CN106830684B - Preparation method of reflective heat-insulation ceramic glazed tile - Google Patents
Preparation method of reflective heat-insulation ceramic glazed tile Download PDFInfo
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- CN106830684B CN106830684B CN201710144203.1A CN201710144203A CN106830684B CN 106830684 B CN106830684 B CN 106830684B CN 201710144203 A CN201710144203 A CN 201710144203A CN 106830684 B CN106830684 B CN 106830684B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
Abstract
The invention discloses a preparation method of a reflective heat-insulation ceramic glazed tile. The preparation method comprises the steps of mixing raw materials of a frit, and melting the raw materials in a frit furnace to obtain the frit, wherein the melting temperature is 1400-1600 ℃ until the raw materials are completely melted; mixing and grinding the prepared frit and the raw material to prepare glaze slurry, wherein the frit accounts for 10-100% of the total mass of the raw material, and the content of titanium dioxide in the glaze is not lower than 8% of the total mass; applying the prepared glaze slip on a blank body; and drying the blank body applied with the glaze slip, and sintering at the temperature of 1100-1250 ℃ to obtain the reflective heat-insulating ceramic glazed tile. According to the invention, the frit is mixed with a certain amount of raw materials, so that the glaze layer taking titanium sphene crystals as a main crystal phase is obtained on the surface of the ceramic tile, the glaze layer has a high reflection effect on sunlight, the absorption of the ceramic tile on solar heat radiation can be effectively reduced, the building energy consumption in areas hot in summer and warm in winter is obviously reduced, the energy-saving and environment-friendly effects are obvious, and the preparation cost is low.
Description
Technical Field
The invention relates to the field of architectural ceramics, in particular to a preparation method of a reflective heat-insulating ceramic glazed tile.
Background
The building energy consumption is parallel to the traffic energy consumption and the industrial energy consumption, and is one of three main energy consumption modes in China. Along with the social and economic development and the improvement of the requirement of people on the comfort level of the indoor environment, the building energy consumption is in a rapid rising trend and continuously rises in the proportion of energy consumption of the whole society.
Various methods are used for reducing or preventing building temperature rise caused by strong solar radiation, reducing refrigeration energy consumption and reducing environmental pollution, and the important research targets of building material energy conservation are achieved. The building outer wall is the most important part of building energy consumption, and the heat insulation performance directly influences the heat exchange of the building, so the research on the energy-saving technology becomes the important research on the energy-saving of the building structure. Meanwhile, considering that the service life of buildings is mostly more than dozens of years and even more than one hundred years, the use of the cooling energy-saving building exterior wall material with high durability and no consumption of extra energy has important significance for energy conservation and emission reduction, atmospheric environment and ecological environment protection, and improvement of the quality of life and the health level of people.
The reflective heat-insulating material can actively reflect solar heat radiation, reduce the indoor temperature, radically reduce the use of the air conditioner and obviously reduce the energy consumption of the air conditioner.
At present, the reflective and heat-insulating materials for the outer wall of buildings except for Low-E glass curtain walls only have the choice of reflective coatings, most buildings such as houses and the like generally do not use glass curtain walls, the service life of the coatings is short, and the recoating brings environmental pollution, so that the development and production of the reflective and heat-insulating materials which have the same service life as the buildings, high reflectivity and attractive appearance become one of the research hotspots of building energy-saving materials in recent years. According to the report of Solar Energy, in Spain and Italy, the Energy can be saved by 2.5-3.5 kW h/m each year by adopting the Solar heat reflecting material which is 17% higher than that of the traditional material2. The reflectivity of the common light-colored ceramic tile to sunlight is about 60%, if the solar heat reflection heat insulation ceramic tile which is 20-30% higher than the common ceramic tile is adopted, the very obvious energy-saving effect is brought, and the application of the ceramic tile has important significance for building energy saving in south China, especially in south China which is warm in winter and hot in summer.
