CN115572067A - Dry grain glaze, matte ceramic tile and preparation method thereof - Google Patents
Dry grain glaze, matte ceramic tile and preparation method thereof Download PDFInfo
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- CN115572067A CN115572067A CN202211128243.4A CN202211128243A CN115572067A CN 115572067 A CN115572067 A CN 115572067A CN 202211128243 A CN202211128243 A CN 202211128243A CN 115572067 A CN115572067 A CN 115572067A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 53
- 239000000203 mixture Substances 0.000 claims abstract description 46
- 239000000126 substance Substances 0.000 claims abstract description 37
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 33
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 28
- 230000001681 protective effect Effects 0.000 claims description 40
- 238000005498 polishing Methods 0.000 claims description 29
- 230000001680 brushing effect Effects 0.000 claims description 25
- 239000000375 suspending agent Substances 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- 238000007639 printing Methods 0.000 claims description 14
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical class O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 229910004116 SrO 2 Inorganic materials 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- RESSOZOGQXKCKT-UHFFFAOYSA-N ethene;propane-1,2-diol Chemical compound C=C.CC(O)CO RESSOZOGQXKCKT-UHFFFAOYSA-N 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001735 carboxylic acids Chemical class 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 4
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 150000002826 nitrites Chemical class 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 11
- 238000009472 formulation Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 5
- 239000008187 granular material Substances 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 23
- 238000010438 heat treatment Methods 0.000 description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 10
- 229910010271 silicon carbide Inorganic materials 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000013329 compounding Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 9
- 239000011449 brick Substances 0.000 description 8
- 230000003373 anti-fouling effect Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000007688 edging Methods 0.000 description 4
- 238000007641 inkjet printing Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000035807 sensation Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000003973 paint Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
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Abstract
The invention provides a dry grain glaze, a matte ceramic tile and a preparation method thereof. The chemical composition of the dry granular glaze comprises SiO according to the mass percentage 2 50～60％、Al 2 O 3 15～20％、K 2 O 3.5～5.5％、Na 2 O 1.5～3.0％、TiO 2 0.05～0.1％、Fe 2 O 3 0.05～0.1％、MgO 0.1～0.5％、CaO 3～5％、BaO 5～10％、SrO 3～5％、ZnO 3～4％、Rb 2 O 0.01～0.05％、B 2 O 3 0.05 to 0.1 percent. According to the dry granular glaze provided by the invention, the components and the content of the components in the dry granular glaze are adjusted and optimized, so that the glaze prepared by taking the dry granular glaze as a raw material is low in glossiness and has a matte effect; by means of SiO 2 With Al 2 O 3 The formulation is matched and the content is limited in a certain range, and the glaze surface prepared by using dry granular glaze as a raw material has a surface after high-temperature sinteringThe ceramic tile has fine granular feeling, the appearance of the granules is round and fine, the whole touch feeling is smoother, and the phenomenon of residual dirt caused by rough surface of the ceramic tile can be avoided; the color development capability of the ceramic tile glaze can be improved by introducing a certain amount of ZnO into the dry particle glaze, so that the color development effect of the glaze is more stable, and the permeability of the glaze is good.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a dry grain glaze, a matte ceramic tile and a preparation method thereof.
Background
The traditional glazed tile is generally classified into the glazed tile with two gloss effects of bright gloss and matte gloss according to the gloss degree due to the limitation of the type of the glaze formula. The glaze brick with bright surface has high glossiness and high light reflection coefficient, and most of light rays can cause certain harm to vision after being emitted, so the glaze brick is not suitable for long-term use by people. The matte glazed tile products are gradually favored by consumers because the gloss is lower and the problems are not solved.
Although the matte glazed tiles in the market have lower glossiness, the particles on the surfaces of the tiles are larger, the texture is rougher, and the hand feeling is not fine enough, so that the requirements of people cannot be met.
Disclosure of Invention
The invention provides a dry particle glaze, a matte ceramic tile and a preparation method thereof, so that the glaze of the ceramic tile is low in glossiness and has a matte effect, the particles of the glaze are fine and smooth, the hand feeling is smoother, and the phenomenon of dirt residue caused by rough surface of the ceramic tile can be avoided.
According to a first aspect of the invention, a dry granular glaze is provided, the chemical composition of which comprises SiO in percentage by mass 2 50～60％、Al 2 O 3 15～20％、K 2 O 3.5～5.5％、Na 2 O 1.5～3.0％、TiO 2 0.05～0.1％、Fe 2 O 3 0.05～0.1％、MgO 0.1～0.5％、CaO 3～5％、BaO 5～10％、SrO 3～5％、ZnO 3～4％、Rb 2 O 0.01～0.05％、B 2 O 3 0.05～0.1％。
According to the dry granular glaze provided by the invention, the components and the contents of the components in the dry granular glaze are adjusted and optimized, so that the glaze surface prepared by taking the dry granular glaze as a raw material is low in glossiness after undergoing the processes of high-temperature sintering and cooling, has a matte effect, and has good thermal stability and breaking strength. And SiO is adopted in the dry particle glaze 2 With Al 2 O 3 The ceramic tile is matched with a design formula, the content of the ceramic tile is limited in a certain range, the surface of a glaze surface prepared by using dry glaze as a raw material has fine granular sensation after being sintered at high temperature, the appearance of the granules is round and fine, the whole touch feeling is smoother, and the phenomenon that the surface of the ceramic tile is rough and dirt remains can be avoided. In addition, a certain amount of ZnO is introduced into the dry granular glaze to improve the color development of the ceramic tile glaze surfaceAnd the color development of the glaze is more stable, and the permeability of the glaze is good.
