CN111646788B - Large-size ceramic rock plate and preparation method thereof - Google Patents
Large-size ceramic rock plate and preparation method thereof Download PDFInfo
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- CN111646788B CN111646788B CN202010440305.XA CN202010440305A CN111646788B CN 111646788 B CN111646788 B CN 111646788B CN 202010440305 A CN202010440305 A CN 202010440305A CN 111646788 B CN111646788 B CN 111646788B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 95
- 239000011435 rock Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title description 11
- 239000012745 toughening agent Substances 0.000 claims abstract description 39
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 20
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 20
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 229910052903 pyrophyllite Inorganic materials 0.000 claims abstract description 15
- 229910052656 albite Inorganic materials 0.000 claims abstract description 13
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 33
- 238000010304 firing Methods 0.000 claims description 32
- 238000003825 pressing Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 13
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052839 forsterite Inorganic materials 0.000 claims description 10
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052863 mullite Inorganic materials 0.000 claims description 10
- MKTRXTLKNXLULX-UHFFFAOYSA-P pentacalcium;dioxido(oxo)silane;hydron;tetrahydrate Chemical class [H+].[H+].O.O.O.O.[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O MKTRXTLKNXLULX-UHFFFAOYSA-P 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 7
- 238000001694 spray drying Methods 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- 238000007641 inkjet printing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229920003086 cellulose ether Polymers 0.000 claims description 3
- 150000004676 glycans Chemical class 0.000 claims description 3
- 229920005610 lignin Polymers 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 229920001282 polysaccharide Polymers 0.000 claims description 3
- 239000005017 polysaccharide Substances 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- 239000010454 slate Substances 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 23
- 239000002253 acid Substances 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 description 13
- 230000035882 stress Effects 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 230000006872 improvement Effects 0.000 description 9
- 238000005520 cutting process Methods 0.000 description 8
- 239000004575 stone Substances 0.000 description 7
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000005034 decoration Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
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- 230000000694 effects Effects 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000011527 polyurethane coating Substances 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 241001122767 Theaceae Species 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910001607 magnesium mineral Inorganic materials 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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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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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
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- 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
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- 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
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
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- 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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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F13/00—Coverings or linings, e.g. for walls or ceilings
- E04F13/07—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor
- E04F13/08—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements
- E04F13/0871—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements having an ornamental or specially shaped visible surface
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- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F13/00—Coverings or linings, e.g. for walls or ceilings
- E04F13/07—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor
- E04F13/08—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements
- E04F13/14—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements stone or stone-like materials, e.g. ceramics concrete; of glass or with an outer layer of stone or stone-like materials or glass
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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Abstract
The invention discloses a large-size ceramic rock plate, the surface area of which is 3-12 m2The thickness is 12-30 mm; it comprises a body layer, a ground glaze layer, a pattern layer and a surface glaze layer; the thickness of the blank layer is 11.5-29.5 mm; the green body layer is mainly prepared from the following raw materials in parts by weight: 15-20 parts of potassium feldspar, 8-15 parts of albite, 15-20 parts of calcined kaolin, 12-20 parts of black mud, 8-15 parts of white mud, 15-20 parts of pyrophyllite and 1-10 parts of a toughening agent; the sum of the parts by weight of the raw materials is 100 parts. The ceramic rock plate can be well adapted to the later-stage deep processing technology, can be widely applied to the fields of floors, curtain walls and veneers, and has the advantages of high strength, high hardness, acid and alkali resistance, high temperature resistance and the like.
Description
Technical Field
The invention relates to the field of ceramic tiles, in particular to a large-size ceramic rock plate and a preparation method thereof.
Background
Along with the improvement of the living standard of people, the beauty is more and more personalized in the selection of decoration and finishing materials, the style and the taste are more emphasized, and the application requirements of the finishing materials such as wall and floor, curtain walls, furniture, cabinets, deck boards and the like in modern decoration are more and more increased. The existing facing materials mainly comprise natural stones and artificial quartz stones. The artificial quartz stone is a plate formed by vibrating and pressing resin, quartz and a pigment and curing at 100-200 ℃, and has low hardness, poor acid and alkali resistance and no high temperature resistance due to the resin material. Although natural stone has relatively high hardness, good high temperature resistance and rich color, natural stone resources are extremely limited.