Chinese patent application 2015104154431 (7/15/2015) discloses an opacifier, a preparation method thereof and a ceramic glaze containing the opacifier. The opacifier is mainly prepared from the following components in percentage by weight: 5-40% of calcium carbonate, 5-40% of titanium dioxide, 0.05-2.5% of dispersing auxiliary agent and the balance of water. The ceramic glaze containing the opacifier is prepared from the following raw materials in parts by weight: 6-10 parts of opacifier, 30-35 parts of quartz, 25-30 parts of potassium feldspar, 2-4 parts of aluminum oxide, 10-12 parts of calcite, 4-6 parts of dolomite, 2-3 parts of zinc oxide, 4-5 parts of kaolin and 1-2.5 parts of fusion cake; the technology aims to solve the problem of yellowing of ceramic glaze surfaces caused by directly adding titanium dioxide particles. The technology considers that the opacifier forms composite particles which take calcium carbonate as a core and crystalline titanium dioxide as a coating, and the calcium carbonate and the titanium dioxide form a stable core-shell structure body through chemical condensation reaction of a large number of hydroxyl groups on the surface of the particles; the chemical bonding of the calcium and titanium components on the surface is realized, so that the titanium dioxide is an important reason for the combination of the titanium dioxide and calcium compounds and other components, the stable titanium sphene crystal form is formed by the titanium dioxide directly and oxides of calcium and silicon under the high-temperature condition, the direct transformation to the rutile phase is not ensured, and the problem of yellowing of a ceramic glaze surface caused by the direct addition of titanium dioxide particles (as an opacifier) is effectively avoided. However, the preparation method of the opacifier comprises the following steps: 1) adding calcium carbonate into partial water, uniformly dispersing and grinding to obtain a calcium carbonate suspension; 2) sequentially adding titanium dioxide and a dispersing aid into the rest part of water, and grinding to obtain a titanium dioxide suspension; 3) and uniformly mixing the calcium carbonate suspension and the titanium dioxide suspension, grinding to obtain composite particle suspension slurry, drying the obtained slurry, and scattering to obtain the opacifier. The calcium carbonate and the titanium dioxide are ground respectively by the opacifier, the mixture is further ground after being mixed, the mixture is further broken up after being dried, the time consumption of the preparation process of the opacifier is long, the power consumption is high, and the industrialization is not facilitated; the opacifier is required to be further prepared into glaze with quartz, potassium feldspar, aluminum oxide, calcite and the like, the glaze is required to be subjected to ball milling for 18-22 hours, and the fineness of the glaze slip is controlled to be about 200 meshes; the glaze slurry is sieved twice, iron is removed for 2 times, glaze is directly applied to a blank by adopting a glaze spraying or glaze dipping method, the thickness of a glaze layer before sintering is controlled to be 0.6-0.8 mm, the glaze is sintered in an oxidizing atmosphere, the optimal sintering temperature of the glaze is 1000-1300 ℃, although titanium sphene can be obtained by the technology, emulsion is prepared firstly, the ball milling workload in the whole process is very large, the steps are multiple, the consumption is large, and particularly, the technology only realizes that rutile which can be solved by stabilizing the formation of the titanium sphene can solve the problem of yellowing of a ceramic glaze surface, so that the content of titanium dioxide in the glaze is lower than 4%, and the technology cannot be used for preparing energy-saving reflective heat-insulating ceramic.
Disclosure of Invention
The invention aims to overcome the problems in the prior art, and provides the preparation method of the reflective heat-insulating ceramic which is simple in preparation method, low in energy consumption and convenient to realize industrialization and takes titanium sphene as a main crystal phase, wherein the solar reflectance ratio of the prepared light-colored reflective heat-insulating ceramic is more than 0.80; compared with the method of completely introducing the titanium element in the form of raw materials, the method can obtain the ceramic tile surface glaze layer with the titanium sphene crystal as the main crystal phase within a firing period of 20-90 min by partially or completely introducing the titanium element in the form of frit.