Preferably, the chemical composition of the dry granular glaze comprises SiO calculated by mass percentage 2 55.01％、Al 2 O 3 17.69％、K 2 O 4.23％、Na 2 O 2.49％、TiO 2 0.07％、Fe 2 O 3 0.08％、MgO 0.39％、CaO 4.05％、BaO 8.58％、SrO 3.95％、ZnO 3.32％、Rb 2 O 0.02％、B 2 O 3 0.07％。
According to a second aspect of the present invention, there is provided a matte ceramic tile comprising a green body, the surface of which is provided in this order with a ground coat layer, a print layer, a protective glaze layer and a matte fine dry glaze layer, wherein the matte fine dry glaze for forming the matte fine dry glaze layer contains the above dry glaze.
The matte ceramic tile provided by the scheme comprises the matte fine dry particle glaze layer, and the matte fine dry particle glaze layer comprises the dry particle glaze provided by the invention, so that the glaze of the ceramic tile has the characteristics of low glossiness and strong color development capability, the ceramic tile glaze has a matte effect, the particles on the surface of the ceramic tile glaze are fine and smooth, the hand feeling is smooth, and the phenomenon of dirt residue caused by rough surface of the ceramic tile can be avoided.
Preferably, the matte fine dry particle glaze also contains a suspending agent; in the matte fine dry glaze, the mass ratio of the dry glaze to the suspending agent is as follows: suspending agent = (30 to 50): (90-110).
Preferably, the suspending agent comprises a polar organic, a nitrite, and a modified bentonite;
calculating polar organic matters according to parts by mass: nitrite salt: modified bentonite = 55-65: 1 to 5:5 to 10;
the polar organic matter comprises alcohol materials and carboxylic acid materials;
the alcohol material comprises at least one of ethylene glycol, propylene glycol and ethylene propylene glycol polymer;
the carboxylic acid materials comprise acetic acid;
the modified bentonite is prepared from modified cellulose ester and aluminum silicate bentonite.
According to the scheme, the dry particle glaze and the suspending agent containing specific components are compounded to obtain the matte fine dry particle glaze, and the matte fine dry particle glaze is used for preparing the ceramic tile, so that the ceramic tile glaze has low glossiness and antifouling property. Moreover, the suspending agent adopted by the scheme is favorable for improving the suspending effect of the dry particle glaze, can prevent the dry particles in the matte fine dry particle glaze from agglomeration, is favorable for improving the polishing uniformity of a subsequent glaze layer, and further improves the antifouling property of the glaze layer.
Preferably, the chemical composition of the protective glaze used for forming the protective glaze layer comprises SiO in mass percent 2 45～50％、Al 2 O 3 15～20％、K 2 O 0.1～0.4％、Na 2 O 1～2％、TiO 2 0.1～0.4％、ZrO 2 0.05～0.1％、Fe 2 O 3 0.10～0.15％、MgO 0.5～1.5％、CaO 0.45～0.50％、BaO 22～23％、SrO 0.05～0.1％、ZnO 5～6％、P 2 O 5 0.15～0.20％。
Preferably, the chemical composition of the protective glaze used for forming the protective glaze layer comprises SiO in mass percent 2 48％、Al 2 O 3 16.9％、K 2 O 0.25％、Na 2 O 1.48％、TiO 2 0.23％、ZrO 2 0.08％、Fe 2 O 3 0.12％、MgO 1.0％、CaO 0.48％、BaO 22.52％、SrO 0.08％、ZnO 5.75％、P 2 O 5 0.17％。
Preferably, the chemical composition of the ground coat for forming the ground coat layer comprises SiO, calculated on a mass percentage basis 2 50～55％、Al 2 O 3 33～38％、K 2 O 2～2.5％、Na 2 O 4.5～5.5％、TiO 2 0.01～0.07％、SrO 2 0.03～0.09％、Fe 2 O 3 0.15～0.20％、MgO 0.45～0.60％、CaO 1.0～1.3％、BaO 0.10～0.18％、ZnO 0.1～0.3％、P 2 O 5 0.01～0.05％。
Preferably, the chemical composition of the ground coat for forming the ground coat layer comprises SiO, calculated in mass percentage 2 53.33％、Al 2 O 3 35.27％、K 2 O 2.29％、Na 2 O 5.05％、TiO 2 0.04％、SrO 2 0.06％、Fe 2 O 3 0.18％、MgO 0.52％、CaO 1.14％、BaO 0.14％、ZnO 0.2％、P 2 O 5 0.03％。
According to a third aspect of the present invention, there is provided a process for preparing the above matt ceramic tile, comprising the steps of:
step one, applying a ground coat on the surface of a blank body for forming a ground coat layer;
step two, manufacturing a printing layer on the surface of the blank body after the base glaze cloth is applied;
step three, laying a protective glaze on the surface of the printing layer for forming a protective glaze layer;
step four, laying Shi Yaguang fine dry grain glaze on the surface of the blank subjected to protective glaze laying for forming a matte fine dry grain glaze layer;
and fifthly, firing the blank body, brushing and polishing to obtain the matte ceramic tile.