In recent years, ceramic large panels are increasingly being used in the field of decoration,the high-temperature-resistant polyurethane coating has the advantages of excellent acid and alkali resistance, high hardness (the Mohs hardness on the surface can reach more than 6 grade), high temperature resistance and the like, and therefore, the high-temperature-resistant polyurethane coating has a very wide application prospect. According to the regulation of national standard (GB/T23266-2009), the surface area of the ceramic plate is not less than 1.62 m2The thickness is not more than 6 mm; at present, the thickness of the ceramic large plate produced in the industry is mostly within 10mm, the ceramic large plate has poor machinability, and can be suitable for paving and pasting large-sized curtain walls or ground surfaces, but the ceramic large plate is difficult to utilize in the field of decorative surfaces. Therefore, further development of ceramic large plates is required.
In recent years, ceramic rock plates are released in the industry, the thickness of the ceramic rock plates can reach 12-20 mm, the ceramic rock plates are suitable for deep processing technology, and the ceramic rock plates can be applied to the fields of ground, curtain walls and home decoration. However, the existing rock plates are mostly 1200X 1600mm in size2、2400×1800mm2、2400×1200mm2And the specifications are equal, and the requirements of large-scale household decoration (a cooking bench, a cabinet, a bathroom cabinet and the like) cannot be met. On the other hand, the existing rock plate production system is immature, so that the number of drying cracked bricks and transportation cracked bricks is large, and the drying qualified rate is lower than 95%; similarly, the firing yield is low, about 90%. In addition, the existing ceramic rock plate is very easy to break in the processing process, and according to statistics, the processing breaking rate of the existing rock plate reaches more than 65%, so that the ceramic rock plate becomes a great problem which puzzles the industry.
Furthermore, in the transition from the development of ordinary ceramic tiles to ceramic slabs, the skilled man develops some experience of curing: for the formulation, in the formulation of ceramic large plates, the deformation of the plates with small thickness is considered to be serious in the firing process, so that calcium-magnesium mineral fluxes are rarely used. For another example, the distribution difficulty of a ceramic large plate with a thin thickness is low, so that the grading of common ceramic powder can meet the production requirement.
Disclosure of Invention
The invention aims to solve the technical problem that the large-size ceramic rock plate provided by the invention is excellent in deep processing performance, low in processing breakage rate and wide in application range.
The technical problem to be solved by the invention is to provide a preparation method of the large-size ceramic rock plate.
In order to solve the technical problem, the invention provides a large-size ceramic rock plate, and the surface area of the large-size ceramic rock plate is 3-12 m2The thickness is 12-30 mm;
comprises a body layer, a ground glaze layer, a pattern layer and a surface glaze layer; the thickness of the blank layer is 11.5-29.5 mm;
the green body layer is mainly prepared from the following raw materials in parts by weight:
15-20 parts of potassium feldspar, 8-15 parts of albite, 15-20 parts of calcined kaolin, 12-20 parts of black mud, 8-15 parts of white mud, 15-20 parts of pyrophyllite and 1-10 parts of a toughening agent; the sum of the parts by weight of the raw materials is 100 parts.
As an improvement of the above technical scheme, the toughening agent comprises a low-temperature toughening agent and a high-temperature toughening agent;
the low-temperature toughening agent can reduce the residual stress in the blank body below 1000 ℃ in the firing process;
the high-temperature toughening agent can reduce the residual stress in the blank body at the temperature of more than 1000 ℃ in the firing process;
as an improvement of the technical scheme, the low-temperature flexibilizer is cellulose ether, sodium polyacrylate, lignin, modified polysaccharide or tobermorite;
the high-temperature flexibilizer is selected from steatite, forsterite, mullite, magnesia, zirconia or alumina.
As an improvement of the technical scheme, the low-temperature flexibilizer is tobermorite; the high-temperature flexibilizer is forsterite.
As an improvement of the technical scheme, the usage ratio of the low-temperature toughening agent to the high-temperature toughening agent is 1: (2-5).
As an improvement of the technical scheme, the calcined kaolin has particles with the particle size of less than 1 mu m accounting for 70-90 wt%.
