersant and 0-15 parts of a cosolvent.
Further, the digital glaze comprises 15-25 parts of feldspar, 8-12 parts of kaolin, 5-8 parts of wollastonite powder, 3-12 parts of zirconium dioxide, 45-60 parts of solvent, 3-8 parts of dispersant and 0-5 parts of cosolvent.
Further, the digital glaze comprises 15 parts of feldspar, 8 parts of kaolin, 5 parts of wollastonite powder, 12 parts of zirconium dioxide, 45 parts of solvent, 8 parts of dispersant and 7 parts of cosolvent.
Further, the feldspar is one of potassium feldspar or albite.
The invention provides a preparation method of the ceramic large plate and rock plate digital glaze, which comprises the following steps:
s1), performing ball milling treatment on the feldspar, the kaolin, the wollastonite powder and the zirconium dioxide powder respectively, and sieving the treated materials respectively;
s2), drying the powder sieved in the step S1);
s3), adding the powder materials dried in the step S2) into different high-speed mixers respectively for mixing, pumping the mixed powder materials into different sand mills respectively for sanding, and obtaining a feldspar pre-mixture, the kaolin pre-mixture, the wollastonite powder pre-mixture and the zirconium dioxide pre-mixture respectively;
s4), adding the solvent, the dispersant and the cosolvent into a high-speed stirrer in sequence according to the mass parts of the components, and mixing and stirring to obtain mixed slurry;
s5), putting the mixed slurry obtained in the step S4) into a high-speed dispersion machine, mixing the premixes obtained in the step S3) according to the mass parts of the components, adding the premixes into the high-speed dispersion machine after mixing, mixing the premixes with the mixed slurry, and dispersing the premixes at a high speed;
s6), filtering the mixture obtained in the step S5) by a four-stage filter vehicle to obtain the digital glaze after filtering.
Further, in the step S1), the ball milling time is 30-40 min; after the ball milling treatment, D50 of each powder is less than 1.5 um.
Further, in the step S1), each of the powder materials after the ball milling process passes through a 250-400-mesh screen.
Further, in the step S2), the drying temperature is 60 to 110 ℃, and the water content of each powder after drying is less than 0.1%.
Further, in the step S3), the mixing time of each powder material in the high-speed mixer is 15-25min, and the rotating speed is 60-150 r/min; the sanding time of each powder in the sand mill is 2-48h, after sanding, the D50 of each powder is 200-500nm, and the D90 is less than 1.2 um.
Further, in step S6), the filter pore size of the four-stage filter vehicle is 10um, 5um, 1um and 1um in sequence.
The invention has the following beneficial effects:
1) the digital glaze disclosed by the invention is higher in whiteness, stronger in covering power and more excellent in color performance, so that the thickness of sprayed glaze is thinner, and the whiteness can be kept at an extremely low glazing thickness; the ink is suitable for various common digital ceramic printers, and has the advantages of high whiteness, strong covering power, no ink drop, no wire drawing and excellent stability.
2) The digital glaze provided by the invention has the advantages that the average particle size is smaller, the particle morphology is closer to a sphere-like shape, the sphere is more stable, and the filtering performance is more excellent.
3) The high-temperature resistance of the digital glaze is obviously enhanced, and the solid content of the digital glaze is obviously improved compared with that of the traditional glaze.
4) According to the preparation method of the digital glaze, the four-stage filter vehicle is used for filtering in multiple stages, so that the digital glaze is better in compatibility and is not easy to drip ink, particles in a product finally obtained by filtering are in a standard range, a filter of an ink-jet printer cannot be blocked, and the storage time is longer.
5) The digital glaze of the invention also has the characteristics of saving raw materials and better highlighting the advantages of the ceramic plate or the rock plate.
Drawings
FIG. 1 is a particle microscopic view of the digital glaze of example 1 of the present invention, at a magnification of 2 ten thousand;
fig. 2 is a particle microscopic view of the digital glaze of example 1 of the present invention, at a magnification of 1 ten thousand.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
The ceramic large plate and rock plate digital glaze comprises, by mass, 10-40 parts of feldspar, 5-15 parts of kaolin, 2-10 parts of wollastonite powder, 2-15 parts of zirconium dioxide, 40-70 parts of a solvent, 2-10 parts of a dispersing agent and 0-15 parts of a cosolvent.
Preferably, the digital glaze comprises, by mass, 15-25 parts of feldspar, 8-12 parts of kaolin, 5-8 parts of wollastonite powder, 3-12 parts of zirconium dioxide, 45-60 parts of a solvent, 3-8 parts of a dispersant and 0-5 parts of a cosolvent.
