CN113735443B - Ball dry particle and preparation method thereof - Google Patents
Ball dry particle and preparation method thereof Download PDFInfo
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- CN113735443B CN113735443B CN202111236196.0A CN202111236196A CN113735443B CN 113735443 B CN113735443 B CN 113735443B CN 202111236196 A CN202111236196 A CN 202111236196A CN 113735443 B CN113735443 B CN 113735443B
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Abstract
The invention relates to a ball dry particle and a preparation method thereof, wherein the preparation method of the ball dry particle comprises the following steps: mixing the raw materials for preparing the ball dry particles, and sintering to prepare a sintered product; quenching and crushing the burnt product to obtain a dry grain semi-finished product; and (3) performing beading treatment on the dry semi-finished product at the temperature of 850-950 ℃ to obtain the dry beaded. The preparation method of the ball dry particle can obtain the ball dry particle with round surface and smooth and fine hand feeling, and can effectively improve the pollution resistance of the corresponding ceramic product.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a ball dry particle and a preparation method thereof.
Background
Along with the iterative upgrading of the ceramic surface auxiliary material, ceramic products are more and more diversified under the promotion of the ceramic auxiliary material, and particularly along with the application of dry grains in recent years, the decoration performance and the physical application performance of the products are greatly improved. At present, the types of dry granules are also relatively large, and the dry granules are mainly classified into full-polished dry granules, candy dry granules, sub-gloss dry granules, metal dry granules, diamond dry granules and the like. Because the dry particle material is fired before being applied to ceramic products, organic matters and decomposable matters are fully decomposed under the firing of high temperature, after the dry particle material is applied to ceramic tiles, the dry particle material is not reduced when being fired with the ceramic tiles, so that the surfaces of the ceramic tiles with the dry particle material have the advantages of high density, low porosity, no clamping parts, stain resistance, wear resistance, corrosion resistance, high thermal stability and the like. However, the related ceramic products manufactured by the dry grains generally have the problems of rough hand feeling, easy dirt accumulation and the like, and are limited in application.
Disclosure of Invention
Based on this, it is necessary to provide a ball dry particle and a method for producing the same. The preparation method of the ball dry particle can obtain the ball dry particle with round surface and smooth and fine hand feeling, and can effectively improve the pollution resistance of the corresponding ceramic product.
A method for preparing a ball dry particle, comprising the steps of:
mixing the raw materials for preparing the ball dry particles, and sintering to prepare a sintered product;
crushing the baked product to obtain a dry grain semi-finished product;
and (3) performing beading treatment on the dry particle semi-finished product at the temperature of 850-950 ℃ to obtain the dry beaded particle.
In some embodiments, the starting materials for preparing the beadlet comprise: 30-45 parts of potassium feldspar, 5-15 parts of albite, 6-10 parts of kaolin, 10-20 parts of barium carbonate, 3-8 parts of wollastonite, 3-10 parts of zinc oxide, 4-10 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of alumina.
In some embodiments, the chemical composition of the potassium feldspar is K 2 The mass percentage of O is more than 9.0 percent;
among the chemical components of the albite, na 2 The mass percentage of O is above 8.5%;
of the chemical components of the kaolin, al 2 O 3 The mass percentage of (2) is more than 35 percent;
the chemical components of the calcite comprise 52-56% of CaO by mass percent;
the wollastonite comprises the following chemical components: siO (SiO) 2 48％～53％，Al 2 O 3 0.1％～1％，CaO 40％～45％；
Of the chemical components of the quartz, siO 2 The mass percentage of the catalyst is more than or equal to 99 percent.
In some embodiments, the mass ratio of the barium carbonate to the zinc oxide to the strontium carbonate is (10-18): 4-8): 6-8.
In some embodiments, the ball dry particle comprises the following main chemical components in percentage by mass: siO (SiO) 2 50％～55％、Al 2 O 3 16％～19％、CaO 3％～5％9 to 12 percent of BaO, 3.5 to 5 percent of SrO, 4.5 to 6.5 percent of KNaO and 3.6 to 4 percent of ZnO.
In some embodiments, the beading step is performed by passing the dry pellet semi-finished product in free-fall through a heating zone of a high temperature furnace, the heating zone having a temperature of 900 ℃ ± 5 ℃.
In some of these embodiments, the firing is performed by the following method;
at a first time t 1 Internally heated to 300 ℃ and then at a second time t 2 Heating to 1100 deg.C, and at a third time t 3 Heating to 1450 deg.C, and maintaining the temperature at 1450 deg.C for a fourth time t 4 Then cooling to 300-400 ℃; t is t 1 Is 8min to 12min, t 2 28 min-32 min, t 3 Is 18 min-22 min, t 4 Is 10 min-15 min.
In some embodiments, the raw materials for preparing the ball dry particles are mixed and stirred to obtain a mixture, and the mixture is conveyed into a frit furnace at a speed of 15-18 kg/min for sintering.