Preferably, in the step one, the glaze specific gravity of the ground glaze is 1.9-2.0 g/cm 3 。
Preferably, in the step one, the operation of applying the ground coat is carried out in such a way that the applying amount of the ground coat on the surface of the blank body is 350-500 g/m 2 。
Preferably, in the third step, the operation of applying the protective glaze is carried out in such a way that the glazing amount of the protective glaze on the surface of the blank body is 60-95 g/m 2 。
Preferably, in the fourth step, the operation of applying the matte fine dry particle glaze is performed in such a way that the glazing amount of the matte fine dry particle glaze on the surface of the blank body is 200-300 g/m 2 。
Preferably, in the fifth step, the firing temperature is 1165-1175 ℃, and the firing time is 45-65 minutes.
Preferably, in the fifth step, the fired green body is brushed and polished by using a soft polishing mold, and the number of brushing and polishing meshes is 1200-1800 meshes.
Preferably, in step five, the soft brush polishing mold is a silicon carbide mold brush.
Preferably, in step five, the specific operation of brushing and polishing is as follows: and (3) carrying out dispersion brushing and polishing on the surface of the sintered blank for 2-3 minutes by adopting 6 groups of silicon carbide mould brushes with 1200 meshes and 6 groups of 1800 meshes.
Drawings
Fig. 1 is a structural side view of the finished matte ceramic tile provided by the invention.
The reference signs are: 1 blank, 2 ground glaze layers, 3 printing layers, 4 protective glaze layers and 5 matte fine dry grain glaze layers.
Fig. 2 is a schematic diagram of a substance before the matte ceramic tile prepared in embodiment 1 of the present invention is brushed and polished.
FIG. 3 is a schematic view of a brushed matte ceramic tile manufactured in example 1 of the present invention.
Fig. 4 is a schematic diagram of a substance before the matte ceramic tile prepared in embodiment 2 of the present invention is brushed and polished.
Fig. 5 is a schematic view of a brushed matte ceramic tile manufactured in embodiment 2 of the present invention.
FIG. 6 is a schematic view of a finished product of a matte ceramic tile manufactured in example 4 of the present invention.
FIG. 7 is a schematic representation of a finished matte ceramic tile prepared in comparative example 1.
FIG. 8 is a schematic view of a finished product of the matte ceramic tile of comparative example 2.
Detailed Description
Technical features in the technical solutions provided by the present invention are further clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In this embodiment, the chemical composition of the materials involved is as follows, calculated by mass percent:
the chemical composition of the dry granular glaze comprises SiO 2 55.01％、Al 2 O 3 17.69％、K 2 O 4.23％、Na 2 O 2.49％、TiO 2 0.07％、Fe 2 O 3 0.08％、MgO 0.39％、CaO 4.05％、BaO 8.58％、SrO 3.95％、ZnO 3.32％、Rb 2 O 0.02％、B 2 O 3 0.07％。
The chemical composition of the protective glaze comprises SiO 2 48％、Al 2 O 3 16.9％、K 2 O 0.25％、Na 2 O 1.48％、TiO 2 0.23％、ZrO 2 0.08％、Fe 2 O 3 0.12％、MgO 1.0％、CaO 0.48％、BaO 22.52％、SrO 0.08％、ZnO 5.75％、P 2 O 5 0.17％。
The chemical composition of the ground glaze comprises SiO 2 53.33％、Al 2 O 3 35.27％、K 2 O 2.29％、Na 2 O 5.05％、TiO 2 0.04％、SrO 2 0.06％、Fe 2 O 3 0.18％、MgO 0.52％、CaO 1.14％、BaO 0.14％、ZnO 0.2％、P 2 O 5 0.03％。
This example prepares matte tiles as follows:
the method comprises the following steps: according to 400g/m 2 The base glaze is applied on the surface of the blank body for forming a base glaze layer.
Step two: and (3) manufacturing a printing layer on the surface of the blank body after the ground coat cloth is applied by using the color ink in an intelligent ink-jet printing mode.
Step three: according to 62.5g/m 2 The amount of the protective glaze is applied to form a protective glaze layer by applying the protective glaze on the surface of the green body on which the print layer is formed.
Step four: according to 250g/m 2 The coating amount of (2) is that Shi Yaguang fine dry grain glaze is coated on the surface of the blank coated with the protective glaze and is used for forming a matte fine dry grain glaze layer; the matte fine dry particle glaze adopted in the step is prepared from dry particle glaze and a suspending agent according to the weight ratio of 40: mixing and compounding according to the mass ratio of 100; the suspending agent is prepared by compounding 47 parts of ethylene propylene glycol polymer, 12 parts of acetic acid, 3 parts of nitrite, 8 parts of modified bentonite and a proper amount of water according to parts by mass.
Step five: and transferring the blank body after the operation to a heating kiln, heating the blank body, and sintering the blank body at the temperature of 1172 ℃ for 55 minutes.