More preferably, the components of the digital glaze and the parts by mass of the components comprise 15 parts of feldspar, 8 parts of kaolin, 5 parts of wollastonite powder, 12 parts of zirconium dioxide, 45 parts of solvent, 8 parts of dispersant and 7 parts of cosolvent.
In the digital glaze, potassium feldspar and albite are added; feldspar is an aluminosilicate mineral containing calcium, sodium and potassium. Common feldspar comprises potassium feldspar, albite, anorthite and celsian, and the potassium feldspar and the albite adopted by the invention are rich in potassium or sodium and are feldspar mainly used in ceramic industry.
Therefore, potassium feldspar or potassium feldspar that is pure white or pure white transparent is preferred. The prepared glaze has less impurities and high whiteness.
Preferably, the solvent is one or more of white oil, mineral oil and diesel oil; it is further preferred that the solvent is not white oil, and the white oil is not limited to one reference number and may be a mixture of any ratio of a plurality of reference numbers, such as a mixture of white oil number 5# and white oil number 7# in any ratio.
Preferably, the dispersing agent is one or a mixture of more of Span80, Span65, Span60, simethicone (50cp), glycerol polyoxyethylene ether and polyethylene glycol.
Preferably, the cosolvent is one of stearic acid polyoxyethylene ether, palmitate, oleic acid, oleylamine and lauric acid.
The preparation method of the ceramic large plate and rock plate digital glaze comprises the following steps:
s1), performing ball milling treatment on the powder of the industrial feldspar containing potassium and sodium, the kaolin, the wollastonite powder and the zirconium dioxide respectively, and sieving the treated powder respectively.
The ball milling treatment time is 30-40 min; after ball milling treatment, D50 of each powder is less than 1.5 um.
Passing each powder after ball milling treatment through a 250-400-mesh screen.
S2), drying the powder sieved in the step S1) by blast air at 60-110 ℃ in an oven until the water content of two samples is less than 0.1% to obtain four kinds of crushed and dried pretreated powder of mineral aggregate.
S3), adding the powder materials dried in the step S2) into a high-speed mixer respectively, mixing, pumping into a sand mill, and sanding to obtain a feldspar pre-mixture, a kaolin pre-mixture, a wollastonite powder pre-mixture and a zirconium dioxide pre-mixture respectively.
Mixing the powder materials in a high-speed mixer for 15-25min at a rotating speed of 60-150 rpm until no obvious bottom precipitation exists at the bottom; the sanding time of each powder in the sand mill is 2-48h, after sanding, the D50 of each powder is 200-500nm, and the D90 is less than 1.2 um.
Preferably, the rotating speed of the high-speed mixer is 60-90 revolutions per minute.
S4), sequentially adding the solvent, the dispersant and the cosolvent into a high-speed stirrer, and mixing and stirring for 15-45min to obtain mixed slurry.
S5), putting the mixed slurry obtained in the step S4) into a high-speed dispersion machine, mixing the premixes obtained in the step S3) according to the mass parts of the components, adding the mixture into the high-speed dispersion machine after mixing, and mixing and stirring the mixture and the mixed slurry for 15-45min at the rotating speed of 60-150 r/min.
Preferably, the rotating speed of the high-speed dispersion machine is 60-90 r/min.
S6), filtering the mixture obtained in the step S5) by a four-stage filter vehicle to obtain digital glaze after filtering; the filtration aperture of the four-stage filter vehicle is 10um, 5um, 1um and 1um in sequence.
The effects of the digital glaze of the present invention are compared and illustrated by examples and comparative examples below.
It is to be noted that in the following examples, the specific chemical compositions of the solvent, the dispersant and the co-solvent have no substantial influence on the properties of the digital glaze, and therefore the specific chemical compositions adopted by the solvent, the dispersant and the co-solvent are not specifically described in each example.
Example 1
This example is a standard example for comparison, and the specific composition and preparation method are as follows:
the digital glaze special for the ceramic large plate and the rock plate comprises the following raw materials in parts by weight: 15 parts of feldspar (containing potassium and albite), 8 parts of kaolin, 5 parts of wollastonite powder, 12 parts of zirconium dioxide, 45 parts of solvent, 8 parts of dispersant and 7 parts of cosolvent.
The specific preparation method of the digital glaze special for the ceramic large plate and the rock plate comprises the following steps:
s1), performing ball milling treatment on the powder of the industrial feldspar containing potassium and sodium, the kaolin, the wollastonite powder and the zirconium dioxide respectively, and sieving the treated powder respectively.