In some of these embodiments, the step of quenching and crushing the fired product to produce a dry pellet semi-finished product comprises the steps of:
introducing the baked product into water with the temperature below 50 ℃ for quenching treatment to obtain a quenched product;
crushing the crushed cold product to form a dry grain semi-finished product, and sieving the dry grain semi-finished product with a 250-300 mesh sieve.
A ball dry granule is prepared by the above preparation method.
After the corresponding dry semi-finished product of the ball dry particle is prepared by the preparation method of the ball dry particle, ball treatment is carried out at a specific temperature, so that the irregular prismatic structure on the surface of the dry particle is ablated, further, ball dry particles with round surface and better hand feeling can be obtained, the hand feeling of the corresponding ceramic product can be effectively improved after the ball dry particle is prepared into the corresponding ceramic product, the ceramic product with smooth and fine hand feeling can be obtained, the occurrence probability of dirt collection can be effectively reduced, and the pollution resistance of the corresponding ceramic product can be improved. And the ceramic product prepared from the ball dry particles also has better anti-skid property.
Drawings
FIG. 1 is an enlarged view of the bead dry pellet of example 3;
FIG. 2 is an enlarged view of the bead dry particle of comparative example 1;
FIG. 3 is an enlarged view of the bead dry particle of comparative example 2;
FIG. 4 is an enlarged view of the bead dry particles of comparative example 3.
Detailed Description
The present invention will be described more fully hereinafter in order to facilitate an understanding of the present invention, and preferred embodiments of the present invention are set forth. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
An embodiment of the invention provides a method for preparing ball dry particles, which comprises the following steps:
s101: and mixing the raw materials for preparing the ball dry particles, and sintering to obtain a sintered product.
In some embodiments, the starting materials for preparing the beadlet dry particle include: 30-45 parts of potassium feldspar, 5-15 parts of albite, 6-10 parts of kaolin, 10-20 parts of barium carbonate, 3-8 parts of wollastonite, 3-10 parts of zinc oxide, 4-10 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of alumina.
In some embodiments, the starting materials for preparing the beadlet dry particle include: 30-40 parts of potassium feldspar, 6-15 parts of albite, 7-9 parts of kaolin, 10-18 parts of barium carbonate, 3-8 parts of wollastonite, 3-8 parts of zinc oxide, 6-8 parts of strontium carbonate, 7-11 parts of calcite, 1.5-2.5 parts of quartz and 3-4 parts of alumina.
In some embodiments, the starting materials for preparing the beadlet dry particle include: the potassium feldspar comprises 35 parts of albite, 8 parts of kaolin, 15 parts of barium carbonate, 6 parts of wollastonite, 5 parts of zinc oxide, 6 parts of strontium carbonate, 11 parts of calcite, 2 parts of quartz and 4 parts of alumina.
In some embodiments, the starting materials for preparing the beadlet dry particle include: the potassium feldspar comprises 40 parts of albite, 6 parts of albite, 8 parts of kaolin, 18 parts of barium carbonate, 3 parts of wollastonite, 4 parts of zinc oxide, 8 parts of strontium carbonate, 7 parts of calcite, 2 parts of quartz and 4 parts of alumina.
In some embodiments, the starting materials for preparing the beadlet dry particle include: the potassium feldspar comprises 30 parts of albite, 15 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of alumina.
By adopting the raw material combination and controlling the proportion of each oxide in a co-phase system, the fine crystal of the divalent oxide is formed, so that the ball dry particles have silky hand feeling and transparent feeling, the hand feeling and quality of corresponding ceramic products can be improved, and the corresponding ceramic products have better performances of wear resistance, pollution resistance, skid resistance, acid and alkali resistance and the like. In addition, the formula combination can ensure that the dry grain material has a wider firing temperature range on the surface of the ceramic tile, and can show stable matte glossiness and silky and fine touch feeling under different firing temperatures of the ceramic tile and different surface glaze bases.
In some embodiments, K is the chemical composition of potassium feldspar 2 The mass percentage of O is more than 9.0 percent; further, K in the chemical composition of the potassium feldspar 2 The mass percentage of O is 9.0-10.5%; in some embodiments, na in the chemical composition of albite 2 The mass percentage of O is more than 7.5 percent; further, na in the chemical composition of albite 2 The mass percent of O is 8.5 percentThe above; further, na in the chemical composition of albite 2 The mass percentage of O is 7.5-9.0%; enough K 2 O and Na 2 The content of O can ensure the stability of alkali metal components in the formula and promote the dry particle formula to be fully melted at a preset temperature to form a sufficient liquid phase.
