CN113860887B - Ceramic plate and preparation method thereof - Google Patents

Ceramic plate and preparation method thereof Download PDF

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Publication number
CN113860887B
CN113860887B CN202111236192.2A CN202111236192A CN113860887B CN 113860887 B CN113860887 B CN 113860887B CN 202111236192 A CN202111236192 A CN 202111236192A CN 113860887 B CN113860887 B CN 113860887B
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parts
glaze
ceramic plate
dry
green brick
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CN113860887A (en
Inventor
黄春林
仝松贞
徐雪英
朱光耀
陈育昆
谢怡伟
宁毓胜
傅建涛
简润桐
叶德林
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New Pearl Guangdong New Materials Co ltd
Foshan Sanshui Newpearl Building Ceramic Industry Co Ltd
Hubei Newpearl Green Building Material Technology Co Ltd
Jiangxi Xinmingzhu Building Materials Co Ltd
Newpearl Group Co Ltd
Original Assignee
Foshan Sanshui Newpearl Building Ceramic Industry Co Ltd
Guangdong Summit Ceramics Co Ltd
Hubei Newpearl Green Building Material Technology Co Ltd
Jiangxi Xinmingzhu Building Materials Co Ltd
Newpearl Group Co Ltd
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Priority to CN202111236192.2A priority Critical patent/CN113860887B/en
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C—CHEMISTRY; METALLURGY
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    • C03C—CHEMICAL 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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Abstract

The invention relates to a ceramic plate and a preparation method thereof, wherein the preparation method of the ceramic plate comprises the following steps: preparing a green brick; preparing protective glaze, applying the protective glaze on the green brick, firing and edging to obtain a dry bead layer; the protective glaze is a solid glaze mixture and comprises a dispersing agent and dry round bead particles dispersed in the dispersing agent; the dry round bead particles are in the shape of round bead spheres and are mainly prepared from the following raw materials in parts by weight: 30-45 parts of potassium feldspar, 6-15 parts of albite, 6-10 parts of kaolin, 10-20 parts of barium carbonate, 3-8 parts of wollastonite, 3-8 parts of zinc oxide, 4-8 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of alumina, wherein the flow speed of the protective glaze is 33-38 seconds per 100 mL. The ceramic plate prepared by the method has excellent matte gloss, fine ceramic texture, excellent stain resistance and other physical properties.

Description

Ceramic plate and preparation method thereof
Technical Field
The invention relates to the technical field of ceramics, in particular to a ceramic plate and a preparation method thereof.
Background
With the continuous upgrading of the technology, in the technical field of ceramics, the continuous upgrading and upgrading of the glaze technology are reflected from the earliest wear-resistant bricks, printed glazed tiles and polished bricks to the current glaze polishing, marble and modern antique types, and the manufacture of high-grade ceramic tiles becomes the general pursuit of ceramic technicians. At present, since the modern antique brick of the matt class has soft gloss and gives people a comfortable and healthy experience in vision, compared with the bright class product, the light of the matt class product cannot give people too much visual impact, and the decoration has an elegant visual effect, so the matt class product is more and more popular with consumers and gradually becomes a mainstream product.
At present, with the popular popularization of ceramic sheets, matte products are applied to the sheets more and more. However, the quality of matte products on the market is not uniform, and most products have visual matte gloss, but have problems in touch and physical properties, such as: rough texture, poor smoothness, poor stain resistance and the like, and cannot well meet the requirements of consumers.
Disclosure of Invention
Based on this, there is a need for a ceramic plate and a method for preparing the same. The ceramic plate prepared by the method is a matte product, and the ceramic plate has fine texture and excellent physical properties such as stain resistance.
A preparation method of a ceramic plate comprises the following steps:
preparing a green brick;
preparing protective glaze, applying the protective glaze on the green brick, firing and edging to form a bead dry particle layer to prepare the ceramic plate;
the protective glaze is a solid glaze mixture and comprises a dispersant and dry round bead particles dispersed in the dispersant; the dried round bead particles are in the shape of round bead spheres and are mainly prepared from the following raw materials in parts by weight: 30-45 parts of potassium feldspar, 6-15 parts of albite, 6-15 parts of kaolin, 10-20 parts of barium carbonate, 3-8 parts of wollastonite, 3-8 parts of zinc oxide, 4-8 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of aluminum oxide, wherein the flow speed of the protective glaze is 33-38 seconds per 100 mL.
In some embodiments, the dispersant is white carbon black, and the mass ratio of the dry beads to the dispersant is (99.7-99.9): (0.1-0.3).
In some of the embodiments, the protective glaze is applied on the green brick, and in the step of firing and edging, the protective glaze is applied at a speed of 35-38 seconds per 100mLIs applied on the green brick with the application amount of 120-150g/m 2 ；
The sintering temperature is 1150-1250 ℃, and the sintering time is 40-80 min.
In some embodiments, the dry beads are prepared by the following method:
(1) mixing the raw materials for preparing the dry beads, and sintering to obtain a sintered product;
(2) crushing the fired product in the step (1) to obtain a dried particle semi-finished product;
(3) and (3) carrying out ball treatment on the semi-finished product of the dried granules obtained in the step (2) at the temperature of 850-950 ℃ to obtain the ball dried granules.
In some of these embodiments, the step of preparing the green brick comprises the steps of:
forming a base layer of a blank;
preparing a ground coat on the base layer of the blank;
and forming a pattern layer on the ground glaze layer to obtain the green brick.
In some of these embodiments, the step of forming the green body base layer comprises the steps of:
grinding the raw materials forming the base layer of the blank body to prepare slurry;
spraying the slurry to prepare powder, thus obtaining spray powder;
molding and drying the spray powder to obtain the base layer of the blank body;
in some embodiments, the chemical composition of the spray powder comprises SiO in percentage by mass 2 60％-64％、Al 2 O 3 22％-26％、TiO 2 +Fe 2 O 3 0.2％-0.6％、MgO 1％-2％、CaO 0.5％-1.2％、K 2 O 1.5％-2.5％、Na 2 O 2.5％-3.5％。
In some embodiments, in the grinding step, the grinding is performed by ball milling, and the ball milling is performed until the slurry passes through a 250-mesh screen, and the balance is 0.8% -1.0%.
In some embodiments, in the step of spray powdering, the moisture content of the spray powder is controlled to be 6.8% to 7.3%.
In some embodiments, in the drying step, the drying temperature is 150-200 ℃, the drying is carried out until the moisture content is 0.3% -0.7%, and the strength of the green body base layer is controlled to be 1.8-2.2 Mpa.
A ceramic plate is prepared by the preparation method.
In some embodiments, the ceramic plate has a thickness of 3-5mm, a width of 600-.
The preparation method of the ceramic plate forms proper amount of oxide through reasonable configuration of raw material components and utilizes K 2 O、Na 2 Multi-element flux such as O, CaO, BaO, ZnO and SrO to generate multi-element feldspar crystal phase, thereby generating low refractive index to promote matte effect and avoiding using Al with melting point up to 2050 DEG C 2 O 3 To eliminate light, thereby avoiding large content of Al 2 O 3 Resulting in a rough texture. And the dry round bead particles in the shape of round bead spheres are adopted to eliminate edges and corners on the surface, so that the dry particles are in the shape of round smooth round bead spheres, and show smooth texture after being applied to the surface of the ceramic plate, and the dry round bead particles can be tightly combined with one another, so that the density of the formed dry round bead particle layer is improved, the corresponding performance of the corresponding ceramic plate can be improved, the problems of dirt hiding and the like can be effectively reduced, and the ceramic plate has excellent performances in the aspects of dirt resistance, acid and alkali resistance and the like.