In general, the pure titanium sphene glaze is mainly white, and if a small amount of impurities is contained, the color tone of the glaze may be yellowish or reddish. The solar reflectance of 0.8 is the national standard for reference reflective coatings, but this is only for white coatings, and the industry standard for colored coatings is otherwise specified. The solar reflectance of a colored material is lower than that of a white material due to a large amount of absorption of visible light, and the reflectance is lower for a darker color.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) mixing the raw materials of the frit, and melting the raw materials in a frit furnace to prepare the frit, wherein the melting temperature is 1400-1600 ℃ until the raw materials are completely melted; the main chemical composition of the frit is as follows (it is common practice in the art to express the chemical composition in terms of oxides):
2) mixing and grinding the frit prepared in the step 1) and the raw material to prepare glaze slurry, wherein the frit accounts for 10-100% of the total mass of the raw material, and the content of titanium dioxide in the glaze is not lower than 8% of the total mass;
3) applying the glaze slip prepared in the step 2) on a blank body;
4) and (3) drying the blank body applied with the glaze slip in the step 3), and then sintering at the temperature of 1100-1250 ℃ for 20-90 min to obtain the reflective heat-insulating ceramic glazed tile.
To further achieve the object of the present invention, preferably, the raw meal comprises one or more of clay, kaolin, quartz, alumina, feldspar, calcite, talc, dolomite, wollastonite, titanium dioxide, barium carbonate, strontium carbonate, zinc oxide, bone ash and spodumene.
Preferably, the glaze slip of step 3) is applied to the body by means of a glaze sprayer.
Preferably, the firing is performed in a roller kiln.
Preferably, the frit has a main chemical composition as follows, in mass percent:
preferably, the thickness of the fired solar heat reflecting layer on the surface of the reflective heat-insulating ceramic glazed tile is 0.1-3.0 mm.
On the basis of the formula of the invention, by researching the relation (table 1) between the content of titanium dioxide in the glaze and the reflection effect of the glaze layer on solar heat, when the content of titanium dioxide is more than 8%, the solar light reflection ratio (the ratio of reflection in the wavelength range of 250-2500 nm to the incident solar radiation flux of the same wave band) of the glaze layer correspondingly obtained reaches more than 0.8, and the performance requirement of the reflective coating in national standard 'architectural reflective heat-insulating coating' on white coating is met. The results in table 1 also show that, within a certain range, the higher the content of titanium dioxide in the glaze, the higher the solar reflectance of the reflective insulating ceramic tile produced. The invention also discovers that the adding amount of the titanium dioxide is related to the firing system of the glaze, excessive titanium dioxide has important influence on the melting performance of the glaze, and the invention defines the reasonable using amount range of the titanium dioxide in the raw materials.
Table 1: relation between titanium dioxide content and sunlight reflectance
The preparation of the frit can realize the precipitation of a large amount of titanium sphene in a short sintering time, and meet the requirement of industrialization; compared with the method of completely introducing the titanium element in the form of raw materials, the method can obtain the ceramic tile surface glaze layer with the titanium sphene crystal as the main crystal phase within a firing period of 20-90 min by partially or completely introducing the titanium element in the form of frit.
Compared with the prior art, the invention has the following advantages:
1) the Chinese patent application 2015104154431 requires that an opacifier is prepared firstly, the opacifier needs to be mixed with calcium carbonate and titanium dioxide, then the mixture needs to be ground continuously, and the opacifier needs to be broken up after drying, so that the preparation process of the opacifier is long in time consumption and large in power consumption, and is not beneficial to realizing industrialization; the opacifier is required to be further prepared into glaze with quartz, potassium feldspar, aluminum oxide, calcite and the like, the glaze is required to be subjected to ball milling for 18-22 hours, and the fineness of the glaze slip is controlled to be about 200 meshes; sieving the glaze slip twice, removing iron for 2 times, adopting a glaze spraying or glaze dipping method, directly glazing the blank, and firing in an oxidizing atmosphere; although titanium sphene can be obtained by the technology, emulsion is prepared first, so that the whole process has the disadvantages of very large ball milling workload, multiple steps and high consumption. The method only needs to mix and grind the prepared frit and the raw material to prepare the glaze slurry, and the grinding workload is small; in addition, the titanium element is introduced partially or completely in the form of the frit, so that the surface glaze layer of the ceramic tile taking titanium sphene crystals as a main crystal phase can be obtained in a firing period of 20-90 min, the requirement of rapid firing in industrial production is met, and the defects of complicated preparation process and high cost of the Chinese patent application 2015104154431 are greatly overcome. This patent does not recognize that a glaze rich in titanium sphene has a high reflection of sunlight and that it has a low titanium sphene content (less than 4% titanium dioxide in the glaze).