In some embodiments, the chemical composition of the kaolin is Al 2 O 3 The mass percentage of (2) is more than 35 percent; further, among the chemical components of kaolin, al 2 O 3 35% -40%; the kaolin is Al 2 O 3 Is mainly derived from Al 2 O 3 When the content is too small, the addition amount is increased, which results in SiO 2 The content of (2) is increased, so that the silicon-aluminum ratio is higher, and the glossiness of the prepared ball dry particle is higher.
In some embodiments, the mass ratio of the barium carbonate, the zinc oxide and the strontium carbonate is (10-18): 4-8): 6-8. In some embodiments, the purity of the barium carbonate is above 99%; in some embodiments, the purity of the zinc oxide is above 99.9%; in some embodiments, the strontium carbonate has a purity of 99.5% or more. If the content of barium carbonate, zinc oxide and strontium carbonate is too high, excessive divalent ions are easily caused to be transparent, excessive barium zinc strontium crystals can be generated, and the permeability of dry particles is low; if the content is too low, the content is due to Al 2 O 3 And SiO 2 Belongs to a substance with high-temperature viscosity, and if not enough flux is used for melting, dry particles are dry, rough and the like.
In some embodiments, the chemical components of wollastonite include: siO (SiO) 2 48％～53％，Al 2 O 3 0.1 to 1 percent and 40 to 45 percent of CaO; in some embodiments, the chemical composition of wollastonite is SiO 2 48% -53% of Al 2 O 3 0.1 to 1 percent, 40 to 45 percent of CaO, 1 to 4 percent of MgO and 2.5 to 4 percent of impurity. In some embodiments, the chemical composition of calcite comprises CaO in an amount greater than 50% by mass; further, the mass percentage of CaO is 52% -56%; further, the mass percentage of CaO is 52%54%. Wollastonite and calcite are main sources of CaO, if the content is low, the high-temperature viscosity of the molten state of dry particles is high, the molded product has coarse hand feeling, and if the content is high, anorthite is excessively precipitated to influence the transparent feeling of the dry particles, so that the color of the product is not transparent enough.
In some embodiments, the chemical composition of the quartz is SiO 2 The mass percentage content of (2) is more than or equal to 99 percent; further, siO 2 99.5% by mass and the balance of trace impurities. Quartz and Al 2 O 3 To supplement the network architecture, the tested content is suitable in this range.
In some embodiments, the bead dry particles comprise the main chemical components: siO (SiO) 2 50％～55％，Al 2 O 3 16 to 19 percent, 3 to 5 percent of CaO, 9 to 12 percent of BaO, 3.5 to 5 percent of SrO, 4.5 to 6.5 percent of KNaO and 3.6 to 4 percent of ZnO; further, caO is 4.3 to 4.7 percent, baO is 10.6 to 11 percent, srO is 4 to 4.4 percent, znO is 3.6 to 4 percent; further, caO is 4.5%, baO is 10.8%, srO is 4.2%, and ZnO is 3.8%.
In some embodiments, the particle fineness of each raw material used to prepare the beadlets is required to be below 300 mesh; further, the particle size is 200 mesh or less, so that liquefaction and reaction are sufficient during firing.
In some embodiments, the water content of each raw material used for preparing the ball dry particles is controlled below 1%, the lower the water content is, the easier and more uniform mixing is performed in the mixing stage, and the energy consumption in the sintering stage can be reduced.
In some embodiments, in step S101, firing is performed using the following method;
at a first time t 1 Heating to 295-305 deg.c and then for the second time t 2 Heating to 1050-1150 deg.c and at the third time t 3 Heating to 1300-1500 deg.c and maintaining the temperature at 1300-1500 deg.c for the fourth time t 4 Then cooling to 300-400 ℃; wherein t is 1 Is 8 min-60 min, t 2 28 min-60 min, t 3 Is 18min to 50min, t 4 10-30 min;
further, at a first time t 1 Internally heated to 300 ℃ and then at a second time t 2 Heating to 1100 deg.C, and at a third time t 3 Heating to 1450 deg.C, and maintaining the temperature at 1450 deg.C for a fourth time t 4 Then cooling to 300-400 ℃; t is t 1 Is 8min to 12min, t 2 28 min-32 min, t 3 Is 18 min-22 min, t 4 10-15 min; further, t 1 10min, t 2 30min, t 3 20min, t 4 For 10min.
In the sintering step, a gradient temperature control program is adopted, and in the first stage, the temperature is firstly increased to 295-305 ℃ in a specific time so as to ensure that structural water and adsorbed water in each material are fully discharged; in the second stage, heating to 1050-1150 deg.c for certain time to decompose organic matter in kaolin, and decomposing carbonate to discharge CO under the fluxing of monovalent oxide 2 The method comprises the steps of carrying out a first treatment on the surface of the In the third stage, 1300-1500 deg.c is reached and heat preservation is carried out at 1300-1500 deg.c 4 So that all materials start to melt, liquid phase starts to be generated under the action of the flux, and all oxides and SiO 2 Al and Al 2 O 3 The ball dry particle material can be suitable for different firing temperatures and different glazes, and can show stable matte glossiness and silky and fine touch feeling at different tile firing temperatures and on different overglaze bases.