In addition, the preparation method of the ceramic plate adopts the solid glaze mixture containing the dry round bead particles and the dispersing agent, and the dry round bead particles are directly distributed on the thin plate in a solid form due to better fluidity, so that the problem that the thin plate is easy to crack caused by using liquid glaze is avoided, and meanwhile, the flowing speed of the protective glaze for protecting the glaze is controlled to be 33-38 seconds/100 mL, so that the thin plate with uniform thickness and compact and dense glaze layer is obtained.
Drawings
Fig. 1 is a schematic view of a ceramic plate according to an embodiment of the present invention;
FIG. 2 is an enlarged view of the dried beads prepared in example 1;
FIG. 3 is an enlarged view of the dried pellets prepared in comparative example 1.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
An embodiment of the present invention provides a method for preparing a ceramic plate, including the steps of:
s100: and (5) preparing a green brick.
It is understood that in step S100, the green brick can be prepared by the existing method, which is not particularly limited herein, and it is understood that the following method is preferred to prepare the green brick within the scope of the present invention:
s110, forming a blank base layer;
in some embodiments, step S110 includes:
s111: grinding the raw materials forming the base layer of the blank body to prepare slurry;
s112: spraying the slurry to prepare powder, thus obtaining spray powder;
s113: and forming and drying the sprayed powder to prepare a blank base layer.
In some embodiments, in step S111, grinding is performed by ball milling; further, ball milling each raw material forming the base layer of the blank until the slurry passes through a 250-mesh screen and the rest is 0.8-1.0%. The technical personnel of the invention find through research that the fineness of the slurry influences the shrinkage rate and the water absorption rate of the green body, and when the fineness is controlled within the range, the base layer of the green body can have better shrinkage rate and water absorption rate, thereby avoiding the phenomena of cracking and the like.
In some embodiments, the flow rate of the slurry in step S111 is controlled to be 45-60 seconds/100 mL, so as to facilitate the subsequent spraying and the like, and save the cost.
In some embodiments, in step S112, the moisture content of the sprayed powder produced after spraying is controlled to be 6.8% to 7.3%.
In some embodiments, in step S112, the chemical composition of the spray powder comprises SiO in percentage by mass 2 60％-64％、Al 2 O 3 22％-26％、TiO 2 +Fe 2 O 3 0.2％-0.6％、MgO 1％-2％、CaO 0.5％-1.2％、K 2 O 1.5％-2.5％、Na 2 O2.5% -3.5%; further, the chemical components of the spray powder comprise: SiO 2 2 62.94％、Al 2 O 3 24.29％、TiO 2 +Fe 2 O 3 0.42％、MgO 1.19％、CaO 0.81％、K 2 O 1.81％、Na 2 O2.81%, trace impurities and the balance being reduced by consideration.
Further, in step S113, a forming press is used for forming and pressing into a rectangular parallelepiped; further, the width is 600-1600mm, and the length is 1200-3200 mm; further, the thickness is 3mm-5 mm. The dry beads in the invention have a wide sintering range, and can show stable matt gloss and silk-like texture in different specifications, so that products with various specifications can be formed in the forming step.
It is understood that the shape of the ceramic plate is not particularly limited, and may be adjusted according to specific requirements, unless otherwise specified, and all such shapes are within the scope of the present invention. In the present invention, when the ceramic plate is a rectangular parallelepiped, the "length", "width" and "height" of the ceramic plate are determined by the conventional understanding in the art, wherein the longer edge of the bottom surface is "length", the shorter edge is "width", the edge perpendicular to the bottom surface is "height" (i.e., thickness), and the bottom surface is a surface parallel to the dry particle layer of the beads. In the present invention, the ceramic plate specification "D × L" indicates that the ceramic plate has a rectangular parallelepiped shape, wherein L and D respectively indicate a length and a width, and the larger of L and D is the length and the smaller is the width.
In some embodiments, the temperature of drying in step S113 is 150-; in some embodiments, in step S113, the drying equipment parameters are: length 80m, set temperature: 150 ℃ and 200 ℃, and the drying period is 70 min; in some embodiments, in step S113, the green body is dried to a moisture content of 0.3% to 0.7% and a strength of 1.8 to 2.2 Mpa; so as to ensure that the green bricks are not damaged in the conveying process on a production line before being sintered.
S120: preparing a ground coat on the base layer of the blank;
in some embodiments, step S120 includes the steps of:
s121: preparing the digital under coat, wherein the digital under coat comprises a basic glaze, an additive and a solvent.
In some embodiments, the base glaze material is 43-48%, the solvent is 30-40%, and the additive is 12-27%; further, 44% -46% of base glaze, 34% -36% of solvent and 18% -22% of additive; further, the base glaze is 45%, the solvent is 35%, and the additive is 20%.
In some embodiments, the base glaze is prepared from the following components in parts by weight: 8-12 parts of calcined kaolin, 20-24 parts of potassium feldspar, 23-27 parts of albite, 4-8 parts of wollastonite, 2-4 parts of barium carbonate, 1-3 parts of zinc oxide and 33-37 parts of clinker, wherein the clinker comprises the following chemical components in percentage by mass: SiO 2 2 57％-59％、Al 2 O 3 20％-22％、CaO6％-7％、MgO 2％-3％、K 2 O 3％-4％、Na 2 O 4％-5％、B 2 O 3 1% -2% and ZnO 2% -3%. Further, the basic glaze is mainly prepared from the following components: 9-11 parts of calcined kaolin, 21-23 parts of potassium feldspar, 24-26 parts of albite, 5-7 parts of wollastonite, 2-4 parts of barium carbonate and oxygen1-3 parts of zinc oxide and 34-36 parts of frit.
Further, the basic glaze is mainly prepared from the following components in parts by weight: 10 parts of calcined kaolin, 22 parts of potassium feldspar, 25 parts of albite, 6 parts of wollastonite, 3 parts of barium carbonate, 2 parts of zinc oxide and 35 parts of frit, wherein SiO is used for preparing the ceramic material according to mass percentage 2 58.18％、Al 2 O 3 21.45％、CaO 6.28％、MgO 2.21％、K 2 O 3.35％、Na 2 O 4.82％、B 2 O 3 1.23％、ZnO 2.48％。
In some embodiments, the additives comprise: functional resin additive, dispersant, suspending agent, defoaming agent, flatting agent and pH regulator. In some embodiments, in the digital under coat, the functional resin additive is 4% to 5%, the dispersant is 12% to 14%, the suspending agent is 0.1% to 0.2%, the defoamer is 0.3% to 0.5%, the leveling agent is 0.4% to 0.6%, and the pH regulator is 0.1% to 0.2% by mass.
In some embodiments, in the step of preparing the digital ground coat, the specific gravity of the product is 1.43g/mL and the particle size D is obtained by a grinding dispersion method 100 Under-glaze ink with the thickness of less than 1 micron; further, D 100 Is 0.9 micron.