Step six: and (3) dispersing, brushing and polishing the surface of the fired green brick for 2-3 minutes by adopting 6 groups of 1200-mesh and 6 groups of 1800-mesh silicon carbide mould brushes, and edging after brushing and polishing to obtain the finished matte ceramic tile product of the embodiment.
The side view of the structure of the finished matte ceramic tile manufactured in this example is shown in fig. 1, and a bottom glaze layer 2, a printing layer 3, a protective glaze layer 4 and a matte fine dry grain glaze layer 5 are sequentially compounded on the surface of a blank body 1.
The schematic diagram of the matte ceramic tile prepared in this embodiment before brushing and polishing is shown in fig. 2, and the schematic diagram of the matte ceramic tile after brushing and polishing is shown in fig. 3.
Example 2
In this embodiment, the chemical composition of the materials involved is as follows, calculated by mass percent:
the chemical composition of the dry granular glaze comprises SiO 2 60％、Al 2 O 3 15％、K 2 O 5.5％、Na 2 O 3％、TiO 2 0.05％、Fe 2 O 3 0.05％、MgO 0.1％、CaO 3％、BaO 5％、SrO 3％、ZnO 4％、Rb 2 O 0.01％、B 2 O 3 0.05％。
The chemical composition of the protective glaze comprises SiO 2 50％、Al 2 O 3 15％、K 2 O 0.1％、Na 2 O 2％、TiO 2 0.1％、ZrO 2 0.05％、Fe 2 O 3 0.1％、MgO 0.5％、CaO 0.45％、BaO 23％、SrO 0.05％、ZnO 5％、P 2 O 5 0.15％。
The chemical composition of the ground glaze comprises SiO 2 55％、Al 2 O 3 33％、K 2 O 2％、Na 2 O 5.5％、TiO 2 0.01％、SrO 2 0.03％、Fe 2 O 3 0.15％、MgO 0.45％、CaO 1.0％、BaO 0.10％、ZnO 0.1％、P 2 O 5 0.01％。
This example prepares matte tiles as follows:
step one: according to 350g/m 2 The base glaze is applied on the surface of the blank body for forming a base glaze layer.
Step two: and (3) manufacturing a printing layer on the surface of the blank body after the ground coat cloth is applied by using the color ink in an intelligent ink-jet printing mode.
Step three: according to 60g/m 2 The amount of the protective glaze is applied to form a protective glaze layer by applying the protective glaze on the surface of the green body on which the print layer is formed.
Step four: according to 200g/m 2 The glaze applying amount of (3) is that Shi Yaguang fine dry grain glaze is applied on the surface of the blank body on which the protective glaze is applied to form a matte fine dry grain glaze layer; the matte fine dry particle glaze adopted in the step is prepared from dry particle glaze and a suspending agent according to the weight ratio of 30:110 by mass ratio; the suspending agent is prepared by compounding 45 parts of ethylene propylene glycol polymer, 10 parts of acetic acid, 1 part of nitrite, 5 parts of modified bentonite and a proper amount of water according to parts by mass.
Step five: and transferring the blank body after the operation to a heating kiln, heating the blank body, and sintering the blank body for 65 minutes at the temperature of 1165 ℃.
Step six: and (3) dispersing, brushing and polishing the surface of the baked green brick for 2-3 minutes by adopting 6 groups of silicon carbide mould brushes with 1200 meshes and 6 groups of silicon carbide mould brushes with 1800 meshes, and edging after brushing and polishing to obtain the finished matte ceramic tile product of the embodiment.
The side view of the structure of the finished matt ceramic tile manufactured in this embodiment is shown in fig. 1, and a base glaze layer 2, a printing layer 3, a protective glaze layer 4 and a matt fine dry grain glaze layer 5 are sequentially compounded on the surface of a blank 1.
The schematic diagram of the matte ceramic tile prepared in this embodiment before brushing and polishing is shown in fig. 4, and the schematic diagram of the matte ceramic tile after brushing and polishing is shown in fig. 5.
Example 3
In this embodiment, the chemical composition of the materials involved is as follows, calculated by mass percent:
the chemical composition of the dry granular glaze comprises SiO 2 50％、Al 2 O 3 20％、K 2 O 3.5％、Na 2 O 1.5％、TiO 2 0.1％、Fe 2 O 3 0.1％、MgO 0.5％、CaO 5％、BaO 10％、SrO 5％、ZnO 3％、Rb 2 O 0.05％、B 2 O 3 0.1％。
The chemical composition of the protective glaze comprises SiO 2 45％、Al 2 O 3 20％、K 2 O 0.4％、Na 2 O 1％、TiO 2 0.4％、ZrO 2 0.1％、Fe 2 O 3 0.15％、MgO 1.5％、CaO 0.50％、BaO 22％、SrO 0.1％、ZnO 6％、P 2 O 5 0.20％。
The chemical composition of the ground glaze comprises SiO 2 50％、Al 2 O 3 38％、K 2 O 2.5％、Na 2 O 4.5％、TiO 2 0.07％、SrO 2 0.09％、Fe 2 O 3 0.20％、MgO 0.60％、CaO 1.3％、BaO 0.18％、ZnO 0.3％、P 2 O 5 0.05％。
This example prepares matte tiles as follows:
the method comprises the following steps: according to 500g/m 2 The base glaze is applied on the surface of the blank body for forming a base glaze layer.