The ball milling time is 30 min; after ball milling treatment, D50 of each powder is less than 1.5 um.
And screening the powder subjected to ball milling treatment by a 400-mesh screen.
S2), drying the powder sieved in the step S1) by blast air at 105 ℃ in an oven until the water content of the two samples is less than 0.1 percent, and obtaining the crushed and dried pretreated powder of four mineral aggregates.
S3), adding the powder materials dried in the step S2) into a high-speed mixer respectively, mixing, pumping into a sand mill, and sanding to obtain a feldspar pre-mixture, a kaolin pre-mixture, a wollastonite powder pre-mixture and a zirconium dioxide pre-mixture respectively.
Mixing the powder materials in the high-speed mixer for 15min until no obvious bottom precipitation exists at the bottom; the sanding time of each powder in the sanding machine is 2-48h, after sanding, the D50 of each powder is 300nm, and the D90 is less than 0.85 um.
S4), sequentially adding the solvent, the dispersant and the cosolvent into a high-speed stirrer, and mixing and stirring for 30min to obtain mixed slurry;
s5), putting the mixed slurry obtained in the step S4) into a high-speed dispersion machine, mixing the premixes obtained in the step S3) for 45min according to the mass parts of the components, adding the mixture into the high-speed dispersion machine after mixing, and mixing the mixture with the mixed slurry;
s6), filtering the mixture obtained in the step S5) by a four-stage filter vehicle to obtain digital glaze after filtering; the filtration aperture of the four-stage filter vehicle is 10um, 5um, 1um and 1um in sequence.
Example 2
This example is an example where no co-solvent is added and the solvent content is increased accordingly, in the composition of this example, the zirconium dioxide content is reduced and the feldspar content is increased accordingly. The concrete composition and the preparation method are as follows:
the digital glaze special for the ceramic large plate and the rock plate comprises the following raw materials in parts by weight: 24 parts of feldspar (containing potassium and albite), 8 parts of kaolin, 5 parts of wollastonite powder, 3 parts of zirconium dioxide, 52 parts of solvent, 8 parts of dispersant and 0 part of cosolvent.
The specific preparation method of the digital glaze special for the ceramic large plate and the rock plate comprises the following steps:
s1), performing ball milling treatment on the powder of the industrial feldspar containing potassium and sodium, the kaolin, the wollastonite powder and the zirconium dioxide respectively, and sieving the treated powder respectively.
The ball milling time is 30 min; after ball milling treatment, D50 of each powder is less than 1.5 um.
And screening the powder subjected to ball milling treatment by a 400-mesh screen.
S2), drying the powder sieved in the step S1) by blast air at 105 ℃ in an oven until the water content of the two samples is less than 0.1 percent, and obtaining the crushed and dried pretreated powder of four mineral aggregates.
S3), adding the powder materials dried in the step S2) into a high-speed mixer respectively, mixing, pumping into a sand mill, and sanding to obtain a feldspar pre-mixture, a kaolin pre-mixture, a wollastonite powder pre-mixture and a zirconium dioxide pre-mixture respectively.
Mixing the powder materials in the high-speed mixer for 15min until no obvious bottom precipitation exists at the bottom; the sanding time of each powder in the sanding machine is 2-48h, after sanding, the D50 of each powder is 300nm, and the D90 is less than 0.85 um.
S4), sequentially adding the solvent, the dispersant and the cosolvent into a high-speed stirrer, and mixing and stirring for 30min to obtain mixed slurry;
s5), putting the mixed slurry obtained in the step S4) into a high-speed dispersion machine, mixing the premixes obtained in the step S3) for 45min according to the mass parts of the components, adding the mixture into the high-speed dispersion machine after mixing, and mixing the mixture with the mixed slurry;
s6), filtering the mixture obtained in the step S5) by a four-stage filter vehicle to obtain digital glaze after filtering; the filtration aperture of the four-stage filter vehicle is 10um, 5um, 1um and 1um in sequence.
Example 3
This example reduces the dispersant content and correspondingly increases the solvent content. The concrete composition and the preparation method are as follows:
the digital glaze special for the ceramic large plate and the rock plate comprises the following raw materials in parts by weight: 15 parts of feldspar (containing potassium and albite), 8 parts of kaolin, 5 parts of wollastonite powder, 12 parts of zirconium dioxide, 49 parts of solvent, 4 parts of dispersant, 7 parts of cosolvent,
The specific preparation method of the digital glaze special for the ceramic large plate and the rock plate comprises the following steps:
s1), performing ball milling treatment on the powder of the industrial feldspar containing potassium and sodium, the kaolin, the wollastonite powder and the zirconium dioxide respectively, and sieving the treated powder respectively.