As an improvement of the technical scheme, the large-size ceramic rock plate is rectangular, the length of the diagonal line of the large-size ceramic rock plate is 2500-6000 mm, and the thickness of the large-size ceramic rock plate is 18-30 mm.
Correspondingly, the invention also discloses a preparation method of the large-size ceramic rock plate, which comprises the following steps:
(1) uniformly mixing various raw materials according to a formula, and performing ball milling to obtain slurry;
(2) spray-drying the slurry, and screening to obtain powder;
(3) pressing the powder to obtain a green body;
(4) applying a ground coat on the green body to form a ground coat layer;
(5) carrying out ink jet printing on the ground coat layer to form a pattern layer;
(6) applying a surface glaze on the pattern layer to form a surface glaze layer to obtain a blank body;
(7) and sintering the blank to obtain a large-size ceramic rock plate finished product.
As an improvement of the technical scheme, the grain composition of the powder material is as follows:
more than 20 meshes accounts for 1-4 wt%; 20-40 mesh accounts for 30-40 wt%; 25-35 wt% of 40-60 meshes, 10-17 wt% of 60-120 meshes, 5-10 wt% of 120-200 meshes and 1-5 wt% of below 200 meshes;
in the step (3), the powder is pressed and formed by adopting a die cavity dry pressing method, and the pressing pressure is not less than 400kg/cm2。
As an improvement of the technical scheme, the step (7) comprises the following steps:
(7.1) firing the blank; wherein the firing temperature is 1200-1300 ℃, and the firing period is 60-150 min;
and (7.2) polishing the sintered blank to obtain a large-size ceramic rock plate finished product.
The implementation of the invention has the following beneficial effects:
(1) the invention provides a large-size ceramic rock plate, the surface area of which is 3-12 m2The thickness of the floor is 12-30 mm, the floor can be well suitable for a later-stage deep processing technology, and the floor can be widely applied to the fields of floors, curtain walls and veneers, such as a washbasin, a tea set, a cooking bench and the like. Can greatly replace natural stone and artificial quartz stone plates; and has the advantages of high strength, high hardness, acid and alkali resistance, high temperature resistance and the like.
(2) The formula disclosed by the invention comprises 15-20 parts of potassium feldspar, 8-15 parts of albite, 15-20 parts of calcined kaolin, 12-20 parts of black mud, 8-15 parts of white mud, 15-20 parts of pyrophyllite and 1-10 parts of a toughening agent; the ceramic rock plate finished product produced by the formula has less stress aggregation, can well adapt to a later-stage deep processing process, and reduces the later-stage processing fracture rate to below 5%.
(3) The toughening agent is introduced into the formula of the invention, so that a weak interface structure can be established in the rock plate matrix, crack propagation energy is absorbed, and meanwhile, the toughening agent can also absorb external energy, so that residual stress is eliminated.
Specifically, the low-temperature toughening agent keeps a good whisker state in a blank body below 1000 ℃, and can fully absorb the stress of the front section of firing; the high-temperature flexibilizer can effectively promote the precipitation and growth of the mullite whisker at the temperature of more than 1000 ℃ to achieve the effect of reducing residual stress. The two are combined to reduce stress aggregation and improve the deep processing performance of the ceramic rock plate.
(4) The low-temperature toughening agent can also play a role in improving the green strength in the pressing and drying processes, and improve the yield. The green strength of the ceramic rock plate green body can reach 1.2-1.8 MPa.
(5) The grain composition of the powder material is more than 20 meshes and accounts for 1-4 wt%; 20-40 mesh accounts for 30-40 wt%; 25-35 wt% of 40-60 meshes, 10-17 wt% of 60-120 meshes, 5-10 wt% of 120-200 meshes and 1-5 wt% of below 200 meshes; the fluidity is high, and the material distribution is easy; and passes through not less than 400kg/cm2After the pressure is pressed, the internal uniformity of the green body is high, the density is uniform, and the later-stage stress accumulation is less.