Step two: and (3) manufacturing a printing layer on the surface of the blank body on which the ground coat is applied by using the color ink in an intelligent ink-jet printing mode.
Step three: according to 95g/m 2 The amount of the protective glaze is applied to form a protective glaze layer by applying the protective glaze on the surface of the green body on which the print layer is formed.
Step four: according to 300g/m 2 The glaze applying amount of (3) is that Shi Yaguang fine dry grain glaze is applied on the surface of the blank body on which the protective glaze is applied to form a matte fine dry grain glaze layer; the matte fine dry particle glaze adopted in the step is prepared from dry particle glaze and a suspending agent according to the weight ratio of 50:90, mixing and compounding; the suspending agent is prepared by compounding 50 parts of ethylene propylene glycol polymer, 15 parts of acetic acid, 5 parts of nitrite, 10 parts of modified bentonite and a proper amount of water according to parts by mass.
Step five: and transferring the blank body after the operation to a heating kiln, heating the blank body, and sintering the blank body at the temperature of 1175 ℃ for 45 minutes.
Step six: and (3) dispersing, brushing and polishing the surface of the baked green brick for 2-3 minutes by adopting 6 groups of silicon carbide mould brushes with 1200 meshes and 6 groups of silicon carbide mould brushes with 1800 meshes, and edging after brushing and polishing to obtain the finished matte ceramic tile product of the embodiment.
The side view of the structure of the finished matte ceramic tile manufactured in this example is shown in fig. 1, and a bottom glaze layer 2, a printing layer 3, a protective glaze layer 4 and a matte fine dry grain glaze layer 5 are sequentially compounded on the surface of a blank body 1.
Example 4
This example prepares matte tiles with reference to example 1. Compared with the embodiment 1, the difference of the structure is that the matte fine dry particle glaze adopted by the embodiment is prepared by mixing dry particle glaze and suspending agent according to the weight ratio of 40:130, mixing and compounding. Except for the above differences, the materials, formulation ratios and preparation operations used in this example were strictly consistent with those of example 1.
The schematic diagram of the finished product of the matte ceramic tile prepared in this example is shown in fig. 6.
Example 5
This example prepares matte tiles with reference to example 1. Compared with the embodiment 1, the difference of the structure is that the matte fine dry particle glaze adopted by the embodiment is prepared by mixing dry particle glaze and suspending agent according to the weight ratio of 20:100, mixing and compounding. Except for the above differences, the materials, formulation ratios and preparation operations used in this example were strictly consistent with those of example 1.
Example 6
In this embodiment, the chemical composition of the materials involved is as follows, calculated by mass percent:
the chemical composition of the dry granular glaze comprises SiO 2 55.01％、Al 2 O 3 17.69％、K 2 O 4.23％、Na 2 O 2.49％、TiO 2 0.07％、Fe 2 O 3 0.08％、MgO 0.39％、CaO 4.05％、BaO 8.58％、SrO 3.95％、ZnO 3.32％、Rb 2 O 0.02％、B 2 O 3 0.07％。
The chemical composition of the protective glaze comprises SiO 2 48％、Al 2 O 3 16.9％、K 2 O 0.25％、Na 2 O 1.48％、TiO 2 0.23％、ZrO 2 0.08％、Fe 2 O 3 0.12％、MgO 1.0％、CaO 0.48％、BaO 22.52％、SrO 0.08％、ZnO 5.75％、P 2 O 5 0.17％。
The chemical composition of the ground glaze comprises SiO 2 53.33％、Al 2 O 3 35.27％、K 2 O 2.29％、Na 2 O 5.05％、TiO 2 0.04％、SrO 2 0.06％、Fe 2 O 3 0.18％、MgO 0.52％、CaO 1.14％、BaO 0.14％、ZnO 0.2％、P 2 O 5 0.03％。
This example prepares matte tiles as follows:
the method comprises the following steps: according to 400g/m 2 The base glaze is applied on the surface of the blank body for forming a base glaze layer.
Step two: and (3) manufacturing a printing layer on the surface of the blank body on which the ground coat is applied by using the color ink in an intelligent ink-jet printing mode.
Step three: according to 250g/m 2 The coating amount of (2) is that Shi Yaguang fine dry grain glaze is coated on the surface of the blank coated with the protective glaze and is used for forming a matte fine dry grain glaze layer; the matte fine dry particle glaze adopted in the step is prepared from dry particle glaze, a suspending agent and a protective glaze according to the weight ratio of 40:100: mixing and compounding according to the mass ratio of 50; the suspending agent is prepared by compounding 47 parts of ethylene propylene glycol polymer, 12 parts of acetic acid, 3 parts of nitrite, 8 parts of modified bentonite and a proper amount of water according to parts by mass.
Step four: and transferring the blank body after the operation to a heating kiln, heating the blank body, and sintering the blank body at the temperature of 1172 ℃ for 55 minutes.
Step five: and (3) dispersing, brushing and polishing the surface of the baked green brick for 2-3 minutes by adopting 6 groups of silicon carbide mould brushes with 1200 meshes and 6 groups of silicon carbide mould brushes with 1800 meshes, and edging after brushing and polishing to obtain the finished matte ceramic tile product of the embodiment.