S122: and spraying and printing the digital ground coat on the base layer of the blank to obtain the ground coat layer.
In some embodiments, in step S122, the jet printing amount is 40-45g/m 2 (ii) a The digital ground coat has strong covering capability, and the ground color of the blank can be covered only by spraying a small amount, so the purpose can be achieved by adopting the spraying amount, and a series of defects caused by over-thick ground coat layer can be effectively avoided. The traditional glaze spraying process is not suitable for the glazing link of a sheet blank with the thickness of 3.0-3.5mm, because the traditional glaze spraying process carries more water, the sheet blank is cracked, and the glaze spraying process effectively avoids the problems.
In some embodiments, the inkjet printer performs inkjet printing in step S122, and the ground glaze printed by the inkjet printer is uniformly distributed and compact.
S130: and forming a pattern layer on the ground glaze layer to obtain a green brick.
In some embodiments, in step S130, the green brick with the ground coat layer is moved to an industrial printer for pattern printing, and the channel is provided with blue, brown, yellow, black, orange, red and other color inks, and the corresponding color of the document is printed according to the design document.
S200: preparing protective glaze, applying the glaze cloth on a brick blank, firing and edging to prepare a dry bead layer;
the protective glaze is a solid glaze mixture and comprises dry round bead particles and a dispersing agent; the dry round bead particles are in the shape of round bead spheres and are mainly prepared from the following raw materials in parts by weight: 30-45 parts of potassium feldspar, 6-10 parts of albite, 6-10 parts of kaolin, 10-20 parts of barium carbonate, 4-7 parts of wollastonite, 3-6 parts of zinc oxide, 4-8 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of aluminum oxide.
It is understood that the sequence of operations between the step of preparing the glaze and the step of forming the green brick is not particularly limited, and the sequence of operations between the step of preparing the materials, such as the slurry in the step S111, the digital ground coat in the step S121, and the protective glaze in the step S200, is not particularly limited, and can be adjusted as required, and all of them are understood to be within the scope of the present invention.
The technicians of the invention find in the research that: with the improvement of the requirement on the glaze effect, the common glaze cannot meet the requirement of the ceramic sheet on the texture and the performance of each aspect, and the appearance and the application of dry particles greatly improve the glaze effect and the application performance of ceramic products. The matt ceramic plate is popular with consumers due to the soft luster, but most of the mechanisms for manufacturing matt glaze at present are realized by reducing the silicon-aluminum ratio in the formula, and the formula of the glaze with the reduced luster has the following defects:
1) the high temperature of the alumina causes rough handfeel of the glaze and is not fine enough;
2) the matte effect is that the matte is generated by the raw burning components and high porosity in the glaze, and the glaze surface has poor antifouling property;
3) the liquid glaze is not suitable for manufacturing the thin plate, and because the thickness of the blank body is thin, the water evaporation is slow after the liquid glaze is sprayed, and the damage of the green blank of the thin plate before sintering is easy to cause;
4) at present, matte products manufactured by using matte dry granules often have the defects of harsh hand feeling and easy dirt hiding after the dry granules are applied to ceramic plates due to irregular edges and corners.
Based on the technical scheme, the invention designs the technical scheme, forms an appropriate amount of oxide through reasonable configuration of raw material components, and applies K 2 O、Na 2 The multi-component flux such as O, CaO, BaO, ZnO, SrO, etc. can generate multi-component feldspar crystal phase, thereby generating low refractive index to promote the matte effect, and avoiding the use of Al with the melting point of 2050 DEG C 2 O 3 To eliminate light, thereby avoiding large content of Al 2 O 3 Resulting in a rough texture. And the dry round bead particles in the shape of a round bead sphere are adopted to eliminate edges and corners on the surface, so that the dry particles are in the shape of round and smooth spheres, smooth texture is presented after the dry round bead particles are applied to the surface of the ceramic plate, the dry round bead particles can be tightly combined, the density of a formed dry round bead particle layer is improved, the corresponding performance of the corresponding ceramic plate can be improved, the probability of occurrence of phenomena such as dirt hiding and the like can be effectively reduced, and the ceramic plate has excellent performances in the aspects of dirt resistance, acid and alkali resistance and the like. In addition, the preparation method of the ceramic plate adopts the solid glaze mixture containing the dried round bead particles and the dispersing agent, and the ceramic plate has better fluidity and is directly distributed on a thin plate in a solid form, so that the problem that the thin plate is easy to crack due to the use of the liquid glaze is avoided.
In some embodiments, in step S200, the dried beads are prepared by the following method:
s210: mixing the raw materials for preparing the dry beads, and sintering to obtain a sintered product.
In some embodiments, the dry beads are prepared from the following raw materials: 35 parts of potassium feldspar, 8 parts of albite, 8 parts of kaolin, 15 parts of barium carbonate, 6 parts of wollastonite, 5 parts of zinc oxide, 6 parts of strontium carbonate, 11 parts of calcite, 2 parts of quartz and 4 parts of aluminum oxide.
In some embodiments, the dry beads are prepared from the following raw materials: 40 parts of potassium feldspar, 6 parts of albite, 8 parts of kaolin, 18 parts of barium carbonate, 3 parts of wollastonite, 4 parts of zinc oxide, 8 parts of strontium carbonate, 7 parts of calcite, 2 parts of quartz and 4 parts of aluminum oxide,
in some embodiments, the dry beads are prepared from the following raw materials: 30 parts of potassium feldspar, 15 parts of albite, 8 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of aluminum oxide.
In some embodiments, the mass ratio of barium carbonate, zinc oxide, strontium carbonate is (10-18): (4-8): (6-8). The contents of barium carbonate, zinc oxide and strontium carbonate need to be controlled within a certain range, if the contents are too high, the divalent ions are easy to be too clear, excessive barium-zinc-strontium crystals can be generated, and the transparency of dry particles is low; if the content is too low, Al is contained in the alloy 2 O 3 And SiO 2 Belongs to a substance with larger high-temperature viscosity, and dry grains can be dry and rough if enough flux is not used for melting.
In some embodiments, the chemical composition of the dried beads comprises, in mass percent: 3 to 5 percent of CaO, 9 to 12 percent of BaO, 3.5 to 5 percent of SrO and 3.6 to 4 percent of ZnO; furthermore, CaO is 4.3% -4.7%, BaO is 10.6% -11%, SrO is 4% -4.4%, and ZnO is 3.6% -4%. In some embodiments, in the chemical composition of the dry bead, SiO 2 50% -55% of Al 2 O 3 16 to 19 percent of CaO, 3 to 5 percent of CaO, 9 to 12 percent of BaO, 3.5 to 5 percent of SrO, 4.5 to 6.5 percent of KNaO and 3.6 to 4 percent of ZnO.