Drawings
FIG. 1 is a schematic structural view of a large-format ceramic rock panel of the present invention;
FIG. 2 is a flow chart of a method for preparing a large-size ceramic rock plate according to the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
With reference to figure 1 of the drawings,the invention provides a large-size ceramic rock plate which comprises a blank layer 1, a ground glaze layer 2, a pattern layer 3 and a surface glaze layer 4; the surface area of the coating is 3 to 12m2The overall thickness is 12-30 mm; wherein, the thickness of the blank layer 1 is 11.5-29.5 mm, and the thickness of the blank layer 1 accounts for more than 95%. Preferably, the ceramic rock plate is rectangular, the length of a diagonal line of the ceramic rock plate is 2500-6000 mm, and the thickness of the ceramic rock plate is 18-30 mm. The ceramic rock plate can be well suitable for later-stage deep processing and is suitable for curtain walls and floors.
The blank layer 1 is mainly prepared from the following raw materials in parts by weight:
15-20 parts of potassium feldspar, 8-15 parts of albite, 15-20 parts of calcined kaolin, 12-20 parts of black mud, 8-15 parts of white mud, 15-20 parts of pyrophyllite and 1-10 parts of a toughening agent; the sum of the parts by weight of the raw materials is 100 parts.
The potassium feldspar and the albite are main fluxing agents, and can promote firing to obtain a ceramic rock plate finished product with the water absorption rate of less than 0.1%, the strength of the ceramic rock plate is improved, micro pores are reduced, and the stain resistance is improved. Wherein the using amount of the potassium feldspar is 15-20 parts, and the using amount of the albite is 8-15 parts; preferably, the using amount of the potassium feldspar is 17-20 parts, and the using amount of the albite is 10-13 parts.
Black mud and white mud are main plastic raw materials, and can improve the strength of green bodies and prevent the green bodies from cracking in the transportation and drying processes; meanwhile, mullite can be formed at a high temperature, so that the strength is improved, and the later deep processing performance is optimized. Wherein the using amount of the black mud is 12-20 parts, and the using amount of the white mud is 8-15 parts; preferably, the using amount of the black mud is 15-20 parts, and the using amount of the white mud is 8-12 parts.
The pyrophyllite can partially replace quartz in the traditional ceramic formula, so that a large amount of stress accumulation caused by quartz phase change is reduced; the pyrophyllite can also react at high temperature to generate a mullite phase, so that the strength of the ceramic rock plate is improved, and the later-stage processing fracture rate is reduced. Specifically, the usage amount of the pyrophyllite is 15-20 parts; when the amount of pyrophyllite is more than 20 parts, the green strength is lowered.
The Al content in the calcined kaolin can reach more than 40 wt%, and a large amount of acicular mullite whiskers can be formed in the subsequent sintering process, so that a weak interface structure is established in the ceramic rock plate matrix, and the residual stress is reduced. Preferably, in order to sufficiently exhibit the function of calcined kaolin, the particle size of the calcined kaolin needs to be controlled, and specifically, particles having a particle size of 1 μm or less account for 70 to 90 wt% of the calcined kaolin. The calcined kaolin is 15-20 parts.
The toughening agent comprises a low-temperature toughening agent and a high-temperature toughening agent; the method has the main functions of establishing a weak interface structure in a firing stage and a ceramic rock plate finished product, reducing residual stress, improving deep processing performance and reducing processing fracture rate; meanwhile, the method also plays a role in ensuring the smooth production.
Wherein, the low-temperature flexibilizer is a substance which plays a toughening role below 1000 ℃; specifically, it can be cellulose ether, sodium polyacrylate, lignin, modified polysaccharide or tobermorite; preferably tobermorite; the tobermorite is in a whisker shape, and can play a role in improving the strength of a green body in a forming stage; when the firing temperature is lower than 1000 ℃, the main reaction is phase change and does not melt, and the whisker structure is maintained; thereby better eliminating the thermal stress in the sintering process.
Wherein, the high-temperature flexibilizer is a substance which plays a toughening role at the temperature of more than 1000 ℃; specifically, it may be steatite, forsterite, mullite, magnesia, zirconia or alumina; among them, mullite, alumina and zirconia can achieve good toughening effect, but the firing temperature can be greatly increased, and the raw materials are high in price. Preferably, steatite or forsterite is selected; more preferably, forsterite is used. The blocky talc and the forsterite can promote the acicular of mullite crystals, reduce stress accumulation and reduce the processing fracture rate of the ceramic rock plate.