2) The method comprises the steps of melting partial titanium, calcium and other components into a frit, and mixing the frit with a certain amount of raw materials to obtain a glaze layer taking titanium sphene crystals as main crystals on the surface of the ceramic tile; because the glaze layer contains titanium sphene crystal phase with high reflectivity to full-wave band sunlight, the reflection effect of the ceramic tile to solar heat radiation is effectively improved, the temperature of the outer wall of a building can be reduced, the indoor and outdoor temperature difference is reduced, the driving force of heat transfer is reduced, the power consumption of refrigeration equipment is reduced, and the energy conservation of the building is realized. The sunlight reflectance of the product of the invention can reach more than 0.8, which is higher than the requirement that the sunlight reflectance of white reflective heat-insulating coating for buildings specified in national standard GB/T25261-2010 reflective heat-insulating coating for buildings is more than or equal to 0.80; although the Chinese patent application 2015104154431 can obtain titanium titanite, the technology only recognizes that rutile which can be remained for stabilizing the formation of the titanium titanite can cause the problem of yellowing of ceramic glaze, so that the content of titanium dioxide in the glaze is lower than 4%, and the titanium dioxide cannot be used for preparing energy-saving reflective heat-insulating ceramic. The invention aims to provide a novel reflective heat-insulating material, belonging to a brand-new ceramic product.
3) The ceramic product has very good weather resistance and can hardly be degraded by sunlight and the like, and the reflective heat-insulating ceramic glazed tile has small change of the reflectivity of the sunlight after long-term use and can be permanently used; the coating has poor weather resistance, and the coating must be recoated after being used for about 10 years generally, so that the existing reflective heat-insulating coating for buildings has problems in the aspect of the aspect; therefore, the reflective heat-insulating ceramic glazed brick has good weather resistance and low cost for long-term use.
4) The invention can prepare the reflective heat-insulating ceramic glazed tile with bright, semi-bright and matte effects suitable for different buildings.
5) The invention can adjust the color according to the needs, enrich the color of the novel ceramic product and meet the market demand.
Drawings
FIG. 1 is an XRD pattern of the sample obtained in example 1.
Figure 2 is the XRD pattern of the sample obtained in example 2.
Figure 3 is an XRD pattern of the sample obtained in example 3.
Figure 4 is an XRD pattern of the sample obtained in example 4.
Figure 5 is an XRD pattern of the sample obtained in example 5.
FIG. 6 is an XRD pattern of the sample obtained in example 6.
Figure 7 is an XRD pattern of the sample obtained in example 7.
Figure 8 is an XRD pattern of the sample obtained in example 8.
Detailed description of the invention
For a better understanding of the present invention, the present invention will be further described with reference to the following drawings and examples, but the present invention is not limited thereto.
Example 1
A preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) fully mixing 26 parts of quartz, 20 parts of feldspar, 6 parts of calcite, 42 parts of titanium dioxide, 4 parts of dolomite, 1.5 parts of alumina and 0.5 part of zinc oxide, and smelting in a clinker furnace until the raw materials are completely molten, wherein the smelting temperature is 1600 ℃, and smelting to prepare clinker; the frit obtained after smelting comprises the following chemical components in percentage by mass: 40 wt% SiO2、6wt％Al2O3、2wt％Na2O、0.5wt％K2O、5wt％CaO、1wt％MgO、0.5wt％ZnO、45wt％TiO2。
2) Mixing and grinding 10 parts by mass of the frit prepared in the step 1) with 8 parts by mass of clay, 5 parts by mass of kaolin, 35 parts by mass of quartz, 15 parts by mass of feldspar, 15 parts by mass of calcite, 7 parts by mass of titanium dioxide and 5 parts by mass of talc to prepare glaze slurry.
3) Applying the glaze slip prepared in the step 2) on the green brick blank through a glaze sprayer.
4) And (3) drying the blank body applied with the glaze slip in the step 3), and sintering in a roller kiln to obtain the reflective heat-insulating ceramic glazed tile, wherein the maximum sintering temperature is 1250 ℃, and the sintering period is 60 minutes.