The ball milling time is 30 min; after ball milling treatment, D50 of each powder is less than 1.5 um.
And screening the powder subjected to ball milling treatment by a 400-mesh screen.
S2), drying the powder sieved in the step S1) by blast air at 105 ℃ in an oven until the water content of the two samples is less than 0.1 percent, and obtaining the crushed and dried pretreated powder of four mineral aggregates.
S3), adding the powder materials dried in the step S2) into a high-speed mixer respectively, mixing, pumping into a sand mill, and sanding to obtain a feldspar pre-mixture, a kaolin pre-mixture, a wollastonite powder pre-mixture and a zirconium dioxide pre-mixture respectively.
Mixing the powder materials in the high-speed mixer for 15min until no obvious bottom precipitation exists at the bottom; the sanding time of each powder in the sanding machine is 2-48h, after sanding, the D50 of each powder is 300nm, and the D90 is less than 0.85 um.
S4), sequentially adding the solvent, the dispersant and the cosolvent into a high-speed stirrer, and mixing and stirring for 30min to obtain mixed slurry;
s5), putting the mixed slurry obtained in the step S4) into a high-speed dispersion machine, mixing the premixes obtained in the step S3) for 45min according to the mass parts of the components, adding the mixture into the high-speed dispersion machine after mixing, and mixing the mixture with the mixed slurry;
s6), filtering the mixture obtained in the step S5) by a four-stage filter vehicle to obtain digital glaze after filtering; the filtration aperture of the four-stage filter vehicle is 10um, 5um, 1um and 1um in sequence.
Example 4
The water content of this example exceeded the standard to about 1.5%. The concrete composition and the preparation method are as follows:
the digital glaze special for the ceramic large plate and the rock plate comprises the following raw materials in parts by weight:
15 parts of feldspar (containing potassium and albite), 8 parts of kaolin, 5 parts of wollastonite powder, 12 parts of zirconium dioxide, 45 parts of solvent, 8 parts of dispersant and 7 parts of cosolvent.
The specific preparation method of the digital glaze special for the ceramic large plate and the rock plate comprises the following steps:
s1), performing ball milling treatment on the powder of the industrial feldspar containing potassium and sodium, the kaolin, the wollastonite powder and the zirconium dioxide respectively, and sieving the treated powder respectively.
The ball milling time is 30 min; after ball milling treatment, D50 of each powder is less than 1.5 um.
And screening the powder subjected to ball milling treatment by a 400-mesh screen.
S2), drying the powder sieved in the step S1) by blast air at 105 ℃ in an oven until the water content of the two samples is less than 0.1 percent, and obtaining the crushed and dried pretreated powder of four mineral aggregates.
S3), adding the powder materials dried in the step S2) into a high-speed mixer respectively, mixing, pumping into a sand mill, and sanding to obtain a feldspar pre-mixture, a kaolin pre-mixture, a wollastonite powder pre-mixture and a zirconium dioxide pre-mixture respectively.
Mixing the powder materials in the high-speed mixer for 15min until no obvious bottom precipitation exists at the bottom; the sanding time of each powder in the sanding machine is 2-48h, after sanding, the D50 of each powder is 300nm, and the D90 is less than 0.85 um.
S4), sequentially adding the solvent, the dispersant and the cosolvent into a high-speed stirrer, and mixing and stirring for 30min to obtain mixed slurry;
s5), putting the mixed slurry obtained in the step S4) into a high-speed dispersion machine, mixing the premixes obtained in the step S3) for 45min according to the mass parts of the components, adding the mixture into the high-speed dispersion machine after mixing, and mixing the mixture with the mixed slurry;
s6), filtering the mixture obtained in the step S5) by a four-stage filter vehicle to obtain digital glaze after filtering; the filtration aperture of the four-stage filter vehicle is 10um, 5um, 1um and 1um in sequence.
Example 5
In this embodiment, the sanding particles are controlled to be greater than 50%. The concrete composition and the preparation method are as follows:
the digital glaze special for the ceramic large plate and the rock plate comprises the following raw materials in parts by weight: 15 parts of feldspar (containing potassium and albite), 8 parts of kaolin, 5 parts of wollastonite powder, 12 parts of zirconium dioxide, 45 parts of solvent, 8 parts of dispersant and 7 parts of cosolvent.
The specific preparation method of the digital glaze special for the ceramic large plate and the rock plate comprises the following steps:
s1), performing ball milling treatment on the powder of the industrial feldspar containing potassium and sodium, the kaolin, the wollastonite powder and the zirconium dioxide respectively, and sieving the treated powder respectively.