The proportion of the low-temperature toughening agent to the high-temperature toughening agent is 1: (2-5), preferably 1 (2.5-4).
In the conventional ceramic large plate (thickness less than 10mm) formula, the use amount of the calcium-containing magnesium raw material is reduced as much as possible, so that deformation defects such as raised grains and micro-warping in the firing process are prevented. In the invention, the ceramic rock plate has larger thickness, higher molding pressure (discussed later) and smaller sintering deformation, so that a small amount of calcium and magnesium raw materials can be introduced, the calcium and magnesium raw materials play a good toughening role, the deep processing performance of the ceramic rock plate is effectively improved, and the processing fracture rate is reduced.
Correspondingly, referring to fig. 2, the invention also discloses a preparation method of the large-size ceramic rock plate, which comprises the following steps:
s1: uniformly mixing various raw materials according to a formula, and performing ball milling to obtain slurry;
specifically, the formula is as follows: 15-20 parts of potassium feldspar, 8-15 parts of albite, 15-20 parts of calcined kaolin, 12-20 parts of black mud, 8-15 parts of white mud, 15-20 parts of pyrophyllite and 1-10 parts of a toughening agent; the sum of the parts by weight of the raw materials is 100 parts. The formula can be well suitable for the existing production line, reduces drying fracture, fracture in the transportation process and fracture in firing process, and improves the yield. Meanwhile, the formula can also ensure that the deformation is uniform in the drying and sintering processes, and the drying qualified rate and the sintering qualified rate are improved.
Preferably, the following components are adopted: 18 parts of potash feldspar, 11 parts of albite, 18 parts of calcined kaolin, 16 parts of black mud, 10 parts of white mud, 17 parts of pyrophyllite, 2.5 parts of tobermorite and 6.5 parts of forsterite.
Specifically, after ball milling, the fineness of the slurry should be controlled to be less than 0.5% of the screen residue of a 250-mesh sieve.
S2: spray-drying the slurry, and screening to obtain powder;
the ceramic rock plate has high thickness, large specification and high requirement on the uniformity of the material distribution. For this reason, the grain composition of the powder needs to be controlled. Specifically, the grain composition of the powder material in the invention is as follows: more than 20 meshes accounts for 1-4 wt%; 20-40 mesh accounts for 30-40 wt%; 25-35 wt% of 40-60 meshes, 10-17 wt% of 60-120 meshes, 5-10 wt% of 120-200 meshes and 1-5 wt% of below 200 meshes.
The traditional ceramic tile powder or ceramic large plate powder is fine, and the proportion of the powder is 30-50% of that of the powder with more than 60 meshes. The proportion of the invention can reach 50-80%; the fluidity is greatly improved, and the material distribution is convenient.
Correspondingly, in order to obtain the powder with the grain composition, the formula and the powder preparation process need to be controlled; specifically, in the aspect of the formula, the black mud and the white mud are controlled: the pyrophyllite is 1-2.1. In the aspect of a powder preparation process, a screening process is added after spray drying; for example, the powder obtained by spraying with a spray tower may be divided into two halves, one half of which is passed through a 60 mesh screen and the other half of which is not passed through a screen, and then the two halves are mixed to obtain the powder.
S3: pressing the powder to obtain a green body;
it should be noted that, at present, there are three methods for pressing large-sized ceramic plates, namely, continuous roll forming, belt dry pressing and die cavity dry pressing. The invention can select belt dry pressing and die cavity dry pressing; preferably, the die cavity is selected for dry pressing and molding, the internal stress is low, and a green blank obtained by pressing has good flatness and high dimensional precision.
Further, the pressing pressure in the pressing process is controlled to be not less than 400kg/cm2(ii) a Because the powder particles in the invention are large and the air content is high, the invention can exhaust by adopting larger pressure, improve the compaction degree of the green body, and improve the drying qualification rate and the firing qualification rate.
S4: applying a ground coat on the green body to form a ground coat layer;
specifically, the green body is dried before applying the ground coat.