In addition, the technical staff of the invention find that the matte effect and the hand feeling of the sintered ball dry particles are closely related to the sintering temperature program, the setting of the sintering temperature program needs to be matched with a formula to form a proper eutectic phase, the divalent oxide distinct crystal is utilized to generate a crystalline phase with low refractive index to reduce the glossiness, and the glossiness fluctuation can not occur due to the temperature fluctuation after the ceramic tile is used, so that the ceramic tile has a large sintering range.
It is understood that in the present invention, the firing step may be performed by using a manner that the mixture is not moved and the temperature is changed, or the mixture may be sequentially moved to a region having a corresponding temperature, which is not particularly limited herein, and should be understood to be within the scope of the present invention.
In some embodiments, in step S101, after mixing the raw materials for preparing the ball dry particles, stirring (preferably stirring for 20-40 min) to obtain a mixture, and conveying the mixture into a frit furnace at a speed of 15-18 kg/min for sintering; further, a screw column is used for transportation. When the conveying amount is smaller, the efficiency is lower, and when the conveying amount is larger, insufficient melting is easy to occur, and the phenomenon that raw materials are clamped can occur, so that the qualification rate of products is affected.
S102: quenching and crushing the burnt product to obtain a dry grain semi-finished product;
in some embodiments, in the quenching step of step S102, the fired product is introduced into water at a temperature below 50 ℃ to obtain a quenched product. The water with lower temperature is adopted, so that the quenching effect is better, and the subsequent crushing treatment is facilitated.
In some embodiments, in the crushing step of step S102, the crushed and cooled product is crushed to form a dry semi-finished product, and the dry semi-finished product is screened by a 250-300 mesh screen to facilitate the subsequent steps.
S103: and (3) carrying out beading treatment on the dry particle semi-finished product at the temperature of 850-950 ℃ and sieving to obtain the dry beaded particle.
The present inventors found in the study that: at present, dry particles are manufactured by firing and then crushing, sharp edges and corners are often formed on a microstructure, and further the problems of rough hand feeling, easy dirt storage, scale storage and the like are caused, so that the application is limited to a certain extent. In particular to a matte ceramic tile product, the matte effect can be achieved only by the high formula temperature of the glaze combined with the dry particles, so that the original form of the dry particles can be kept relatively complete, and if the dry particles are irregular in shape, the manufactured product is rough in touch sense and not fine and moist enough.
Based on the above, the present invention designs the preparation method of the ball dry particle, and the preparation method comprises the steps of firstly sintering, quenching and crushing, preparing a corresponding semi-finished product of the ball dry particle, and then performing ball treatment at 850-950 ℃ to ablate irregular prismatic structures on the surface of the ball dry particle, so that ball spherical structure dry particles with round surfaces can be obtained, and the treatment is performed at the temperature, so that the hand feeling and the texture of the ceramic product corresponding to the ball dry particle can be improved, and the product with smooth and fine hand feeling can be obtained. Further, it has been found that the temperature of the beading treatment has a large influence on the treatment effect, and when the temperature is low, the softening degree of the dried beads is insufficient, and the dried beads are not round enough, and when the temperature is high, the dried beads are easy to excessively fire and agglomerate, and the beading treatment temperature is preferably 850-950 ℃.
Further, the preferred beading treatment temperature is 860 ℃ to 930 ℃; further, the preferred beading treatment temperature is 880-920 ℃; further, it is preferable that the beading treatment temperature is 900 ℃ + -5 ℃ to obtain the best technical effect.
In some embodiments, the beading temperature is 870 ℃, 875 ℃, 880 ℃, 885 ℃, 890 ℃, 892 ℃, 894 ℃, 895 ℃, 896 ℃, 897 ℃, 898 ℃, 899 ℃, 900 ℃, 901 ℃, 902 ℃, 903 ℃, 904 ℃, 905 ℃, 906 ℃, 907 ℃, 908 ℃, 909 ℃, 915 ℃, 920 ℃, 925 ℃, 930 ℃, 935 ℃, or 940 ℃.
In the invention, the term "beading treatment" refers to heating a semi-finished product of dry particles in a high-temperature environment, eliminating edges and corners by using high temperature, and improving the roundness of the dry particles, and specifically, heating equipment commonly used in the art can be adopted, and only the corresponding temperature can be reached, and the method is not limited in particular, and is understood to be within the protection scope of the invention.
In some embodiments, in step S103, the dry pellet semi-finished product is passed through the heating zone of the high temperature furnace in a free-falling manner. The semi-finished product passes through the heating zone of the high-temperature melting furnace in a free falling manner, the self weight of the semi-finished product is utilized, the roundness of the ball dry particles can be effectively improved, and the deformation caused by heating treatment of the dry particle semi-finished product in a specific container is avoided.