The crystal phase of the glaze was analyzed by an X-ray diffractometer, and the XRD pattern of the sample of example 1 was obtained (fig. 1). The strong peak in FIG. 1 is associated with titanium titanite (TiCaSiO)5) The XRD standard patterns are compared and are very consistent, and the main crystal phase of the surface glaze layer is titanium sphene crystal.
And (3) testing the solar light reflectance of the ceramic tile prepared in the step 4) according to the solar absorption ratio spectrum testing method (absolute method) of the satellite thermal control coating prepared by the method 210 in the GJB 2502-1996 satellite thermal control coating testing method. According to the relative energy distribution of sunlight in the wavelength range of heat rays, the sunlight reflectance of the sample in the wavelength range of 250-2500 nm is calculated by a weighted average method to be 0.85, which exceeds the requirement that the sunlight reflectance of a white product in GB/T25261-2010 reflective heat-insulating coating for buildings is not less than 0.80.
Example 2
A preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) fully mixing 30 parts of quartz, 25 parts of feldspar, 10.5 parts of calcite, 27 parts of titanium dioxide, 3 parts of talcum, 1.5 parts of alumina, 1 part of zinc oxide, 1 part of barium carbonate and 1 part of apatite in parts by mass, and melting into a frit in a frit furnace, wherein the melting temperature is 1550 ℃; the frit comprises the following chemical components in percentage by mass: 50 wt% SiO2、7wt％Al2O3、3wt％Na2O、7wt％CaO、1wt％MgO、1wt％ZnO、0.5wt％BaO、0.5wt％P2O5、30wt％TiO2。
2) Mixing and grinding 30 parts of the frit prepared in the step 1) with 7 parts of clay, 25 parts of quartz, 15 parts of feldspar, 15 parts of wollastonite, 5 parts of titanium dioxide and 3 parts of dolomite to prepare glaze slurry.
3) Applying the glaze slip prepared in the step 2) on the green brick blank through a glaze sprayer.
4) And (3) drying the blank body applied with the glaze slip in the step 3), and sintering in a roller kiln to obtain the reflective heat-insulating ceramic glazed tile, wherein the maximum sintering temperature is 1230 ℃, and the sintering period is 45 minutes.
The crystal phase of the glaze was analyzed by an X-ray diffractometer, and the XRD pattern of the sample of example 2 was obtained (fig. 2). The strong peak in FIG. 2 is associated with titanium titanite (TiCaSiO)5) The XRD standard patterns are compared and are very consistent, and the main crystal phase of the surface glaze layer is titanium sphene crystal.
The same test method as that of the example 1 is adopted to obtain the sunlight reflection ratio of 0.92, which is far more than the requirement of GB/T25261-2010 reflective thermal insulation coating for buildings on the sunlight reflection ratio of a white product being more than or equal to 0.80.
Example 3
A preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) fully mixing 23 parts of quartz, 25 parts of feldspar, 12 parts of ground calcium carbonate, 18 parts of titanium dioxide, 9 parts of alumina, 11 parts of talc and 2 parts of strontium carbonate, and melting into a frit in a frit furnace, wherein the melting temperature is 1550 ℃; the frit comprises the following chemical components in percentage by mass: 49 wt% SiO2、15wt％Al2O3、3wt％K2O、8wt％CaO、4wt％MgO、1wt％SrO、20wt％TiO2。
2) Mixing and grinding 50 parts of the frit prepared in the step 1), 8 parts of clay, 13 parts of quartz, 10 parts of feldspar, 10 parts of calcite, 5 parts of talcum, 2 parts of strontium carbonate, 1 part of titanium dioxide and 1 part of spodumene to prepare glaze slurry.
3) Applying the glaze slip prepared in the step 2) on the green brick blank through a glaze sprayer.
4) And (3) drying the blank body applied with the glaze slip in the step 3), and sintering in a roller kiln to obtain the reflective heat-insulating ceramic glazed tile, wherein the maximum sintering temperature is 1210 ℃, and the sintering period is 20 minutes.
The crystal phase of the glaze was analyzed by an X-ray diffractometer, and the XRD pattern of the sample of this example was obtained (FIG. 3). The strong peak in FIG. 3 is associated with titanium sphene (TiCaSiO)5) The XRD standard patterns are compared and are very consistent, and the main crystal phase of the surface glaze layer is titanium sphene crystal.