The surface of the body of the finished matte ceramic tile product prepared in this example was compounded with a ground glaze layer, a printed layer, and a matte fine dry grain glaze layer in this order.
Example 7
This example prepares matte tiles with reference to example 1. Compared with the embodiment 1, the difference of the structure is that the ground coat adopted in the embodiment is different, and the ground coat adopted in the embodiment is SiO 2 58.44％、Al 2 O 3 30.24％、K 2 O 0.75％、Na 2 O 4.85％、TiO 2 0.07％、SrO 2 0.02％、Fe 2 O 3 0.19％、MgO 1.75％、CaO 0.75％、BaO 0.04％、ZnO 0.02％、P 2 O 5 0.04 percent. Except for the above differences, the materials, formulation ratios and preparation operations used in this example were strictly consistent with those of example 1.
Example 8
This example prepares matte tiles according to example 1. Compared with the embodiment 1, the difference of the structure is that the ground coat adopted in the embodiment is different, and the ground coat adopted in the embodiment is SiO 2 59.42％、Al 2 O 3 30.06％、Fe 2 O 3 0.15％、TiO 2 0.01％、ZrO 2 0.1％、CaO 1.59％、MgO 1.6％、K 2 O 1.39％、Na 2 O 3.00％、ZnO 0.5％、P 2 O 5 0.18 percent. Except for the above differences, the materials, formulation ratios and preparation operations used in this example were strictly consistent with those of example 1.
Example 9
This example prepares matte tiles with reference to example 1. Compared with the embodiment 1, the difference of the structure is that the firing process adopted in the step five of preparing the matte ceramic tile is different, specifically: and transferring the blank body after the operation to a heating kiln, heating the blank body, and sintering the blank body at the temperature of 1200 ℃ for 55 minutes. Except for the above differences, the materials, formulation ratios and preparation operations used in this example were strictly consistent with those of example 1.
Example 10
This example prepares matte tiles with reference to example 1. Compared with the embodiment 1, the difference of the composition is that the brushing and polishing process adopted in the sixth step of preparing the matte ceramic tile is different, and specifically comprises the following steps: and (3) performing dispersed brushing and polishing on the surface of the baked green brick for 2-3 minutes by adopting 12 groups of 1200-mesh silicon carbide mould brushes, and performing edge grinding after brushing and polishing to obtain the finished matte ceramic tile product of the embodiment. Except for the above differences, the materials, formulation ratios and preparation operations used in this example were strictly consistent with those of example 1.
Comparative example 1
This comparative example prepares matte tiles with reference to example 1. Compared with the example 1, the difference of the constitution is that the chemical composition of the dry particle glaze adopted in the comparative example is different in the process of preparing the matte fine particle glaze layer, and the chemical composition of the dry particle glaze adopted in the comparative example comprises SiO according to the mass percentage 2 47.8％、Al 2 O 3 12.5％、K 2 O 4.23％、Na 2 O 2.49％、TiO 2 0.07％、Fe 2 O 3 0.08％、MgO 0.39％、CaO 4.05％、BaO 8.58％、SrO 3.95％、ZnO 3.32％、Rb 2 O 0.02％、B 2 O 3 0.07 percent. Except for the above differences, the materials, formulation ratios and preparation operations used in this comparative example were strictly consistent with those of example 1.
The schematic diagram of the finished product of the matte ceramic tile prepared in the comparative example is shown in FIG. 7.
Comparative example 2
This comparative example makes a matt ceramic tile with reference to example 1. Compared with the example 1, the difference of the constitution is that the chemical composition of the dry particle glaze adopted in the comparative example is different in the process of preparing the matte fine particle glaze layer, and the chemical composition of the dry particle glaze adopted in the comparative example comprises SiO according to the mass percentage 2 68.5％、Al 2 O 3 26％、K 2 O 4.23％、Na 2 O 2.49％、TiO 2 0.07％、Fe 2 O 3 0.08％、MgO 0.39％、CaO 4.05％、BaO 8.58％、SrO 3.95％、ZnO 3.32％、Rb 2 O 0.02％、B 2 O 3 0.07 percent. Except for the above differences, the materials, formulation ratios and preparation operations used in this comparative example were strictly consistent with those of example 1.
The schematic diagram of the finished product of the matte ceramic tile prepared in the comparative example is shown in FIG. 8.
Comparative example 3
This comparative example prepares matte tiles with reference to example 1. Compared with the example 1, the difference of the constitution is that the chemical composition of the dry particle glaze adopted in the comparative example is different in the process of preparing the matte fine particle glaze layer, and the chemical composition of the dry particle glaze adopted in the comparative example comprises SiO according to the mass percentage 2 52.05％、Al 2 O 3 18.50％、K 2 O 3.18％、Na 2 O 3.33％、TiO 2 0.03％、Fe 2 O 3 0.09％、MgO 1.25％、CaO 5.78％、BaO 0.05％、SrO 5.51％、ZnO 8.45％、Rb 2 O 0.13％、Li 2 0.51 percent of O. Except for the above differences, the materials, formulation ratios and preparation operations used in this comparative example were strictly consistent with those of example 1.