In some embodiments, the high temperature furnace comprises an inlet, an outlet and a heating zone, wherein the inlet and the outlet are respectively arranged at two ends of the heating zone, the inlet is arranged on the upper side of the high temperature furnace, the outlet is arranged on the lower side of the high temperature furnace, so that semi-finished products can pass through the heating zone after entering the high temperature furnace through the inlet, move through the heating zone through free falling bodies and are discharged from the outlet.
In some embodiments, a cyclone fan is used to spray the semi-finished product of the ball dry particles into the high-temperature melting furnace, so that the dispersibility of the semi-finished product in the high-temperature melting furnace is improved, and the agglomeration phenomenon is avoided.
In some embodiments, in step S103, after the beading treatment, the method further includes a step of screening; further, the ball is processed by a 250-300 mesh screen mesh to obtain ball dry particles with the required particle size.
An embodiment of the invention provides a ball dry particle, which is prepared by the preparation method. Compared with the ball dry particle prepared by the traditional method, the ball dry particle has higher roundness and fine hand feeling, and effectively solves the problems of rough hand feeling, easy dirt collection, scale deposit and the like of the traditional product. The ball dry particles have matte luster, excellent wear resistance and anti-skid performance, and fine touch feeling and anti-skid function.
The present invention is illustrated by the following specific examples, which are given by way of illustration only and should not be construed as limiting the invention.
Example 1
The raw material formulation of this example: 35 parts of potassium feldspar, 8 parts of albite, 8 parts of kaolin, 15 parts of barium carbonate, 6 parts of wollastonite, 5 parts of zinc oxide, 6 parts of strontium carbonate, 11 parts of calcite, 2 parts of quartz and 4 parts of aluminum oxide;
the preparation method comprises the following steps:
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, and the dry grain semi-finished dry grain product which is smaller than the required mesh is sintered and melted.
(5) Spraying the fine powder dry particles passing through 250-300 meshes in the step (4) into a high-temperature melting furnace from an inlet of the high-temperature melting furnace through a cyclone fan, enabling the fine powder dry particles to pass through a heating zone in a free falling mode, performing beading treatment, collecting the fine powder dry particles from an outlet, and passing through a screen 250-300 meshes to obtain a finished product of the dry beads.
Example 2
The raw material formulation of this example: 40 parts of potassium feldspar, 6 parts of albite, 8 parts of kaolin, 18 parts of barium carbonate, 3 parts of wollastonite, 4 parts of zinc oxide, 8 parts of strontium carbonate, 7 parts of calcite, 2 parts of quartz and 4 parts of aluminum oxide.
The preparation method comprises the following steps:
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, and the dry grain semi-finished dry grain product which is smaller than the required mesh is sintered and melted.
(5) Spraying the fine powder dry particles passing through 250-300 meshes in the step (4) into a high-temperature melting furnace from an inlet of the high-temperature melting furnace through a cyclone fan, enabling the fine powder dry particles to pass through a heating zone in a free falling mode, performing beading treatment, collecting the fine powder dry particles from an outlet, and passing through a screen 250-300 meshes to obtain a finished product of the dry beads.
Example 3
The raw material formulation of this example: 30 parts of potassium feldspar, 15 parts of albite, 8 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of aluminum oxide.
The preparation method comprises the following steps:
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, and the dry grain semi-finished dry grain product which is smaller than the required mesh is sintered and melted.
(5) Spraying the fine powder dry particles passing through 250-300 meshes in the step (4) into a high-temperature melting furnace from an inlet of the high-temperature melting furnace through a cyclone fan, enabling the fine powder dry particles to pass through a heating zone in a free falling mode, performing beading treatment, collecting the fine powder dry particles from an outlet, and passing through a screen 250-300 meshes to obtain a finished product of the dry beads.
Example 4
Substantially the same as in example 3, except that the temperature of the heating zone of the beading process was 950 ℃, specifically:
the raw material formulation of this example: 30 parts of potassium feldspar, 15 parts of albite, 8 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of aluminum oxide.
The preparation method comprises the following steps:
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, and the dry grain semi-finished dry grain product which is smaller than the required mesh is sintered and melted.
(5) Spraying the fine powder dry particles passing through 250-300 meshes in the step (4) into a high-temperature melting furnace from an inlet of the high-temperature melting furnace through a cyclone fan, enabling the fine powder dry particles to pass through a heating zone in a free falling mode, performing beading treatment, collecting the fine powder dry particles from an outlet, and passing through a screen 250-300 meshes to obtain a finished product of the dry beads.
Example 5
Substantially the same as in example 3, except that the temperature of the heating zone of the beading process was 850 ℃, specifically:
the raw material formulation of this example: 30 parts of potassium feldspar, 15 parts of albite, 8 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of aluminum oxide. The preparation method comprises the following steps:
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, and the dry grain semi-finished dry grain product which is smaller than the required mesh is sintered and melted.