In some embodiments, in step S201, firing is performed by the following method;
at a first time t 1 Internal heating to 295-305 ℃, and then heating for a second time t 2 Internally heating to 1050-1150 deg.C, and then heating for a third time t 3 Internally heating to 1300-1500 ℃, and then preserving the heat for a fourth time t within the range of 1300-1500 DEG C 4 Then cooling to 300-400 ℃; wherein, t 1 Is 8min-60min, t 2 Is 28min-60min, t 3 Is 18-50min，t 4 Is 10-30 min;
further, at a first time t 1 Internal heating to 300 deg.C, and then at a second time t 2 Internally heating to 1100 deg.C, and then making third time t 3 Internally heating to 1450 deg.C, and keeping the temperature at 1450 deg.C for a fourth time t 4 Then cooling to 300-400 ℃; t is t 1 Is 8-12 min, t 2 Is 28min-32min, t 3 Is 18min-22min, t 4 Is 10min-15 min; further, t 1 Is 10min, t 2 Is 30min, t 3 Is 20min, t 4 It is 10 min.
In the gradient temperature control sintering method, in the first stage, the temperature is increased to 295-305 ℃ within a specific time to ensure that the structural water and the adsorbed water in each material are fully discharged; in the second stage, the kaolin is heated to 1050-1150 ℃ in a specific time to decompose organic matters in the kaolin, and carbonate is decomposed to discharge CO under the fluxing of the monovalent oxide 2 (ii) a The third stage reaches 1300-1500 ℃ and keeps the temperature t within the range of 1300-1500 DEG C 4 So that the materials begin to melt, liquid phase begins to generate under the action of the flux, and oxides and SiO 2 And Al 2 O 3 The feldspar crystals with proper proportion are formed, so that the dry bead particles are guaranteed to have excellent hand feeling, the prepared dry bead particle material can be suitable for different firing temperatures and different glazes, and stable matte glossiness and silky fine touch can be presented at different tile firing temperatures and on the basis of different overglazes. In addition, the inventor of the invention finds that the matte effect and the hand feeling of the fired dry beads are closely related to the firing curve, the setting and the formula of the firing curve are required to be adapted to form a proper eutectic phase, the crystalline phase with low refractive index is generated by utilizing the clear crystal of the divalent oxide to reduce the glossiness, and the gloss cannot fluctuate due to the fluctuation of the temperature after the ceramic tile is used for the ceramic tile, so that the ceramic tile has a large firing range.
S220: and crushing the fired product to obtain a dried particle semi-finished product.
In some embodiments, in the cooling step of step S220, the fired product is introduced into water at a temperature of less than 50 ℃ to obtain a cooled product. The water with lower temperature is adopted, so that the crushing effect is better, and the subsequent crushing treatment is facilitated.
In some embodiments, in the crushing step of step S220, the crushed product is crushed to form a semi-finished dry pellet, and the semi-finished dry pellet is passed through a 300-mesh screen of 250 meshes, so as to facilitate the subsequent steps.
S230: and (3) carrying out ball balling treatment on the semi-finished product of the dried granules at the temperature of 850-950 ℃ to obtain the ball dried granules.
In the invention, the term "spheroidizing" refers to heating the semi-finished dry pellets in a high temperature environment, eliminating the edges and corners by using high temperature, and improving the roundness of the dry pellets, and can be realized by adopting heating equipment commonly used in the field and only reaching the corresponding temperature, and is not limited particularly, but is understood to be within the scope of the invention.
After the corresponding semi-finished product of the dried round bead is prepared by the preparation method of the dried round bead, round bead treatment is carried out at a specific temperature, so that irregular prismatic structures on the surfaces of the dried round bead are eliminated, further, the dried round bead with a round bead spherical structure and a round bead layer can be obtained, the formation of a compact dried round bead layer is facilitated, and the treatment at the temperature can improve the hand feeling of the ceramic product corresponding to the dried round bead to obtain a product with smooth and fine hand feeling.
In some embodiments, the temperature of the beading process in step S230 is 900 ℃, 901 ℃, 902 ℃, 903 ℃, 904 ℃, 905 ℃, 906 ℃, 907 ℃, 908 ℃, 909 ℃, 910 ℃, 915 ℃, 920 ℃, 925 ℃, 930 ℃, 935 ℃ or 940 ℃.
In some embodiments, in step S230, the dry pellet semi-finished product is passed through a heating zone of a high temperature furnace in a free-fall manner. The semi-finished product passes through a heating zone of a high-temperature smelting furnace in a free falling mode, and the self weight of the semi-finished product is utilized, so that the roundness of the dry beads can be effectively improved, and the deformation caused by the heat treatment of the dry bead semi-finished product in a specific container is avoided.
In some embodiments, in step S200, the dispersant is white carbon black, which has very excellent dispersibility, and can effectively reduce the addition amount of the dispersant, and at the same time, make the protective glaze have very excellent fluidity, and because the adopted dry particles are in the shape of spherical balls, the fluidity of the protective glaze can be further improved, so that the dry particles also have higher fluidity in the absence of water, and thus can avoid the use of water, the method of the present invention can be used for preparing thin plate ceramic plate products, and broadens the application field.
In some embodiments, the mass ratio of the dry beads to the dispersant is (99.5-99.9): (0.1-0.5); further, the mass ratio of the dry round bead particles to the dispersing agent is (99.7-99.9): (0.1-0.3); further, the mass ratio of the dry beads to the dispersing agent is 99.8: 0.2.
in some embodiments, the protective glaze does not contain water in step S200.
In some embodiments, the flow rate of the protective glaze in step S200 is 33-38S/100mL (i.e., seconds/100 mL); so as to obtain a thin plate with uniform thickness and compact glaze layer. In some embodiments, the application amount is 120-150g/m 2 So as to obtain a compact bead dry particle layer with the target thickness, and the bead particles are uniformly distributed.
In some embodiments, the protective glaze is stored in a bin on the glaze line and is applied using a roller application device that applies dry solid glaze to the green brick as it passes by at a certain rate of rotation.
Because the invention adopts the formula of the dry beads, the invention can keep better matte luster and fine hand feeling in a wider sintering temperature range, so the sintering temperature range can be adjusted as required, and in the preferred step S200, the sintering temperature is 1100-1300 ℃; further, the sintering temperature is 1150-1250 ℃; furthermore, the sintering temperature is 1200 ℃ to obtain better comprehensive technical effect.
In some embodiments, in step S200, the firing time is 40-80 min; further, the firing time was 60 min.
An embodiment of the present invention provides a ceramic plate prepared by the above preparation method. The ceramic plate disclosed by the invention not only has excellent matte light sensation and silky handfeel, but also has excellent antifouling, acid and alkali resistance, chemical corrosion resistance, acid and alkali resistance, anti-skid performance and the like.
As shown in fig. 1, an embodiment of the present invention provides a ceramic board 10 including a green brick 100 and a layer 200 of dried beads coated on the green brick 100; further, the green brick 100 comprises a green body base layer 101, a ground coat layer 102 and a pattern layer 103 which are sequentially stacked, the pattern layer 103 is in contact with the bead dry particle layer 200, and relevant features of each functional layer are as described above and will not be described herein again. In some embodiments, ceramic plate 10 has a thickness of 2-4 mm; further, the ceramic plate 10 has a thickness of 3 to 3.7 mm; further, the ceramic plate 10 has a thickness of 3 to 3.5 mm; in some embodiments, the thickness of the green base layer 101 is 3-3.5 mm; in some embodiments, the thickness of the ground glaze layer 102 is 0.01-0.02 mm; in some embodiments, the thickness of the layer of dry beads 200 is 0.05-0.1 mm; in one embodiment, the width of the ceramic plate 10 is 600-.