Test example
1. Reference object
The matte tiles obtained in examples 1 to 10 and comparative examples 1 to 3 were used as the reference of the test examples.
2. Test items
The test items of the test example include the thermal stability, glossiness, antifouling performance, glaze display effect, and breaking strength of the test object.
Thermal stability: taking a sample of a finished ceramic tile product with the size of 15cm multiplied by 15cm, putting the sample into an oven with the temperature of 180 ℃, taking out the sample after placing the sample for 20 minutes, then putting the sample into cold water (running water at normal temperature) for cooling for 15 minutes, then wiping the surface of the ceramic tile with oily ink to observe whether cracks exist, repeating the operation for 3 times, wherein the thermal stability is qualified if the surface of the ceramic tile does not have cracks, and the thermal stability is unqualified if the surface of the ceramic tile has cracks.
Breaking strength (breaking strength): refer to the national standard GB/T4100-2015.
Gloss: the gloss of a tile surface refers to the ability of the tile surface to reflect light. The gloss of the tile surface was measured by means of a gloss meter model WGG60-Y4 manufactured by Koshijia photoelectric instruments, ltd.
Antifouling performance: adopt black pen ink evenly to paint on the ceramic tile brick face after the polishing wax removal, afterwards with stepping on the mode and carrying out destructive processing, treat ceramic tile surface's ink test 24 hours after, wash with clear water and rag to the change of product glaze effect before and after the contrast test.
3. Test results
The heat stability, glossiness, antifouling property, glaze display effect, and bending strength of the subjects to be tested are shown in table 1.
Table 1 various property tests of the tiles
The surface of the body of the finished matt ceramic tile prepared in example 1 is sequentially compounded with a ground glaze layer, a printing layer, a protective glaze layer and a matt fine dry grain glaze layer, and in the process of preparing the matt ceramic tile, the matt fine dry grain glaze for forming the matt fine dry grain glaze layer is prepared from dry grain glaze and a suspending agent according to the weight ratio of 40:100, and the glazing amount of the matte fine dry particle glaze is 250g/m 2 The ceramic tile is sintered for 65 minutes at 1165 ℃, and then the baked green tile is dispersed and brushed by adopting 6 groups of 1200-mesh and 6 groups of 1800-mesh soft brushing and polishing modules, so that the finally obtained matt ceramic tile glaze has low glossiness, good thermal stability and flexural strength, uniform and fine glaze particles, more distribution, smoothness, fineness and good antifouling property. Compared with the example 1, the matte ceramic tiles prepared in the examples 2 and 3 have small number of particles although the glaze surface particles are uniform, fine, smooth and fine.
Compared with the embodiment 1, in the embodiments 4 to 5, in the process of preparing the matt ceramic tile, the mass ratio of the dry glaze to the suspending agent in the matt fine dry glaze layer for forming the matt fine dry glaze layer is different, and is 40: 130. 20:100, the glossiness of the finally prepared matte ceramic tile is slightly higher than that of the ceramic tile in the embodiment 1, and the distribution of glaze particles is extremely small.
The surface of the body of the finished matte ceramic tile product prepared in example 6 is sequentially compounded with a ground glaze layer, a printed layer and a matte fine dry-grained glaze layer, and in the process of preparing the matte ceramic tile, the matte fine dry-grained glaze used for forming the matte fine dry-grained glaze layer is prepared from a matte fine dry-grained glaze, a suspending agent and a protective glaze according to the weight ratio of 40:100:50, the glossiness of the finally prepared matte ceramic tile is obviously higher than that of the ceramic tile in the embodiment 1, and the glaze particles are rough and not fine in hand feeling.
In the preparation process of the matte ceramic tiles of the embodiments 7 to 8, the adopted ground coat has different chemical composition and content from those of the embodiment 1, the folding strength of the finally prepared matte ceramic tiles is lower than that of the embodiment 1, and the glaze particles are not uniformly distributed.
The firing temperature adopted in the preparation process of the matte ceramic tile in the embodiment 9 is 1200 ℃, which is higher than that in the embodiment 1, and the finally prepared matte ceramic tile has poor thermal stability and antifouling property, and the glaze surface has coarse particles and extremely wrinkled glaze surface.
In the preparation process of the matte ceramic tile in the embodiment 10, 12 groups of 1200-mesh soft brushing and polishing modules are adopted to perform dispersed brushing and polishing on the baked green tile, so that the matte degree of the finally prepared matte ceramic tile is obviously higher than that of the matte ceramic tile in the embodiment 1, and the glaze surface has no granular feeling.
Matte tile of comparative example 1, using SiO in dry-grain glaze during the preparation 2 And Al 2 O 3 The content of (A) is lower than that of example 1, the matte degree of the finally prepared matte ceramic tile is obviously higher than that of example 1, and the glaze surface has no granular feeling.
Matte tile of comparative example 2, using SiO in dry-grain glaze during the preparation 2 And Al 2 O 3 The content of (A) is higher than that of example 1, the matte degree of the finally prepared matte ceramic tile is equivalent to that of example 1, but the glaze surface particles are large.
In the preparation process of the matte ceramic tile in the comparative example 3, the chemical composition and the content of the dry granular glaze are different from those in the example 1, the glossiness of the finally prepared matte ceramic tile is obviously higher than that in the example 1, the distribution of glaze particles is extremely small, and the particles are extremely small.