The ball milling time is 30 min; after ball milling treatment, D50 of each powder is less than 1.5 um.
And screening the powder subjected to ball milling treatment by a 400-mesh screen.
S2), drying the powder sieved in the step S1) by blast air at 105 ℃ in an oven until the water content of the two samples is less than 0.1 percent, and obtaining the crushed and dried pretreated powder of four mineral aggregates.
S3), adding the powder materials dried in the step S2) into a high-speed mixer respectively, mixing, pumping into a sand mill, and sanding to obtain a feldspar pre-mixture, a kaolin pre-mixture, a wollastonite powder pre-mixture and a zirconium dioxide pre-mixture respectively.
Mixing the powder materials in the high-speed mixer for 15min until no obvious bottom precipitation exists at the bottom; the sanding time of each powder in the sanding machine is 2-48h, after sanding, the D50 of each powder is 300nm, and the D90 is less than 1.7 um.
S4), sequentially adding the solvent, the dispersant and the cosolvent into a high-speed stirrer, and mixing and stirring for 30min to obtain mixed slurry;
s5), putting the mixed slurry obtained in the step S4) into a high-speed dispersion machine, mixing the premixes obtained in the step S3) for 45min according to the mass parts of the components, adding the mixture into the high-speed dispersion machine after mixing, and mixing the mixture with the mixed slurry;
s6), filtering the mixture obtained in the step S5) by a four-stage filter vehicle to obtain digital glaze after filtering; the filtration aperture of the four-stage filter vehicle is 10um, 5um, 1um and 1um in sequence.
Example 6
This example did not pass through the fourth stage vehicle filter. The concrete composition and the preparation method are as follows:
the digital glaze special for the ceramic large plate and the rock plate comprises the following raw materials in parts by weight:
15 parts of feldspar (containing potassium and albite), 8 parts of kaolin, 5 parts of wollastonite powder, 12 parts of zirconium dioxide, 45 parts of solvent, 8 parts of dispersant and 7 parts of cosolvent.
The specific preparation method of the digital glaze special for the ceramic large plate and the rock plate comprises the following steps:
s1), performing ball milling treatment on the powder of the industrial feldspar containing potassium and sodium, the kaolin, the wollastonite powder and the zirconium dioxide respectively, and sieving the treated powder respectively.
The ball milling time is 30 min; after ball milling treatment, D50 of each powder is less than 1.5 um.
And screening the powder subjected to ball milling treatment by a 400-mesh screen.
S2), drying the powder sieved in the step S1) by blast air at 105 ℃ in an oven until the water content of the two samples is less than 0.1 percent, and obtaining the crushed and dried pretreated powder of four mineral aggregates.
S3), adding the powder materials dried in the step S2) into a high-speed mixer respectively, mixing, pumping into a sand mill, and sanding to obtain a feldspar pre-mixture, a kaolin pre-mixture, a wollastonite powder pre-mixture and a zirconium dioxide pre-mixture respectively.
Mixing the powder materials in the high-speed mixer for 15min until no obvious bottom precipitation exists at the bottom; the sanding time of each powder in the sanding machine is 2-48h, after sanding, the D50 of each powder is 300nm, and the D90 is less than 0.85 um.
S4), sequentially adding the solvent, the dispersant and the cosolvent into a high-speed stirrer, and mixing and stirring for 30min to obtain mixed slurry;
s5), putting the mixed slurry obtained in the step S4) into a high-speed dispersion machine, mixing the premixes obtained in the step S3) for 45min according to the mass parts of the components, adding the mixture into the high-speed dispersion machine after mixing, and mixing the mixture with the mixed slurry; the finished product of the digital glaze is directly obtained without filtering by a four-stage filter vehicle.
The physical and chemical properties and the actual ink-jet effect of each of the above examples 1 to 6 and the commercial digital glaze were compared.
1. Comparison of physicochemical Properties
The digital glazes of examples 1 to 6 and a commercially available common digital glaze (comparative example) were applied to the same ceramic green sheet and after uniformly sintering under the same conditions, the comparative test results are shown in table 1:
TABLE 1 comparison of physicochemical Properties of the digital glazes of examples 1 to 6 with those of comparative examples
Figure BDA0003227455410000121
Figure BDA0003227455410000131
As can be seen from the data in table 1, examples 1-6 have the following advantages compared to the comparative example:
1) in the digital glaze of embodiments 1-6, the average particle size is smaller, the particle morphology is closer to a sphere-like shape, the sphere is more stable, and the filtering performance is more excellent, benefiting from a series of pretreatment such as ball milling crushing, sieving and forced air drying of the mineral powder in the early stage.