S5: carrying out ink jet printing on the ground coat layer to form a pattern layer;
s6: applying a surface glaze on the pattern layer to form a surface glaze layer to obtain a blank body;
specifically, the ground glaze, ink and overglaze can adopt the prior art.
S7: firing the blank to obtain a large-size ceramic rock plate finished product;
specifically, S7 includes:
s71: firing the blank; wherein the firing temperature is 1200-1300 ℃, and the firing period is 60-150 min;
s72: polishing the sintered blank to obtain the finished product of the large-size ceramic rock plate.
The invention is illustrated below with specific examples:
example 1
This example provides a large format ceramic rock plate of dimensions 3600X 2000X 20mm3(ii) a Wherein the thickness of the green body layer is 19 mm;
the formula of the blank layer is as follows:
19 parts of potassium feldspar, 12 parts of albite, 16 parts of calcined kaolin, 18 parts of black mud, 10 parts of white mud, 18 parts of pyrophyllite, 1 part of low-temperature toughening agent and 6 parts of high-temperature toughening agent;
wherein, the particle size of 80 percent of particles in the calcined kaolin is less than 1 μm; the low-temperature toughening agent is methyl cellulose, and the high-temperature toughening agent is mullite whisker;
the preparation method of the ceramic rock plate comprises the following steps:
(1) uniformly mixing various raw materials according to a formula, and performing ball milling to obtain slurry;
wherein the 250-mesh screen residue of the slurry is 0.2 percent;
(2) spray drying the slurry, and screening to obtain powder;
specifically, the grain composition of the powder is as follows:
2 wt% of more than 20 meshes; 38 wt% of 20-40 meshes; 32 wt% of 40-60 meshes, 16 wt% of 60-120 meshes, 8 wt% of 120-200 meshes and 4 wt% of below 200 meshes.
(3) Pressing the powder to obtain a green body;
concretely, a HT36000 type press is adopted for pressing, and the forming pressure is 450kg/cm2。
(4) Applying a ground coat on the green body to form a ground coat layer;
(5) carrying out ink jet printing on the ground coat layer to form a pattern layer;
(6) applying a surface glaze on the pattern layer to form a surface glaze layer to obtain a blank body;
(7) firing the blank to obtain a large-size ceramic rock plate finished product;
wherein the sintering temperature is 1300 ℃, and the sintering period is 120 min.
Example 2
This example provides a large format ceramic rock plate of dimensions 3600X 1800X 25mm3(ii) a Wherein,the thickness of the green body layer is 24.5 mm;
the formula of the blank layer is as follows:
19 parts of potassium feldspar, 12 parts of albite, 16 parts of calcined kaolin, 18 parts of black mud, 10 parts of white mud, 18 parts of pyrophyllite, 1 part of low-temperature toughening agent and 6 parts of high-temperature toughening agent;
wherein 90% of the particles in the calcined kaolin have a particle size less than 1 μm; the low-temperature flexibilizer is tobermorite, and the high-temperature flexibilizer is steatite;
the preparation method of the ceramic rock plate comprises the following steps:
(1) uniformly mixing various raw materials according to a formula, and performing ball milling to obtain slurry;
wherein the 250-mesh screen residue of the slurry is 0.4 percent;
(2) spray drying the slurry, and screening to obtain powder;
specifically, the grain composition of the powder is as follows:
2 wt% of more than 20 meshes; the proportion of 20-40 meshes is 37 wt%; 33 wt% of 40-60 meshes, 16 wt% of 60-120 meshes, 9 wt% of 120-200 meshes and 3 wt% of below 200 meshes.
(3) Pressing the powder to obtain a green body;
concretely, a HT36000 type press is adopted for pressing, and the forming pressure is 480kg/cm2。
(4) Applying a ground coat on the green body to form a ground coat layer;
(5) carrying out ink jet printing on the ground coat layer to form a pattern layer;
(6) applying a surface glaze on the pattern layer to form a surface glaze layer to obtain a blank body;
(7) firing the blank to obtain a large-size ceramic rock plate finished product;
wherein the sintering temperature is 1280 ℃, and the sintering period is 100 min.