The solar reflectance of the ceramic tile produced in step 4) was determined to be 88% using the same test method as in example 1.
Example 4
A preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) fully mixing 17 parts of quartz, 35 parts of feldspar, 25.5 parts of ground calcium carbonate, 14 parts of titanium dioxide, 6 parts of calcium borate and 2.5 parts of zinc oxide, and melting into a frit in a frit furnace, wherein the melting temperature is 1530 ℃; the frit comprises the following chemical components in percentage by mass: 45 wt% SiO2、7wt％Al2O3、3wt％B2O3、4wt％Na2O、1wt％K2O、20wt％CaO、3wt％ZnO、17wt％TiO2。
2) Mixing and grinding 60 parts of the frit prepared in the step 1), 8 parts of clay, 11 parts of quartz, 10 parts of feldspar, 10 parts of calcite, 5 parts of barium carbonate, 5 parts of titanium dioxide and 1 part of bone ash to prepare glaze slurry.
3) Applying the glaze slip prepared in the step 2) on a green brick blank body through a glaze sprayer.
4) And (3) drying the blank body applied with the glaze slip in the step 3), and sintering in a roller kiln to obtain the reflective heat-insulating ceramic glazed tile, wherein the maximum sintering temperature is 1190 ℃, and the sintering period is 35 minutes.
The crystal phase of the glaze was analyzed by an X-ray diffractometer, and the XRD pattern of the sample of example 4 was obtained (fig. 4). The strong peak in FIG. 4 is associated with titanium titanite (TiCaSiO)5) The XRD standard patterns are compared and are very consistent, and the main crystal phase of the surface glaze layer is titanium sphene crystal.
The sunlight reflectance of the ceramic tile prepared in the step 4) is determined to be 95% by adopting the same test method as that of the embodiment 1, and the sunlight reflectance is far more than or equal to 0.80 of the requirement of GB/T25261-2010 reflective heat-insulating coating for building on the sunlight reflectance of a white product.
Example 5
A preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) fully mixing 50 parts of feldspar, 8 parts of calcite, 25 parts of talcum, 13 parts of titanium dioxide and 4 parts of sodium carbonate, and melting into a frit in a frit furnace, wherein the melting temperature is 1500 ℃; the frit comprises the following chemical components in percentage by mass: 50 wt% SiO2、10wt％Al2O3、10wt％Na2O、5wt％CaO、10wt％MgO、15wt％TiO2。
2) Mixing and grinding 70 parts of the frit prepared in the step 1) with 8 parts of clay, 5 parts of quartz, 5 parts of feldspar, 5 parts of wollastonite, 5 parts of talc and 2 parts of zinc oxide to prepare glaze slurry.
3) Applying the glaze slip prepared in the step 2) on the green brick blank through a glaze sprayer.
4) Drying the green body applied with the glaze slip in the step 3), and sintering in a roller kiln to obtain the reflective heat-insulating ceramic glazed tile, wherein the maximum sintering temperature is 1160 ℃, and the sintering period is 90 minutes.
The crystal phase of the glaze was analyzed by an X-ray diffractometer, and the XRD pattern of the sample of example 5 was obtained (fig. 5). The strong peak in FIG. 5 is associated with titanium sphene (TiCaSiO)5) The XRD standard patterns are compared and are very consistent, and the main crystal phase of the surface glaze layer is titanium sphene crystal.
The solar reflectance of the ceramic tile produced in step 4) was determined to be 91% by the same test method as in example 1. The solar light reflection ratio of the white product is far more than the requirement of GB/T25261-2010 reflecting and heat-insulating coating for buildings that is more than or equal to 0.80.
Example 6
A preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) fully mixing 30 parts of quartz, 33 parts of feldspar, 8 parts of calcite, 15 parts of boric acid, 9 parts of titanium dioxide, 3 parts of zinc oxide, 1 part of barium carbonate and 1 part of apatite, and melting into a frit in a frit furnace, wherein the melting temperature is 1400 ℃; the frit raw material comprises the following components in percentage by mass: 60 wt% SiO2、6wt％Al2O3、10wt％B2O3、5wt％K2O、5wt％CaO、3wt％ZnO、0.5wt％BaO、0.5wt％P2O5、10wt％TiO2。
2) Mixing and grinding 90 parts of the frit prepared in the step 1), 5 parts of clay, 5 parts of the frit prepared in the step (1) and a raw material with the mass fraction of 10% to prepare glaze slurry.