In conclusion, the dry granular glaze provided by the invention has the advantages that the components and the content of the components in the dry granular glaze are adjusted and optimized, so that the glaze surface prepared by using the dry granular glaze as a raw material has low glossiness after the processes of high-temperature sintering and cooling, has a matte effect, and has good thermal stability and breaking strength. And SiO is adopted in the dry particle glaze 2 With Al 2 O 3 The ceramic tile is matched with a design formula, the content of the ceramic tile is limited in a certain range, the surface of a glaze surface prepared by using dry glaze as a raw material has fine granular sensation after being sintered at high temperature, the appearance of the granules is round and fine, the whole touch feeling is smoother, and the phenomenon that the surface of the ceramic tile is rough and dirt remains can be avoided.
Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A dry particle glaze is characterized in that: the chemical composition of the dry granular glaze comprises SiO according to the mass percentage 2 50～60％、Al 2 O 3 15～20％、K 2 O 3.5～5.5％、Na 2 O 1.5～3.0％、TiO 2 0.05～0.1％、Fe 2 O 3 0.05～0.1％、MgO 0.1～0.5％、CaO 3～5％、BaO 5～10％、SrO 3～5％、ZnO 3～4％、Rb 2 O 0.01～0.05％、B 2 O 3 0.05～0.1％。
2. The dry-grain glaze of claim 1, wherein: the chemical composition of the dry granular glaze comprises SiO according to the mass percentage 2 55.01％、Al 2 O 3 17.69％、K 2 O 4.23％、Na 2 O 2.49％、TiO 2 0.07％、Fe 2 O 3 0.08％、MgO 0.39％、CaO 4.05％、BaO 8.58％、SrO 3.95％、ZnO 3.32％、Rb 2 O 0.02％、B 2 O 3 0.07％。
3. A matte ceramic tile is characterized in that:
the matte ceramic tile comprises a green body, wherein a ground glaze layer, a printing layer, a protective glaze layer and a matte fine dry particle glaze layer are sequentially arranged on the surface of the green body, wherein the matte fine dry particle glaze for forming the matte fine dry particle glaze layer contains the dry particle glaze as claimed in any one of claims 1-2.
4. The matte tile of claim 3, wherein:
the matte fine dry particle glaze also contains a suspending agent;
in the matte fine dry glaze, the mass ratio of the dry glaze to the suspending agent is as follows: the suspending agent = (30 to 50): (90-110).
5. The matte tile of claim 4, wherein:
the suspending agent comprises a polar organic matter, nitrite and modified bentonite;
the polar organic matter is calculated according to the mass parts: the nitrite salt: the modified bentonite = 55-65: 1 to 5:5 to 10;
the polar organic matter comprises an alcohol material and a carboxylic acid material;
the alcohol material comprises at least one of ethylene glycol, propylene glycol and ethylene propylene glycol polymer;
the carboxylic acid material comprises acetic acid;
the modified bentonite is prepared from modified cellulose ester and aluminum silicate bentonite.
6. The matte tile of claim 3, wherein:
the chemical composition of the protective glaze for forming the protective glaze layer comprises SiO according to mass percentage 2 45～50％、Al 2 O 3 15～20％、K 2 O 0.1～0.4％、Na 2 O 1～2％、TiO 2 0.1～0.4％、ZrO 2 0.05～0.1％、Fe 2 O 3 0.10～0.15％、MgO 0.5～1.5％、CaO 0.45～0.50％、BaO 22～23％、SrO 0.05～0.1％、ZnO 5～6％、P 2 O 5 0.15～0.20％。
7. A matte ceramic tile according to claim 3, wherein:
the chemical composition of the ground coat for forming the ground coat layer comprises SiO according to the mass percentage 2 50～55％、Al 2 O 3 33～38％、K 2 O 2～2.5％、Na 2 O 4.5～5.5％、TiO 2 0.01～0.07％、SrO 2 0.03～0.09％、Fe 2 O 3 0.15～0.20％、MgO 0.45～0.60％、CaO 1.0～1.3％、BaO 0.10～0.18％、ZnO 0.1～0.3％、P 2 O 5 0.01～0.05％。
8. A process for the preparation of a matte ceramic tile according to any one of claims 3 to 7, comprising the following steps:
step one, applying a ground coat on the surface of the blank body for forming the ground coat layer;
step two, manufacturing the printing layer on the surface of the blank body after the base glaze cloth is applied;
step three, laying a protective glaze on the surface of the printing layer for forming the protective glaze layer;
step four, distributing the matte fine dry grain glaze on the surface of the blank after the protective glaze is distributed, and forming the matte fine dry grain glaze layer;
and fifthly, firing the blank body, and brushing and polishing to obtain the matte ceramic tile.
9. A process for the preparation of matte ceramic tiles according to claim 8, wherein: in the fifth step, the firing temperature is 1165-1175 ℃, and the firing time is 45-65 minutes.
10. A process for the preparation of matte ceramic tiles according to claim 8, wherein: and in the fifth step, brushing and polishing the fired green body by using a soft polishing mould, wherein the number of brushing and polishing meshes is 1200-1800 meshes.
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