The present invention will be described below by way of specific examples, which are intended to be illustrative only and should not be construed as limiting the invention.
Example 1
The preparation method of the ceramic plate of this example is as follows:
(1) preparing spray powder:
ball-milling the blanks by using raw material minerals until slurry passes through a 250-mesh screen and has a screen residue of 0.8-1.0%, controlling the flow rate of the slurry at 45-60 seconds/100 mL, and preparing the slurry into spray powder by spraying, wherein the moisture of the spray powder is controlled at 6.8-7.3%, and the chemical components of the spray powder are SiO in percentage by mass 2 :62.94％、Al 2 O 3 ：24.29％、TiO 2 +Fe 2 O 3 ：0.42％、MgO：1.19％、CaO：0.81％、K 2 O：1.81％、Na 2 O: 2.81 percent, and the balance of trace impurities and reduction.
(2) Preparing a digital under coat:
the basic glaze formula comprises 10% of calcined kaolin and potassium by mass percent22% of feldspar, 25% of albite, 6% of wollastonite, 35% of clinker, 3% of barium carbonate and 2% of zinc oxide, wherein the clinker comprises the following chemical components in percentage by mass: SiO 2 2 :58.18％、Al 2 O 3 :21.45％、CaO:6.28％、MgO:2.21％、K 2 O：3.35％、Na 2 O:4.82％、B 2 O 3 ：1.23％、ZnO：2.48％；
Selecting the basic glaze materials according to the mass percentage: 45% of basic glaze, 5% of functional resin additive, 35% of ethyl acetate solvent, 13.8% of dispersing agent, 0.15% of suspending agent, 0.4% of defoaming agent, 0.5% of flatting agent and 0.15% of pH value regulator. Grinding and dispersing to obtain the product with specific gravity of 1.43g/mL and particle diameter of D 100 Is a 0.9 micron digital ground coat.
(3) Preparation of protective glaze:
firstly, weighing the following raw materials in parts by weight: 35 parts of potassium feldspar, 8 parts of albite, 8 parts of kaolin, 15 parts of barium carbonate, 6 parts of wollastonite, 5 parts of zinc oxide, 6 parts of strontium carbonate, 11 parts of calcite, 2 parts of quartz and 4 parts of aluminum oxide; then uniformly mixing the raw materials to obtain a mixture, conveying the mixture into a frit furnace for firing, melting the mixture into liquid at a high temperature of 1450 ℃, flowing into cold water for crushing to obtain granular glass bodies, and crushing to obtain dry granular semi-finished products with the mesh number of 200-300 meshes; the semi-finished product of the dry particles is sprayed in a melting furnace at 900 ℃ for spheroidizing treatment, the dry particles of the beads are collected and pass through a 250-mesh and 300-mesh sieve for grading the particle composition, and the enlarged picture is shown in fig. 2.
Mixing the dry round bead particles and the white carbon black according to a mass ratio of 99.8: 0.2, and mixing evenly to obtain the protective glaze, wherein the flow rate is controlled to be 33-38s/100 mL.
(4) Preparation of green body substrate layer
And (3) forming the spray powder prepared in the step (1) by using a forming press, and after the green brick is formed, feeding the green brick into drying equipment, wherein the parameters of the drying equipment are as follows: length 80m, set temperature: 150 ℃ and 200 ℃, and the drying period is as follows: and (5) controlling the moisture of the dried green brick to be 0.5% and controlling the strength of the green brick to be 2.0MPa for 70 min.
(5) Preparation of the ground glaze layer
Conveying the dried green bricks in the step (4) to an industrial printer by a conveyor for printing, and spray-printing the digital ground coat in the step (2), wherein the spray-printing amount is 40-45g/m 2 And forming a ground coat layer.
(6) Preparation of the patterned layer
And (4) feeding the green bricks subjected to the digital under glaze printing in the step (5) into a second industrial printer for pattern printing, wherein the channel is provided with blue, brown, yellow, black, orange, red and other color inks, and the corresponding colors of the file are printed according to the design file.
(7) Preparation of a layer of dry beads
The green bricks after the patterns are printed in the step (6) enter a dry particle distribution process, the protective glaze in the step (3) is stored in a box body on a glaze line and distributed through a roller distribution device at the flow rate of 35-38 seconds/100 mL, when the green bricks pass through, the roller distributes dry particle solid glaze to the surfaces of the bricks at a certain rotation speed, and the distribution amount is 150 g/m- 2 。
And conveying the adobes coated with the protective glaze into a roller kiln for firing at 1200 ℃ for 60 minutes, discharging the adobes out of the kiln to obtain a crude ceramic plate, conveying the crude ceramic plate into edging equipment for edging, and obtaining the ceramic plate of the embodiment when the crude ceramic plate reaches the required standard size.
Example 2
The preparation method of the ceramic plate of this example is as follows:
(1) preparing spray powder:
ball-milling each blank by using raw material minerals until slurry passes through a 250-mesh screen and has a screen residue of 0.8-1.0%, controlling the flow rate of the slurry at 45-60s/mL, and carrying out spray milling on the slurry to prepare spray powder, wherein the moisture of the spray powder is controlled at 6.8-7.3%, and the chemical components of the spray powder are SiO in percentage by mass 2 :62.94％、Al 2 O 3 ：24.29％、TiO 2 +Fe 2 O 3 ：0.42％、MgO：1.19％、CaO：0.81％、K 2 O：1.81％、Na 2 O: 2.81 percent, and the balance of trace impurities and reduction.
(2) Preparing a digital under coat:
the basic glaze formula comprises, by mass, 10% of calcined kaolin, 22% of potassium feldspar, 25% of albite, 6% of wollastonite, 35% of frit, 3% of barium carbonate and 2% of zinc oxide, wherein the frit comprises the following chemical components in percentage by mass: SiO 2 2 :58.18％、Al 2 O 3 :21.45％、CaO:6.28％、MgO:2.21％、K 2 O：3.35％、Na 2 O:4.82％、B 2 O 3 ：1.23％、ZnO：2.48％；
Selecting the basic glaze materials according to the mass percentage: 45% of basic glaze, 5% of functional resin additive, 35% of ethyl acetate solvent, 13.8% of dispersing agent, 0.15% of suspending agent, 0.4% of defoaming agent, 0.5% of flatting agent and 0.15% of pH value regulator. Grinding and dispersing to obtain the product with specific gravity of 1.43g/mL and particle diameter of D 100 Is a 0.9 micron digital ground coat.
(3) Preparation of protective glaze:
firstly, weighing the following raw materials in parts by weight: 40 parts of potassium feldspar, 6 parts of albite, 8 parts of kaolin, 18 parts of barium carbonate, 3 parts of wollastonite, 4 parts of zinc oxide, 8 parts of strontium carbonate, 7 parts of calcite, 2 parts of quartz and 4 parts of aluminum oxide; then uniformly mixing the raw materials to obtain a mixture, conveying the mixture into a frit furnace for firing, melting the mixture into liquid at a high temperature of 1450 ℃, flowing into cold water for crushing to obtain granular glass bodies, and crushing to obtain dry granular semi-finished products with the mesh number of 200-300 meshes; spraying the semi-finished product of the dry particles in a melting furnace at the temperature of 900 ℃ for spheroidization, collecting the dry particles of the round particles, and grading the dry particles of the round particles by a sieve with 250-mesh and 300-mesh meshes.