2) The digital glaze of the embodiments 1 to 6 has significantly enhanced high temperature resistance, and the digital glaze is more stable and resistant to high temperature owing to the addition of zirconium dioxide in the formula.
3) The effective component in the digital glaze of the embodiments 1 to 6, namely the solid content, is obviously higher, so that the selection of the solvent, the cosolvent and the dispersant in the formula is more excellent, and the proportion is more reasonable.
2. Comparison of actual ink-jet effects
The digital glazes of examples 1 to 6 and the commercial common digital glaze (comparative example) were characterized and analyzed, and the specific results are shown in table 2:
TABLE 2 actual ink-jet effect of digital glaze applied to ceramic large plate and rock plate production
Figure BDA0003227455410000132
Figure BDA0003227455410000141
As can be seen from the test results in Table 2, examples 1-6 have the advantages of:
1) the covering power of the embodiment 1-6 is stronger, the color performance is more excellent, so that the thickness of glaze spraying is thinner, raw materials can be effectively saved, and the advantages of the rock plate are more prominent.
2) The digital glaze, the ceramic large plate and the rock plate in the embodiments 1-6 have better compatibility, are not easy to drip ink, benefit from the fact that the digital glaze post-treatment is subjected to multi-stage filtration by a four-stage filter vehicle, ensure that particles in a product finally obtained by filtration are in a standard range, prevent the filter of an ink-jet printer from being blocked, and have longer storage time.
3) The digital glaze of the embodiments 1 to 6 has higher whiteness, can ensure that the whiteness can be maintained under the condition of extremely low glazing thickness, and is benefited by adding zirconium dioxide in the formula.
As can be seen from the comparative tests, the digital glaze of the embodiments 1 to 6 of the scheme has significant advantages compared with the products sold on the market.
The digital glaze of example 1 was subjected to particle microscopic analysis and performance measurement to further demonstrate the composite use standard of the digital glaze of the present scheme.
(1) Particle microstructure analysis
The particle microstructure of the digital glaze of example 1 was analyzed using a scanning electron microscope. The test instrument used was a Korea Seisakusho scanning electron microscope SEM-4500M.
The microstructure analysis procedure of the digital glaze particles of example 1: pretreating the digital glaze, drying the solvent, spraying the dried solvent on the conductive adhesive, and placing the conductive adhesive in a gold plating box for gold plating; sequentially starting a computer, starting a scanning electron microscope SEM-4500M and software, and then loading the processed sample; vacuumizing, and then primarily adjusting the orientation X, Y, R of the test bench to find the position of the sample; fine tuning X, Y the orientation of the test station on the software to find the particular sub-microscopic structure to be observed; and photographing and storing the data in a specified folder, recording the data, shutting down the computer, and taking out the sample.
The results of the tests are shown in figures 1 and 2. As can be seen from the figures 1 and 2, the digital glaze powder of the embodiment 1 has regular particle shapes, is elliptical and spherical, has the particle size of 0.3-1.1um after being dried, and meets the requirements of the shape and the particle size.
(2) Particle size testing
The particle size test method is a dynamic laser scattering method, and the adopted instrument is a laser particle size analyzer. The particle size testing process comprises the following steps: starting up and starting up the computer and cleaning equipment by using a specified solvent; selecting the type and name of the test particles; diluting the digital glaze sample by 10 times, and carrying out ultrasonic treatment for 2min for later use; clicking 'start test', dropping a proper amount of diluted digital glaze pigment until the indication bar is in a green area when 'please drop the sample' appears in the computer; wait for 30s, read the results, and the test results are shown in table 3:
table 3 example 1 particle size test results for digital glaze
Test items Unit of Results Limit value Conclusion
Digital glaze particle size (D50, first time) um 0.304 X<0.80 Conform to
Digital glaze particle size (D50, second time) um 0.315 X<0.80 Conform to
Digital glaze particle size (D50, third time) um 0.303 X<0.80 Conform to
Mean value of um 0.307 X<0.80 Conform to
Digital glaze particle size (D90, first time) um 0.884 X<2.00 Conform to
Digital glaze particle size (D90, second time) um 0.822 X<2.00 Conform to
Digital glaze particle size (D90, third time) um 0.841 X<2.00 Conform to
Mean value of um 0.856 X<2.00 Conform to
Note: d50, wherein the particle size of 50 percent of particles is less than the particle size; d90: the particle size of 90% of the particles is below this size.