Example 3
This example provides a large-format ceramic rock plate of dimensions 3600X 1800X 20mm3(ii) a Wherein the thickness of the green body layer is 19 mm;
the formula of the blank layer is as follows:
18 parts of potassium feldspar, 11 parts of albite, 18 parts of calcined kaolin, 16 parts of black mud, 11 parts of white mud, 17 parts of pyrophyllite, 2.5 parts of a low-temperature toughening agent and 6.5 parts of a high-temperature toughening agent;
wherein 90% of the particles in the calcined kaolin have a particle size less than 1 μm; the low-temperature flexibilizer is tobermorite, and the high-temperature flexibilizer is forsterite;
the preparation method of the ceramic rock plate comprises the following steps:
(1) uniformly mixing various raw materials according to a formula, and performing ball milling to obtain slurry;
wherein the 250-mesh screen residue of the slurry is 0.4 percent;
(2) spray drying the slurry, and screening to obtain powder;
specifically, the grain composition of the powder is as follows:
2 wt% of more than 20 meshes; 20-40 meshes accounts for 36 wt%; 34 wt% of 40-60 meshes, 17 wt% of 60-120 meshes, 8 wt% of 120-200 meshes and 3 wt% of below 200 meshes.
(3) Pressing the powder to obtain a green body;
concretely, a HT36000 type press is adopted for pressing, and the forming pressure is 460kg/cm2。
(4) Applying a ground coat on the green body to form a ground coat layer;
(5) carrying out ink jet printing on the ground coat layer to form a pattern layer;
(6) applying a surface glaze on the pattern layer to form a surface glaze layer to obtain a blank body;
(7) firing the blank to obtain a large-size ceramic rock plate finished product;
wherein the firing temperature is 1260 ℃, and the firing period is 88 min.
Comparative example 1
The specification of a certain Jiangxi manufacturer is 2400 multiplied by 1200 multiplied by 15mm3The ceramic rock plate of (2) is used for measuring various properties.
Comparative example 2
The specification of a certain enterprise is 800 multiplied by 11mm3The performance of 50 common polished tiles was measured.
The performance of the materials in examples 1-3 and comparative examples 1-2 was measured, and the specific results are as follows (refer to GB/T3810-:
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Water absorption (%) | 0.09％ | 0.06％ | 0.05％ | 0.1％ | 0.2％ |
| Modulus of rupture (MPa) | 45.6 | 45.1 | 48.2 | 37.5 | 45.1 |
Example 4 measurement of drying and firing yield
1, determination of drying yield
Pressing 500 ceramic rock plate green bodies and drying.
After drying, if the green body is broken or the corners have small cracking lines, the green body is counted as unqualified, otherwise, the green body is counted as qualified;
after drying, 20 sheets of green compacts were taken and tested for edge bending and center bending (GB 3810.2-2016).
2, measurement of firing yield
And firing the dried qualified ceramic rock plate green body.
After the sintering, if the fracture or the edge has cracking lines or the obvious warping is visible by naked eyes, the product is determined to be unqualified; otherwise, the product is qualified;
after firing, 20 acceptable ceramic rock plates were selected and the degree of bending and the degree of central curvature were measured.
The results of the measurements are given in the following table (where the data for comparative example 2 is empirical):
example 5 measurement of work breakage rate
The processing fracture rate is divided into a cutting processing fracture rate and a carving processing fracture rate; the specific test method comprises the following steps:
1, cutting processing breakage rate: and respectively cutting the edge (within the side length of 1/3) and the center (central line) of the rock plate by an electric saw cutting machine.
If a crack or a broken line other than the cut line is generated after cutting, the crack is counted as a crack. If no cracks are visible to the naked eye after cutting, determining the modulus of rupture of the ceramic rock plate after cutting (GB/T3810.4-2016); if the modulus of rupture changes to less than 90% of the original modulus of rupture, then calculating as rupture; otherwise, it is counted as not broken.
2, engraving fracture rate: and engraving a central area of the ceramic rock plate by adopting a numerical control water jet scalpel to form an annular hole with the depth of 5-10 mm, the inner diameter of 495mm and the outer diameter of 500 mm.
If the ceramic rock plate is broken in the engraving process or after engraving, marking as breaking; when no cracks were visible to the naked eye in the ceramic rock plate after engraving, the modulus of rupture of the ceramic rock plate after engraving was measured, and when the modulus of rupture was changed to 80% or less of the original modulus of rupture, it was counted as a fracture. Otherwise, it is counted as not broken.