Mixing the dry round bead particles and the white carbon black according to a mass ratio of 99.8: 0.2, and mixing evenly to obtain the protective glaze, wherein the flow rate is controlled to be 33-38s/100 mL.
(4) Preparation of green body substrate layer
And (3) forming the spray powder prepared in the step (1) by using a forming press, and after the green brick is formed, feeding the green brick into drying equipment, wherein the parameters of the drying equipment are as follows: length 80m, set temperature: 150 ℃ and 200 ℃, and the drying period is as follows: and (5) controlling the moisture of the dried green brick to be 0.5% and controlling the strength of the green brick to be 2.0MPa for 70 min.
(5) Preparation of the ground glaze layer
Conveying the dried green bricks in the step (4) to an industrial printer by a conveyor for printing, and spray-printing the digital ground glaze in the step (2) with the spray-printing amount of 40-45g/m 2 And forming a ground coat layer.
(6) Preparation of the patterned layer
And (5) feeding the adobes subjected to the digital under glaze printing in the second industrial printer for pattern printing, wherein the channel is provided with blue, brown, yellow, black, orange, red and other color inks, and the corresponding colors of the file are printed according to the design file.
(7) Preparation of a layer of dry beads
And (3) putting the green brick printed with the pattern in the step (6) into a dry particle distribution process, storing the protective glaze in the step (3) in a box on a glaze line, distributing the protective glaze at a flow rate of 35-38 seconds/100 mL by a roller distribution device, and distributing dry particle solid glaze to the surface of the green brick at a certain rotation speed by a roller when the green brick passes through the roller. The application amount of the cloth is 120-150g/m 2 。
And conveying the adobes coated with the protective glaze into a roller kiln for firing at 1200 ℃ for 60 minutes, discharging the adobes out of the kiln to obtain a crude ceramic plate, conveying the crude ceramic plate into edging equipment for edging, and obtaining the ceramic plate of the embodiment when the crude ceramic plate reaches the required standard size.
Example 3
The preparation method of the ceramic plate of this example is as follows:
(1) preparing spray powder:
ball-milling each blank by using raw material minerals until slurry passes through a 250-mesh screen and has a screen residue of 0.8-1.0%, controlling the flow rate of the slurry at 45-60s/mL, and carrying out spray milling on the slurry to prepare spray powder, wherein the moisture of the spray powder is controlled at 6.8-7.3%, and the chemical components of the spray powder are SiO in percentage by mass 2 :62.94％、Al 2 O 3 ：24.29％、TiO 2 +Fe 2 O 3 ：0.42％、MgO：1.19％、CaO：0.81％、K 2 O：1.81％、Na 2 O: 2.81% and the balance of microImpurity amount and reduction.
(2) Preparing a digital under coat:
the basic glaze formula comprises, by mass, 10% of calcined kaolin, 22% of potassium feldspar, 25% of albite, 6% of wollastonite, 35% of frit, 3% of barium carbonate and 2% of zinc oxide, wherein the frit comprises the following chemical components: SiO 2 2 :58.18％、Al 2 O 3 :21.45％、CaO:6.28％、MgO:2.21％、K 2 O：3.35％、Na 2 O:4.82％、B 2 O 3 ：1.23％、ZnO：2.48％；
Selecting the basic glaze materials according to the mass percentage: 45% of basic glaze, 5% of functional resin additive, 35% of ethyl acetate solvent, 13.8% of dispersing agent, 0.15% of suspending agent, 0.4% of defoaming agent, 0.5% of flatting agent and 0.15% of pH value regulator. Grinding and dispersing to obtain the product with specific gravity of 1.43g/ml and particle diameter of D 100 Is a 0.9 micron digital ground coat.
(3) Preparation of protective glaze:
firstly, weighing the following raw materials in parts by weight: 30 parts of potassium feldspar, 15 parts of albite, 8 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of aluminum oxide; then uniformly mixing the raw materials to obtain a mixture, conveying the mixture into a frit furnace for firing, melting the mixture into liquid at a high temperature of 1450 ℃, flowing into cold water for crushing to obtain granular glass bodies, and crushing to obtain dry granular semi-finished products with the mesh number of 200-300 meshes; spraying the semi-finished product of the dry particles in a melting furnace at the temperature of 900 ℃ for spheroidization, collecting the dry particles of the round particles, and grading the dry particles of the round particles by a sieve with 250-mesh and 300-mesh meshes.
Mixing the dry round bead particles and the white carbon black according to a mass ratio of 99.8: 0.2, and mixing uniformly to obtain the protective glaze, wherein the flow rate is controlled to be 33-38 seconds/100 mL.
(4) Preparation of green body substrate layer
And (3) forming the spray powder prepared in the step (1) by using a forming press, and after the green brick is formed, feeding the green brick into drying equipment, wherein the parameters of the drying equipment are as follows: length 80m, set temperature: 150 ℃ and 200 ℃, and the drying period is as follows: and (5) controlling the moisture of the dried green brick to be 0.5% and controlling the strength of the green brick to be 2.0MPa for 70 min.
(5) Preparation of the ground glaze layer
Conveying the dried green bricks in the step (4) to an industrial printer by a conveyor for printing, and spray-printing the digital ground glaze in the step (2) with the spray-printing amount of 40-45g/m 2 And forming a ground coat layer.
(6) Preparation of the patterned layer
And (5) feeding the adobes subjected to the digital under glaze printing in the second industrial printer for pattern printing, wherein the channel is provided with blue, brown, yellow, black, orange, red and other color inks, and the corresponding colors of the file are printed according to the design file.
(7) Preparation of a layer of dry beads
And (3) putting the green brick printed with the pattern in the step (6) into a dry particle distribution process, storing the protective glaze in the step (3) in a box body on a glaze line, distributing the protective glaze through a roller distributing device at a flow rate of 35-38 seconds/100 ml, and distributing dry particle solid glaze to the surface of the green brick at a certain rotating speed by a roller when the green brick passes through the roller. The application amount of the cloth is 120-150g/m 2 。
And conveying the adobes coated with the protective glaze into a roller kiln for firing at 1200 ℃ for 60 minutes, discharging the adobes out of the kiln to obtain a crude ceramic plate, conveying the crude ceramic plate into edging equipment for edging, and obtaining the ceramic plate of the embodiment when the crude ceramic plate reaches the required standard size.
Comparative example 1
This comparative example differs from example 1 in that the formulation and morphology of the dry particles in the protective glaze are different, in particular:
(1) preparing spray powder:
ball-milling the blanks by using raw material minerals until slurry passes through a 250-mesh screen and has a screen residue of 0.8-1.0%, controlling the flow rate of the slurry at 45-60 seconds/mL, and spraying the slurry to prepare powder, wherein the moisture of the powder is controlled at 6.8-7.3%, and the chemical components of the powder are SiO in percentage by mass 2 :62.94％、Al 2 O 3 ：24.29％、TiO 2 +Fe 2 O 3 ：0.42％、MgO：1.19％、CaO：0.81％、K 2 O：1.81％、Na 2 O: 2.81 percent, and the balance of trace impurities and reduction.