(3) Digital glaze viscosity test
The viscosity of the digital glaze is measured by a rotary viscosity meter, and the measuring method comprises the following steps: placing the sample in a clean plastic cup, controlling the temperature of the sample, selecting a proper rotor and rotating speed when the temperature is stabilized at 25 ℃, inserting the rotor into the sample to be tested, enabling the liquid level of the sample to be just in contact with the groove in contact with the rotor, starting the viscometer, and recording the reading v when the dial is stabilized. The viscosity number is obtained from the formula μ ═ vc and is expressed in mPa · s. The viscometer viscosity index is shown in Table 4 and the test results are shown in Table 5.
TABLE 4 viscometer viscosity coefficient Table
Figure BDA0003227455410000161
The viscosity of the digital glaze is generally in the range of 15-30 mPa.s, a 1# rotor is selected, and the rotating speed is 1.5 or 3.
(4) Determination of solid content of digital glaze
The solid content of the digital glaze refers to the proportion of the effective components except the solvent and all the auxiliary agents in the digital glaze. The determination method comprises the steps of weighing and drying a clean aluminum plate W1 (the precision is 0.1mg, the same below), adding 3-5 g of ceramic ink into the aluminum plate, weighing the mass mg, then placing the aluminum plate into a constant-temperature oven at 500 ℃ for drying for 2h, taking out the aluminum plate, weighing the weight of the aluminum plate as W2, and calculating the solid content according to the following formula:
Figure BDA0003227455410000162
in the formula: w1 is empty disc mass, unit is g; m is the sample mass in g; w2 is the weight of the dried empty plate, and the unit is g.
The test results are shown in table 5.
(5) Digital glaze ink-jet test: the test results are shown in table 5.
(6) Testing the storage stability of the digital glaze: the test method is free settling at 25 ℃, and the test standard is that the test method is that after shaking for 30min by a swinging machine, the test method is kept still for one day, and the amount of the precipitated pigment is more than 5 wt%. The test results are shown in table 5.
TABLE 5 digital glaze viscosity, solid content, ink jet test and storage stability test results
Figure BDA0003227455410000171
As can be seen from the tests, the performance of the digital glaze in all aspects of the scheme meets the use standard, and therefore the digital glaze can meet the existing market demand.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1.一种陶瓷大板或岩板的数码釉,其特征在于,所述数码釉的组分以质量份数计,组分包括,长石10-40份、高岭土5-15份、硅灰粉2-10份、二氧化锆2-15份、溶剂40-70份、分散剂2-10份,以及助溶剂0-15份。1. the digital glaze of a ceramic slab or slate, is characterized in that, the component of described digital glaze is in parts by mass, and the component comprises, 10-40 parts of feldspar, 5-15 parts of kaolin, silica fume 2-10 parts of powder, 2-15 parts of zirconium dioxide, 40-70 parts of solvent, 2-10 parts of dispersant, and 0-15 parts of cosolvent. 2.根据权利要求1所述一种陶瓷大板或岩板的数码釉,其特征在于,所述数码釉的组分包括,长石15-25份、高岭土8-12份、硅灰粉5-8份、二氧化锆3-12份、溶剂45-60份、分散剂3-8份,以及助溶剂0-5份。2. the digital glaze of a kind of ceramic slab or slate according to claim 1, is characterized in that, the component of described digital glaze comprises, 15-25 parts of feldspar, 8-12 parts of kaolin, 5 parts of silica fume -8 parts, 3-12 parts of zirconium dioxide, 45-60 parts of solvent, 3-8 parts of dispersant, and 0-5 parts of cosolvent. 3.根据权利要求2所述一种陶瓷大板或岩板的数码釉,其特征在于,所述数码釉的组分包括,长石15份、高岭土8份、硅灰粉5份、二氧化锆12份、溶剂45份、分散剂8份、助溶剂7份。3. the digital glaze of a kind of ceramic slab or slate according to claim 2, it is characterized in that, the component of described digital glaze comprises, 15 parts of feldspar, 8 parts of kaolin, 5 parts of silica fume, carbon dioxide 12 parts of zirconium, 45 parts of solvent, 8 parts of dispersant, and 7 parts of cosolvent. 