(5) Spraying the fine powder dry particles passing through 250-300 meshes in the step (4) into a high-temperature melting furnace from an inlet of the high-temperature melting furnace through a cyclone fan, enabling the fine powder dry particles to pass through a heating zone in a free falling mode, performing beading treatment, collecting the fine powder dry particles from an outlet, and passing through a screen 250-300 meshes to obtain a finished product of the dry beads.
Example 6
Substantially the same as in example 3, except that the following formulation was adopted in this example: 28 parts of potassium feldspar, 20 parts of albite, 8 parts of kaolin, 5 parts of barium carbonate, 10 parts of zinc oxide, 11 parts of strontium carbonate, 6 parts of calcite and 2 parts of quartz.
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, and the dry grain semi-finished dry grain product which is smaller than the required mesh is sintered and melted.
(5) Spraying the fine powder dry particles passing through 250-300 meshes in the step (4) into a high-temperature melting furnace from an inlet of the high-temperature melting furnace through a cyclone fan, enabling the fine powder dry particles to pass through a heating zone in a free falling mode, performing beading treatment, collecting the fine powder dry particles from an outlet, and passing through a screen 250-300 meshes to obtain a finished product of the dry beads.
Comparative example 1
Substantially the same as in example 3, except that the beading treatment was not performed, specifically:
the raw material formula of the comparative example: 30 parts of potassium feldspar, 15 parts of albite, 8 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of aluminum oxide.
The preparation method comprises the following steps:
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, the raw material which is smaller than the required mesh is sintered and melted, and the dry grain product is obtained after passing through the screen of 250-300 meshes.
Comparative example 2
The raw material formula of the comparative example: 30 parts of potassium feldspar, 15 parts of albite, 8 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of aluminum oxide.
The preparation method comprises the following steps:
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, and the dry grain semi-finished dry grain product which is smaller than the required mesh is sintered and melted.
(5) Spraying the fine powder dry particles passing through 250-300 meshes in the step (4) into a high-temperature melting furnace from an inlet of the high-temperature melting furnace through a cyclone fan, enabling the fine powder dry particles to pass through a heating zone in a free falling mode, performing beading treatment, collecting the dry particles from an outlet, and sieving the dry particles with 250-300 meshes to obtain a dry particle finished product.
Comparative example 3
The raw material formula of the comparative example: 30 parts of potassium feldspar, 15 parts of albite, 8 parts of kaolin, 10 parts of barium carbonate, 8 parts of wollastonite, 8 parts of zinc oxide, 8 parts of strontium carbonate, 8 parts of calcite, 2 parts of quartz and 3 parts of aluminum oxide.
The preparation method comprises the following steps:
(1) The raw materials are mixed, the mixed materials are accurately conveyed into a mixer by a belt scale for mixing, the capacity of the mixer is 2 tons, and the mixing time is 30 minutes.
(2) The mixed materials with the weight of 15-18 kg/min are gradually conveyed into a frit furnace by adopting a spiral column for sintering, and the sintering is carried out according to the following method:
heating to 300 ℃ for 10min, then heating to 1100 ℃ for 30min, then heating to 1450 ℃ for 20min, then preserving heat for 10min within the range of 1450 ℃, and then cooling to 300-400 ℃;
(3) And (3) flowing the high-temperature liquid burned material after the sintering treatment into a cold water tank below the frit furnace from a gate to perform quenching, controlling the water temperature of the cold water tank to be below 50 ℃, and obtaining a glass-state dry grain semi-finished product after quenching.
(4) The moisture of the semi-finished dry grain product is controlled below 1%, the semi-finished dry grain product is conveyed into a pair roller machine for crushing, the crushed fine powder passes through a 250-300 mesh screen, the dry grain fine powder in the range of 250-300 meshes is taken, the rest of the dry grain fine powder which is larger than the required mesh is crushed again until the qualified mesh is reached, and the dry grain semi-finished dry grain product which is smaller than the required mesh is sintered and melted.
(5) Spraying the fine powder dry particles passing through the 250-300 meshes in the step (4) into a high-temperature melting furnace from an inlet of the high-temperature melting furnace through a cyclone fan, enabling the fine powder dry particles to pass through a heating zone in a free falling mode, performing beading treatment, collecting the fine powder dry particles from an outlet, and sieving the fine powder dry particles with a 250-300 meshes sieve to obtain a dry particle finished product.
Performance testing
(1) Surface topography detection
Dry pellets of example 3, comparative example 1-comparative example 3 were examined using an MG10085-1a1500X microscope, wherein an enlarged view of example 3 is shown in fig. 1, an enlarged view of comparative example 1 is shown in fig. 2, an enlarged view of comparative example 2 is shown in fig. 3, and an enlarged view of comparative example 3 is shown in fig. 4.