(2) Preparing a digital under coat:
the basic glaze formula comprises, by mass, 10% of calcined kaolin, 22% of potassium feldspar and sodium feldspar: 25%, wollastonite: 6%, frit: 35 percent of fused block, 3 percent of barium carbonate and 2 percent of zinc oxide, wherein the fused block comprises the following chemical components in percentage by mass: SiO 2 2 :58.18％、Al 2 O 3 :21.45％、CaO:6.28％、MgO:2.21％、K 2 O：3.35％、Na 2 O:4.82％、B 2 O 3 ：1.23％、ZnO：2.48％；
Selecting the basic glaze materials according to the mass percentage: 45% of basic glaze, 5% of functional resin additive, 35% of ethyl acetate solvent, 13.8% of dispersing agent, 0.15% of suspending agent, 0.4% of defoaming agent, 0.5% of flatting agent and 0.15% of pH value regulator. Grinding and dispersing to obtain the product with specific gravity of 1.43g/mL and particle diameter of D 100 Is a 0.9 micron digital ground coat.
(3) Preparation of protective glaze:
firstly, weighing the following raw materials in parts by weight: 35 parts of potassium feldspar, 8 parts of albite, 12 parts of kaolin, 8 parts of wollastonite, 15 parts of calcite, 12 parts of calcined talc, 5 parts of quartz and 5 parts of alumina; then, the raw materials are uniformly mixed to obtain a mixed material, the mixed material is transported into a frit furnace to be fired, is melted into liquid at the high temperature of 1450 ℃, flows into cold water to be crushed into granular glass bodies, and is crushed to form dry granules with the mesh number of 200-300, and the enlarged view is shown in figure 3.
Mixing dry particles and white carbon black according to a mass ratio of 99.8: 0.2 mixing and uniformly mixing, wherein the flow rate is controlled to be 50-53s/mL, and the flow rate of the prepared dry particle solid glaze mixture is larger because the dry particles are not in the shape of round bead dry particles.
(4) Preparation of green body substrate layer
And (3) forming the spray powder prepared in the step (1) by using a forming press, and after the green brick is formed, feeding the green brick into drying equipment, wherein the parameters of the drying equipment are as follows: length 80m, set temperature: 150 ℃ and 200 ℃, and the drying period is as follows: and (5) controlling the moisture of the dried green brick to be 0.5% and controlling the strength of the green brick to be 2.0MPa for 70 min.
(5) Preparation of the ground glaze layer
Conveying the dried green bricks in the step (4) to an industrial printer by a conveyor for printing, and spray-printing the digital ground glaze in the step (2) with the spray-printing amount of 40-45g/m 2 And forming a ground coat layer.
(6) Preparation of the patterned layer
And (5) feeding the adobes subjected to the digital under glaze printing in the second industrial printer for pattern printing, wherein the channel is provided with blue, brown, yellow, black, orange, red and other color inks, and the corresponding colors of the file are printed according to the design file.
(7) Preparation of a layer of dry beads
And (3) storing the green bricks subjected to pattern printing in the step (6) in a box body on a glaze line by adopting the protective glaze in the step (3), distributing the green bricks by a roller distribution device at a flow rate of 50-53s/100mL, and distributing dry solid glaze to the surfaces of the green bricks by a roller at a certain rotating speed when the green bricks pass. The application amount of the cloth is 120-150g/m 2 。
And conveying the adobes coated with the protective glaze into a roller kiln for firing at 1200 ℃ for 60 minutes, discharging the adobes out of the kiln to obtain a crude ceramic plate, conveying the crude ceramic plate into edging equipment for edging, and obtaining the ceramic plate of the comparative example after the crude ceramic plate reaches the required standard size.
Comparative example 2
This comparative example differs from example 1 in that the protective glaze is a bead dry liquid glaze, in particular: (1) preparing spray powder:
ball-milling the blanks by using raw material minerals until slurry passes through a 250-mesh screen and has a screen residue of 0.8-1.0%, controlling the flow rate of the slurry at 45-60s/mL, and spraying the slurry to prepare powder, wherein the moisture of the powder is controlled at 6.8-7.3%, and the chemical components of the powder are SiO in percentage by mass 2 :62.94％、Al 2 O 3 ：24.29％、TiO 2 +Fe 2 O 3 ：0.42％、MgO：1.19％、CaO：0.81％、K 2 O：1.81％、Na 2 O: 2.81 percent, and the balance of trace impurities and reduced by consideration.
(2) Preparing a digital under coat:
the basic glaze formula comprises, by mass, 10% of calcined kaolin, 22% of potassium feldspar and the following components: 25%, wollastonite: 6%, frit: 35 percent, 3 percent of barium carbonate and 2 percent of zinc oxide, wherein the frit comprises the following chemical components in percentage by mass: SiO 2 2 :58.18％、Al 2 O 3 :21.45％、CaO:6.28％、MgO:2.21％、K 2 O：3.35％、Na 2 O:4.82％、B 2 O 3 ：1.23％、ZnO：2.48％；
Selecting the basic glaze materials according to the mass percentage: 45% of basic glaze, 5% of functional resin additive, 35% of ethyl acetate solvent, 13.8% of dispersing agent, 0.15% of suspending agent, 0.4% of defoaming agent, 0.5% of flatting agent and 0.15% of pH value regulator. Grinding and dispersing to obtain the product with specific gravity of 1.43g/ml and particle diameter of D 100 Is a 0.9 micron digital ground coat.
(3) Preparation of protective glaze:
firstly, weighing the following raw materials in parts by weight: 35 parts of potassium feldspar, 8 parts of albite, 8 parts of kaolin, 15 parts of barium carbonate, 6 parts of wollastonite, 5 parts of zinc oxide, 6 parts of strontium carbonate, 11 parts of calcite and 2 parts of quartz; then uniformly mixing the raw materials to obtain a mixture, conveying the mixture into a frit furnace for firing, melting the mixture into liquid at a high temperature of 1450 ℃, flowing into cold water for crushing to obtain granular glass bodies, and crushing to obtain dry granular semi-finished products with the mesh number of 200-300 meshes; spraying the semi-finished product of the ball bead into a melting furnace at 900 ℃ for balling, collecting the ball bead dry particles, and grading the ball bead dry particles through a 250-300-mesh screen.
Mixing the dried round bead granules and a suspending agent 9022A in a mass ratio of 30: 100 to obtain the ball dry particle liquid glaze, and the flow rate of the ball dry particle liquid glaze is controlled to be 33-38 seconds/100 mL.
(4) Preparation of green body substrate layer
And (3) forming the spray powder prepared in the step (1) by using a forming press, and after the green brick is formed, feeding the green brick into drying equipment, wherein the parameters of the drying equipment are as follows: length 80m, set temperature: 150 ℃ and 200 ℃, and the drying period is as follows: and (5) controlling the moisture of the dried green brick to be 0.5% and controlling the strength of the green brick to be 2.0MPa for 70 min.
(5) Preparation of the ground glaze layer
Conveying the dried green bricks in the step (4) to an industrial printer by a conveyor for printing, and spray-printing the digital ground glaze in the step (2) with the spray-printing amount of 40-45g/m 2 And forming a ground coat layer.
(6) Preparation of the patterned layer
And (5) feeding the adobes subjected to the digital under glaze printing in the second industrial printer for pattern printing, wherein the channel is provided with blue, brown, yellow, black, orange, red and other color inks, and the corresponding colors of the file are printed according to the design file.