4.根据权利要求1~3任意一项所述一种陶瓷大板或岩板的数码釉,其特征在于,所述长石为钾长石或钠长石中的一种。4 . The digital glaze of a ceramic slab or slate according to any one of claims 1 to 3 , wherein the feldspar is one of potassium feldspar or albite. 5 . 5.一种如权利要求1~4任意一项所述的陶瓷大板或岩板的数码釉的制备方法,其特征在于,包括以下步骤:5. a preparation method of the digital glaze of a large ceramic slab or slate as claimed in any one of claims 1 to 4, is characterized in that, comprises the following steps: S1)、将所述长石、所述高岭土、所述硅灰粉、所述二氧化锆的粉料分别进行球磨处理,处理后分别过筛;S1), the powder material of described feldspar, described kaolin, described silica fume powder, described zirconium dioxide is respectively carried out ball milling treatment, respectively sieves after treatment; S2)、将所述步骤S1)中过筛后的各粉料进行干燥;S2), each powder material after sieving in the described step S1) is dried; S3)、将所述步骤S2)干燥后的各粉料分别加入不同的高混机中进行混合,混合后再分别抽入不同砂磨机中进行砂磨,分别得到长石预混物、所述高岭土预混物、所述硅灰粉预混物以及所述二氧化锆预混物;S3), adding each powder after drying in the step S2) into different high-speed mixers and mixing, respectively, after mixing, pumping into different sand mills for sand grinding, respectively obtaining feldspar premix, all the kaolin premix, the silica fume premix and the zirconium dioxide premix; S4)、按照各组分的质量份数,将所述溶剂、所述分散剂和所述助溶剂依次加入高速搅拌机中混合搅拌,得到混合浆料;S4), according to the mass fraction of each component, the solvent, the dispersant and the cosolvent are successively added to the high-speed mixer for mixing and stirring to obtain a mixed slurry; S5)、将所述步骤S4)得到的所述混合浆料放入高速分散机中,再将所述步骤S3)得到的各所述预混物按照各组分的质量份数混合,混合后加入所述高速分散机中再与所述混合浆料进行混合并高速分散;S5), put the mixed slurry obtained in the step S4) into a high-speed disperser, and then mix the premixes obtained in the step S3) according to the mass fraction of each component, and after mixing Add into the high-speed disperser and then mix with the mixed slurry and disperse at high speed; S6)、将所述步骤S5)得到的混合物通过四级滤车过滤,过滤后得到数码釉。S6), the mixture obtained in the step S5) is filtered through a four-stage filter car, and the digital glaze is obtained after the filtration. 6.根据权利要求5所述一种陶瓷大板或岩板的数码釉的制备方法,其特征在于,所述步骤S1)中,所述球磨处理的时间为30-40min;球磨处理后,各所述粉料的D50小于1.5um。6. the preparation method of the digital glaze of a kind of ceramic slab or slate according to claim 5, is characterized in that, in described step S1), the time of described ball milling is 30-40min; The D50 of the powder is less than 1.5um. 7.根据权利要求5所述一种陶瓷大板或岩板的数码釉的制备方法,其特征在于,所述步骤S1)中,球磨处理后的各所述粉料过250-400目筛网。7. the preparation method of the digital glaze of a kind of ceramic slab or slate according to claim 5, is characterized in that, in described step S1), each described powder after ball milling treatment passes through 250-400 mesh screen . 8.根据权利要求5所述一种陶瓷大板或岩板的数码釉的制备方法,其特征在于,所述步骤S2)中,干燥温度为60-110℃,干燥后各所述粉料的含水量小于0.1%。8. the preparation method of the digital glaze of a kind of ceramic slab or slate according to claim 5, is characterized in that, in described step S2), drying temperature is 60-110 ℃, after drying each described powder material The moisture content is less than 0.1%. 9.根据权利要求5所述一种陶瓷大板或岩板的数码釉的制备方法,其特征在于,所述步骤S3)中,9. the preparation method of the digital glaze of a kind of ceramic slab or slate according to claim 5, is characterized in that, in described step S3), 各所述粉料在所述高混机中的混合时间为15-25min,转速为60~150转/分钟;The mixing time of each of the powders in the high-speed mixer is 15-25 min, and the rotating speed is 60-150 rpm; 各所述粉料在所述砂磨机中的砂磨时间为2-48h,砂磨后,各所述粉料的D50为200-500nm,D90小于1.2um。The sanding time of each of the powders in the sand mill is 2-48h, and after sanding, the D50 of each of the powders is 200-500nm, and the D90 is less than 1.2um. 10.根据权利要求5所述一种陶瓷大板或岩板的数码釉的制备方法,其特征在于,所述步骤S6)中,所述四级滤车的过滤孔径依次为,10um、5um、1um以及1um。10. the preparation method of the digital glaze of a kind of ceramic slab or slate according to claim 5, is characterized in that, in described step S6), the filter aperture of described four-stage filter car is successively, 10um, 5um, 1um and 1um.
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