As can be seen from FIG. 1, the beads of example 3 were substantially round, round in surface, uniform in particle size, and excellent in transparency. As can be seen from fig. 2, the surface of the dry pellet which has not been beaded has a significant angle. The method provided by the invention can effectively improve the roundness of the ball dry particles.
As can be seen from fig. 3 and fig. 4, the effect of the beading treatment at different temperatures is greatly different, and when the temperature is too low, only part of the dry particles are in the shape of beads, possibly because the softening degree of the dry particles is insufficient, the edges of the dry particles of the manufactured beads are not round enough; when the temperature is higher, the dry particles are agglomerated into sheets, and the round bead dry particles cannot be formed, and the dry particles are likely to be agglomerated due to easy excessive fire. The invention shows that the ball treatment temperature range can effectively improve the roundness of the ball dry particles, and further can effectively avoid a series of problems caused by the edges and corners of the dry particles.
(2) Matte effect and hand feel detection
The glossiness detection method is to test by using a glossiness meter, the test adopts a WGG60-E4 photometer, after the machine is started, a standard plate is used for adjusting a 0 glossiness point and a highlight 97.0 degree point, and then the glossiness meter is placed on a measured sample to obtain glossiness data. According to the national standard, refer to ISO-2767, GB 8941.2. The results of the above examples and comparative examples are shown in Table 1, with 75 degrees or more defined as specular, 30 to 75 degrees defined as plain, 5 to 30 degrees defined as matte, and 5 degrees or less defined as matt;
hand feel evaluation criteria: the method is determined by touch hand feeling judgment, and is superior to 10 points, preferably 7-9 points, generally 4-6 points and inferior to 1-3 points; the higher the score, the better the hand, preferably greater than 7 points, and the test results of the above examples and comparative examples are shown in Table 2.
Table 1:
TABLE 2
As can be seen from Table 1, the round bead dry particles of the present invention are shown to have a matte gloss and to exhibit stable matte gloss at firing temperatures of different specifications, so that the round bead dry particles are applicable not only to small-specification ceramic products but also to matte dry particle materials of large-specification large-plate rock plates.
As can be seen from Table 2, the ball dry particles of the present invention exhibit superior hand feeling at firing temperatures of different specifications, and the ball dry particles can improve the problem of rough hand feeling of the related ceramic products. In addition, example 3 and example 6 were compared, except that the formulation of the components was different, wollastonite was absent in example 6, and the contents of some components were different, and it can be seen from Table 2 that the hand feeling of example 3 was significantly better than that of example 6. Illustrating the effect of preferably wollastonite in improving hand, the following materials are preferably used: 30-45 parts of potassium feldspar, 5-15 parts of albite, 6-10 parts of kaolin, 10-20 parts of barium carbonate, 3-8 parts of wollastonite, 3-10 parts of zinc oxide, 4-10 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of alumina.
(3) Stain resistance and anti-skid properties
The dry pellets of the above examples and comparative examples were examined to prepare ceramic tiles, specifically: preparing green bricks, drying, applying overglaze, spraying and printing patterns, spraying glaze slurry containing dry grains of examples and comparative examples on the green bricks, firing at 1200 ℃, polishing to obtain ceramic products, and detecting the stain resistance and the skid resistance of the ceramic products, wherein the specific conditions are shown in table 3:
TABLE 3 Table 3
As can be seen from Table 3, the ceramic products prepared from the ball dry particles of the present invention have excellent contamination resistance and anti-slip level. In addition, it can be seen from comparative example 3 and comparative examples 1 to 3 that the beading treatment at a specific temperature can effectively improve the stain resistance and the slip resistance of the corresponding ceramic articles. As can be seen from comparative examples 3 and 6, the raw material formulation of the ball dry particles has a certain influence on stain resistance and anti-slip properties, and the following raw materials are preferably used: 30-45 parts of potassium feldspar, 5-15 parts of albite, 6-10 parts of kaolin, 10-20 parts of barium carbonate, 3-8 parts of wollastonite, 3-10 parts of zinc oxide, 4-10 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of alumina.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. A method for preparing a ball dry particle, comprising the steps of:
(1) Mixing the raw materials for preparing the ball dry particles, and sintering to prepare a sintered product;
(2) Quenching and crushing the baked product to obtain a dry grain semi-finished product;
(3) Performing beading treatment on the dry semi-finished product at the temperature of 850-950 ℃ to obtain the dry beaded;
the firing is carried out by adopting the following method:
at a first time t 1 Heating to 295-305 deg.c and then for the second time t 2 Heating to 1050-1150 deg.c and at the third time t 3 Heating to 1300-1500 deg.C, and 1300-1500 deg.CHeat preservation for the fourth time t 4 Then cooling to 300-400 ℃; wherein t is 1 Is 8 min-60 min, t 2 28 min-60 min, t 3 Is 18min to 50min, t 4 10-30 min;
the raw materials for preparing the ball dry particles comprise: 30-45 parts of potassium feldspar, 5-15 parts of albite, 6-10 parts of kaolin, 10-20 parts of barium carbonate, 3-8 parts of wollastonite, 3-10 parts of zinc oxide, 4-10 parts of strontium carbonate, 7-13 parts of calcite, 1-4 parts of quartz and 1-5 parts of alumina.