3) Applying the glaze slip prepared in the step 2) on the green brick blank through a glaze sprayer.
4) And (3) drying the blank body applied with the glaze slip in the step 3), and sintering in a roller kiln to obtain the reflective heat-insulating ceramic glazed tile, wherein the maximum sintering temperature is 1130 ℃, and the sintering period is 50 minutes.
The crystal phase of the glaze was analyzed by an X-ray diffractometer, and the XRD pattern of the sample of example 6 was obtained (fig. 6). The strong peak in FIG. 6 is associated with titanium sphene (TiCaSiO)5) XRD standard pattern.
The solar reflectance of the ceramic tile produced in step 4) was measured to be 86% by the same test method as in example 1.
Example 7
A preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) fully mixing 20 parts of quartz, 30 parts of feldspar, 35.5 parts of ground calcium carbonate, 6.5 parts of titanium dioxide and 8 parts of zinc oxide, and melting into a frit in a frit furnace, wherein the melting temperature is 1450 ℃; by the natureThe frit raw material comprises the following components in percentage by weight: 46 wt% SiO2、7wt％Al2O3、4wt％K2O、25wt％CaO、10wt％ZnO、8wt％TiO2。
2) Grinding the frits prepared in the step 1) to prepare glaze slip.
3) Applying the glaze slip prepared in the step 2) on a green brick blank body through a glaze sprayer.
4) And (3) drying the blank body applied with the glaze slip in the step 3), and sintering in a roller kiln to obtain the reflective heat-insulating ceramic glazed tile, wherein the maximum sintering temperature is 1100 ℃, and the sintering period is 40 minutes.
The crystal phase of the glaze was analyzed by an X-ray diffractometer, and the XRD pattern of the sample of example 7 was obtained (fig. 7). The strong peak in FIG. 7 is associated with titanium sphene (TiCaSiO)5) The XRD standard patterns are compared and are very consistent, and the main crystal phase of the surface glaze layer is titanium sphene crystal.
The sunlight reflectance of the ceramic tile prepared in the step 4) is determined to be 0.83 by adopting the same test method as the example 1, and the requirement that the sunlight reflectance of a white product is more than or equal to 0.80 in GB/T25261-2010 reflective heat-insulating coating for buildings is met.
Example 8
A preparation method of a reflective heat-insulating ceramic glazed tile comprises the following steps:
1) fully mixing 40 parts of quartz, 38 parts of spodumene, 11 parts of calcite, 7 parts of titanium dioxide and 4 parts of lithium carbonate, and melting the mixture in a frit furnace to prepare frit, wherein the melting temperature is 1550 ℃; the frit raw material comprises the following components in percentage by mass: the frit had a chemical composition: 70 wt% SiO2、10wt％Al2O3、5wt％Li2O、7wt％CaO、8wt％TiO2。
2) Grinding the frits prepared in the step 1) to prepare glaze slip.
3) Applying the glaze slip prepared in the step 2) on a green brick blank body through a glaze sprayer.
4) And (3) drying the blank body applied with the glaze slip in the step 3), and firing the dried blank body in a roller kiln to obtain the reflective heat-insulating ceramic glazed tile, wherein the maximum firing temperature is 1180 ℃, and the firing period is 80 minutes.
The crystal phase of the glaze was analyzed by an X-ray diffractometer, and the XRD pattern of the sample of example 8 was obtained (fig. 8). The strong peak in FIG. 8 is associated with titanium sphene (TiCaSiO)5) The XRD standard patterns are compared and are very consistent, and the main crystal phase of the surface glaze layer is titanium sphene crystal.
The solar reflectance of the ceramic tile produced in step 4) was determined to be 81% by the same test method as in example 1.