Selecting 50 pieces of the ceramic rock plates in examples 1-3 and 50 pieces of the ceramic rock plates in comparative example 1 (comparative example 1); 50 polished tiles of comparative example 2 (comparative example 2); the processing fracture rate test is carried out, and the test data are as follows:
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Rate of fracture by cutting | 0％ | 4％ | 0％ | 48％ | 0％ |
| Rate of rupture of the engraving | 4％ | 4％ | 4％ | 64％ | 8％ |
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The large-size ceramic rock plate is characterized in that the surface area of the large-size ceramic rock plate is 3-12 m2The thickness is 12-30 mm;
comprises a body layer, a ground glaze layer, a pattern layer and a surface glaze layer; the thickness of the blank layer is 11.5-29.5 mm;
the green body layer is prepared from the following raw materials in parts by weight:
15-20 parts of potassium feldspar, 8-15 parts of albite, 15-20 parts of calcined kaolin, 12-20 parts of black mud, 8-15 parts of white mud, 15-20 parts of pyrophyllite and 1-10 parts of a toughening agent; the sum of the parts by weight of the raw materials is 100 parts.
2. The large format ceramic rock panel of claim 1, wherein the toughening agent comprises a low temperature toughening agent and a high temperature toughening agent;
the low-temperature toughening agent can reduce the residual stress in the blank body below 1000 ℃ in the firing process;
the high-temperature toughening agent can reduce the residual stress in the blank body at the temperature of more than 1000 ℃ in the sintering process.
3. The large format ceramic rock panel of claim 2, wherein the low temperature toughening agent is selected from cellulose ethers, sodium polyacrylate, lignin, modified polysaccharides, or tobermorite;
the high-temperature flexibilizer is selected from steatite, forsterite, mullite, magnesia, zirconia or alumina.
4. The large format ceramic rock panel of claim 3, wherein the low temperature toughening agent is selected from tobermorite; the high-temperature flexibilizer is forsterite.
5. The large format ceramic rock panel of claim 2, wherein the low temperature toughening agent and the high temperature toughening agent are used in a ratio of 1: (2-5).
6. The large format ceramic slate of claim 1, wherein the calcined kaolin has particles of less than 1 μm in an amount of 70 to 90 wt%.
7. The large format ceramic rock panel of claim 1, wherein the large format ceramic rock panel is rectangular, having a diagonal length of 2500 to 6000mm and a thickness of 18 to 30 mm.
8. A method of making a large format ceramic rock panel according to any one of claims 1 to 7, comprising:
(1) uniformly mixing various raw materials according to a formula, and performing ball milling to obtain slurry;
(2) spray-drying the slurry, and screening to obtain powder;
(3) pressing the powder to obtain a green body;
(4) applying a ground coat on the green body to form a ground coat layer;
(5) carrying out ink jet printing on the ground coat layer to form a pattern layer;
(6) applying a surface glaze on the pattern layer to form a surface glaze layer to obtain a blank body;
(7) and sintering the blank to obtain a large-size ceramic rock plate finished product.
9. The method of making a large format ceramic rock panel of claim 8, wherein the powder has a grain size distribution of:
more than 20 meshes accounts for 1-4 wt%; 20-40 mesh accounts for 30-40 wt%; 25-35 wt% of 40-60 meshes, 10-17 wt% of 60-120 meshes, 5-10 wt% of 120-200 meshes and 1-5 wt% of below 200 meshes;
in the step (3), the powder is pressed and formed by adopting a die cavity dry pressing method, and the pressing pressure is not less than 400kg/cm2。
10. The method of making a large format ceramic rock panel of claim 8, wherein step (7) comprises:
(7.1) firing the blank; wherein the firing temperature is 1200-1300 ℃, and the firing period is 60-150 min;
and (7.2) polishing the sintered blank to obtain a large-size ceramic rock plate finished product.
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| US10227782B2 (en) * | 2015-02-06 | 2019-03-12 | Joseph F. DeLorenzo | Process for production of glazed, high density engineered surface products and products thereof |
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