2. The method according to claim 1, wherein the raw materials for preparing the ball dry particles comprise: 30-40 parts of potassium feldspar, 6-15 parts of albite, 7-9 parts of kaolin, 10-18 parts of barium carbonate, 3-8 parts of wollastonite, 3-8 parts of zinc oxide, 6-8 parts of strontium carbonate, 7-11 parts of calcite, 1.5-2.5 parts of quartz and 3-4 parts of alumina.
3. The method according to claim 2, wherein K is a chemical component of the potassium feldspar 2 The mass percentage of O is more than 9.0 percent;
among the chemical components of the albite, na 2 The mass percentage of O is above 8.5%;
of the chemical components of the kaolin, al 2 O 3 The mass percentage of (2) is more than 35 percent;
the chemical components of the calcite comprise 52-56% of CaO by mass percent;
the wollastonite comprises the following chemical components: siO (SiO) 2 48％～53％，Al 2 O 3 0.1％～1％，CaO 40％～45％；
Of the chemical components of the quartz, siO 2 The mass percentage of the catalyst is more than or equal to 99 percent.
4. The preparation method according to claim 2, wherein the mass ratio of the barium carbonate to the zinc oxide to the strontium carbonate is (10-18): 4-8): 6-8.
5. The preparation method according to claim 2, wherein the ball dry particles comprise the following main chemical components in percentage by mass: siO (SiO) 2 50％～55％、Al 2 O 3 16 to 19 percent, 3 to 5 percent of CaO, 9 to 12 percent of BaO, 3.5 to 5 percent of SrO, 4.5 to 6.5 percent of KNaO and 3.6 to 4 percent of ZnO.
6. The method according to claim 2, wherein in the step of beading, the dry pellet semi-finished product is passed through a heating zone of a high temperature melting furnace in a free falling manner, the temperature of the heating zone being 900 ℃ ± 5 ℃.
7. The method according to any one of claims 1 to 6, wherein the firing is performed by the following method;
at a first time t 1 Internally heated to 300 ℃ and then at a second time t 2 Heating to 1100 deg.C, and at a third time t 3 Heating to 1450 deg.C, and maintaining the temperature at 1450 deg.C for a fourth time t 4 Then cooling to 300-400 ℃; t is t 1 Is 8min to 12min, t 2 28 min-32 min, t 3 Is 18 min-22 min, t 4 Is 10 min-15 min.
8. The method according to any one of claims 1 to 6, wherein the raw materials for preparing the bead dry particles are mixed and stirred to obtain a mixture, and the mixture is fed into a frit furnace at a speed of 15 to 18kg/min for the firing.
9. The method according to any one of claims 1 to 6, wherein the step of quenching and crushing the fired product to obtain a dry pellet semi-finished product comprises the steps of:
introducing the baked product into water with the temperature below 50 ℃ and quenching to obtain a quenched product;
crushing the crushed cold product to form a dry grain semi-finished product, and sieving the dry grain semi-finished product with a 250-300 mesh sieve.
10. A dry bead prepared by the method of any one of claims 1-9.
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Address after: 528061 1st floor, No.18 taobo Avenue, Huaxia Ceramics Expo City, Nanzhuang Town, Chancheng District, Foshan City, Guangdong Province Applicant after: New Pearl Group Co.,Ltd. Applicant after: FOSHAN SANSHUI NEW PEARL CONSTRUCTION CERAMICS INDUSTRIAL Co.,Ltd. Applicant after: New Pearl (Guangdong) New Materials Co.,Ltd. Applicant after: Jiangxi Xinmingzhu Building Materials Co.,Ltd. Applicant after: Hubei new Ming Zhu Green Building Materials Technology Co.,Ltd. Address before: 528061 1st floor, No.18 taobo Avenue, Huaxia Ceramics Expo City, Nanzhuang Town, Chancheng District, Foshan City, Guangdong Province Applicant before: New Pearl Group Co.,Ltd. Applicant before: FOSHAN SANSHUI NEW PEARL CONSTRUCTION CERAMICS INDUSTRIAL Co.,Ltd. Applicant before: GUANGDONG SUMMIT CERAMICS Co.,Ltd. Applicant before: Jiangxi Xinmingzhu Building Materials Co.,Ltd. Applicant before: Hubei new Ming Zhu Green Building Materials Technology Co.,Ltd. |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |