阅读说明：本技术 一种陶瓷大板或岩板的数码釉及其制备方法 (Digital glaze for ceramic large plate or rock plate and preparation method thereof ) 是由 李杜鹃 张立 罗锡才 李助军 郑毅 于 2021-08-24 设计创作，主要内容包括：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。(The invention relates to a digital glaze for a ceramic large plate or a rock plate and a preparation method thereof. The 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 dispersant and 0-15 parts of a cosolvent. The digital glaze has the characteristics of high whiteness, strong covering power, no ink dripping, no wire drawing, excellent stability and more excellent filtering performance. The high-temperature resistance of the digital glaze is obviously enhanced, and the solid content is obviously improved compared with that of the traditional glaze. The digital glaze is particularly suitable for ceramic slabs and rock slabs, saves materials, and can better highlight the advantages of the ceramic slabs or the rock slabs.)

1. The digital glaze for the ceramic large plate or rock plate is characterized by comprising, 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.

2. The digital glaze for ceramic slabs or rock slabs as claimed in claim 1, wherein 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.

3. The digital glaze for ceramic slabs or rock slabs as claimed in claim 2, wherein 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.

4. The digital glaze for ceramic large plates or rock plates according to any one of claims 1 to 3, wherein the feldspar is one of potassium feldspar or albite.

5. A method for preparing the digital glaze of ceramic slabs or rock slabs according to any one of claims 1 to 4, comprising 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.

6. The method for preparing the digital glaze for ceramic slabs or rock plates according to claim 5, wherein in the step S1), the ball milling time is 30-40 min; after ball milling treatment, D50 of each powder is less than 1.5 um.

7. The method as claimed in claim 5, wherein in step S1), each powder material after ball milling is passed through a 250-400 mesh screen.

8. The method for preparing the digital glaze of ceramic slabs or rock slabs according to claim 5, wherein in the step S2), the drying temperature is 60-110 ℃, and the water content of each powder after drying is less than 0.1%.

9. The method for preparing digital glaze for ceramic slabs or rock boards as claimed in claim 5, wherein in step S3),

the mixing time of the powder materials 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.

10. The method according to claim 5, wherein in step S6), the filter pore size of the four-stage filter vehicle is 10um, 5um, 1um and 1 um.

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

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

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

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:

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

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.