(7) Preparation of a layer of dried beads
And (3) putting the green brick printed with the pattern in the step (6) into a dry particle distribution process, storing the protective glaze in the step (3) in a box on a glaze line, distributing the protective glaze at a flow rate of 35-38 seconds/100 mL by a roller distribution device, and distributing dry particle solid glaze to the surface of the green brick at a certain rotation speed by a roller when the green brick passes through the roller. The application amount of the cloth is 120-150g/m 2 。
And conveying the adobes coated with the protective glaze into a roller kiln for firing at 1200 ℃ for 60 minutes, discharging the adobes out of the kiln to obtain a crude ceramic plate, conveying the crude ceramic plate into edging equipment for edging, and obtaining the ceramic plate of the embodiment when the crude ceramic plate reaches the required standard size.
Performance testing
The physical properties and breakage rate of the ceramic plates of examples 1 to 3 and comparative examples 1 to 2 were measured and shown in tables 1 to 7.
TABLE 1
Figure BDA0003317579550000201
TABLE 2
Figure BDA0003317579550000202
TABLE 3
Figure BDA0003317579550000203
TABLE 4
Figure BDA0003317579550000204
Figure BDA0003317579550000211
TABLE 5
Figure BDA0003317579550000212
TABLE 6
Figure BDA0003317579550000213
TABLE 7
Figure BDA0003317579550000214
As can be seen from tables 1 to 6, the ceramic plates of examples 1 to 3 have superior wear resistance, stain resistance, chemical resistance, acid and alkali resistance, and anti-slip properties. The ceramic plate prepared by the method has excellent matte luster and silky hand feel, excellent wear resistance, stain resistance, chemical corrosion resistance, acid and alkali resistance and anti-skid performance, and can well meet the requirements of consumers.
In addition, comparative example 1 was conducted using a general flux K 2 O, NaO, CaO and MgO are used as flux, the prepared dry particles are all 250-300 meshes in processing thickness, the appearance is close, soThe prepared dry particles are in the category of matt dry particles, but the dry particle solid glaze prepared in the comparative example 1 has a large flow rate, can only be controlled within 53-58s/100mL, is not beneficial to being applied to a sheet blank in the dry particle application stage, and the physical properties of the prepared ceramic plate are weaker than those of the ceramic plates in the examples 1-3. The invention effectively improves the fluidity of the protective glaze by optimizing the formula and the shape of the dry particles of the round beads.
Comparative example 2 is that the round bead dry particles are made into liquid glaze and are applied on the surface of a thin plate blank, because the thin plate blank is thin, the yield of the liquid glaze after being applied on the blank is lower than that of the solid glaze (shown in table 7), and the breakage rate of the comparative example 2 is far greater than that of the solid glaze by adopting a liquid glaze process. The solid protective glaze of the invention can effectively reduce the breakage rate.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A preparation method of a ceramic plate is characterized by comprising the following steps:
preparing a green brick;
preparing protective glaze, applying the protective glaze on the green brick, firing and edging to form a bead dry particle layer to prepare the ceramic plate;
the protective glaze is a solid glaze mixture and comprises a dispersant and dry round bead particles dispersed in the dispersant; the dried round bead particles are in the shape of round bead spheres and are mainly prepared from the following raw materials in parts by weight: 30-45 parts of potassium feldspar, 6-15 parts of albite, 6-15 parts of kaolin, 10-20 parts of barium carbonate, 3-8 parts of wollastonite, 3-8 parts of zinc oxide, 4-8 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of alumina, wherein the flow speed of the protective glaze is 33-38 seconds per 100 mL;
the bead dry particles are prepared by the following method:
(1) mixing the raw materials for preparing the dry beads, and sintering to obtain a sintered product; wherein the firing operation comprises the steps of: at a first time t 1 Internal heating to 295-305 ℃, and then heating for a second time t 2 Internally heating to 1050-1150 deg.C, and then heating for a third time t 3 Internally heating to 1300-1500 ℃, and then preserving the heat for a fourth time t within the range of 1300-1500 DEG C 4 Then cooling to 300-400 ℃; wherein, t 1 Is 8min-60min, t 2 Is 28min-60min, t 3 Is 18-50min, t 4 Is 10-30 min;
(2) crushing the fired product in the step (1) to prepare a dried particle semi-finished product;
(3) and (3) carrying out ball treatment on the semi-finished product of the dried granules obtained in the step (2) at the temperature of 850-950 ℃ to obtain the ball dried granules.
2. The preparation method according to claim 1, wherein the dispersant is white carbon black, and the mass ratio of the dry round bead particles to the dispersant is (99.7-99.9): (0.1-0.3).
3. The method as claimed in claim 2, wherein the step of applying the protective glaze to the green brick, firing and edging comprises applying the protective glaze to the green brick at a rate of 35-38 seconds/100 mL in an amount of 120-150g/m 2 (ii) a The sintering temperature is 1150-1250 ℃, and the sintering time is 40-80 min.
4. The method of claim 1, wherein the firing step comprises the steps of:
at a first time t 1 Internal heating to 300 deg.C, and then at a second time t 2 Internally heating to 1100 deg.C, and then making third time t 3 Internally heating to 1450 deg.C, and keeping the temperature at 1450 deg.C for a fourth time t 4 Then cooling to 300-400 ℃; t is t 1 Is 8min-12min, t 2 Is 28min-32min, t 3 Is 18min-22min, t 4 Is 10min-15 min.
5. The method for manufacturing according to any one of claims 1 to 4, wherein the step of manufacturing a green brick comprises the steps of:
forming a base layer of a blank;
preparing a ground coat on the base layer of the blank;
and forming a pattern layer on the ground glaze layer to obtain the green brick.
6. The method of manufacturing of claim 5, wherein the step of forming the green base layer comprises the steps of:
grinding the raw materials forming the base layer of the blank body to prepare slurry;
spraying the slurry to prepare powder, thus obtaining spray powder;
and forming and drying the spray powder to obtain the base layer of the blank body.
7. The preparation method of claim 6, wherein the chemical components of the spray powder comprise, by mass percent: SiO 2 2 60%-64%、Al 2 O 3 22%-26%、TiO 2 +Fe 2 O 3 0.2%-0.6%、MgO 1%-2%、CaO 0.5%-1.2%、K 2 1.5 to 2.5 percent of O and Na 2 O 2.5%-3.5%。
8. The production method according to claim 6,
in the grinding step, a ball milling method is adopted for grinding until the slurry passes through a 250-mesh screen and the rest is 0.8-1.0%;
in the step of preparing powder by spraying, controlling the water content of the sprayed powder to be 6.8-7.3%;
in the drying step, the drying temperature is 150-200 ℃, the drying is carried out until the moisture content is 0.3-0.7%, and the strength of the base layer of the blank body is controlled to be 1.8-2.2 Mpa.
9. A ceramic plate, characterized by being produced by the production method according to any one of claims 1 to 8.
10. A ceramic plate as claimed in claim 9, wherein the ceramic plate is cuboid, the thickness of the ceramic plate is 3-5mm, the width of the ceramic plate is 600-1600mm, and the length of the ceramic plate is 1200-3200 mm.
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