As can be seen from the above examples, the invention only needs to mix and grind the prepared frit and the raw meal to prepare the glaze slurry, and the grinding workload is small; in addition, the titanium element is introduced partially or completely in the form of the frit, so that the surface glaze layer of the ceramic tile taking titanium sphene crystals as a main crystal phase can be obtained in a firing period of 20-90 min, the requirement of rapid firing in industrial production is met, and the defects of complicated preparation process and high cost of the Chinese patent application 2015104154431 are greatly overcome.
The method comprises the steps of melting partial titanium, calcium and other components into a frit, and mixing the frit with a certain amount of raw materials to obtain a glaze layer taking titanium sphene crystals as main crystals on the surface of the ceramic tile; because the glaze layer contains titanium sphene crystal phase with high reflectivity to full-wave band sunlight, the reflection effect of the ceramic tile to solar heat radiation is effectively improved, the temperature of the outer wall of a building can be reduced, the indoor and outdoor temperature difference is reduced, the driving force of heat transfer is reduced, the power consumption of refrigeration equipment is reduced, and the energy conservation of the building is realized. The sunlight reflectance of the product of the invention can reach more than 0.8, which is higher than the requirement that the sunlight reflectance of white reflective heat-insulating coating for buildings specified in national standard GB/T25261-2010 reflective heat-insulating coating for buildings is more than or equal to 0.80;
because the ceramic product has very good weatherability and can hardly be degraded by sunlight and the like, the reflective heat-insulating ceramic glazed tile has small change of the reflectivity of the sunlight after long-term use and can be permanently used; the coating has poor weather resistance, and the coating must be recoated after being used for about 10 years generally, so that the existing reflective heat-insulating coating for buildings has problems in the aspect of the aspect; therefore, the reflective heat-insulating ceramic glazed brick has good weather resistance and low cost for long-term use.
Claims (6)
1. A preparation method of a reflective heat-insulation ceramic glazed tile is characterized by comprising the following steps:
1) mixing the raw materials of the frit, and melting the raw materials in a frit furnace to prepare the frit, wherein the melting temperature is 1400-1600 ℃ until the raw materials are completely melted; the main chemical composition of the frit is as follows:
2) mixing and grinding the frit prepared in the step 1) and the raw material to prepare glaze slurry, wherein the frit accounts for 10-100% of the total mass of the raw material, and the content of titanium dioxide in the glaze is not lower than 8% of the total mass;
3) applying the glaze slip prepared in the step 2) on a blank body;
4) and (3) drying the blank body applied with the glaze slurry in the step 3), and then sintering at the temperature of 1100-1250 ℃ for 20-90 min to prepare the reflective heat-insulating ceramic glazed tile with the glaze layer taking titanium sphene crystals as a main crystal phase, so that the high reflection effect on sunlight is realized, and the reflective heat-insulating effect of the reflective heat-insulating ceramic glazed tile is improved.
2. The method for preparing a reflective insulating ceramic glazed tile according to claim 1, wherein the raw material comprises one or more of clay, kaolin, quartz, alumina, feldspar, calcite, talc, dolomite, wollastonite, titanium dioxide, barium carbonate, strontium carbonate, zinc oxide, bone ash and spodumene.
3. The method for preparing a reflective insulating ceramic glazed tile according to claim 1, wherein the glaze slurry of step 3) is applied on the green body by means of an enamel sprayer.
4. The process for preparing a ceramic glazed tile with reflective and thermal insulation according to claim 1, wherein the firing is carried out in a roller kiln.
5. The method for preparing a reflective insulating ceramic glazed tile according to claim 1, wherein the frit comprises the following main chemical components in percentage by mass:
6. the preparation method of the reflective heat-insulating ceramic glazed tile according to claim 1, wherein the thickness of the fired solar reflective layer on the surface of the reflective heat-insulating ceramic glazed tile is 0.1-3.0 mm.
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| CN111875414B (en) * | 2020-06-30 | 2022-08-05 | 蒙娜丽莎集团股份有限公司 | High solar light reflectivity ceramic plate and preparation method thereof |
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| CN115304277A (en) * | 2022-08-03 | 2022-11-08 | 重庆唯美陶瓷有限公司 | Titanium white opacified ground glaze and ceramic plate |
| CN115650587B (en) * | 2022-12-26 | 2023-03-21 | 新明珠集团股份有限公司 | Reflective heat-insulation glaze, reflective heat-insulation ceramic tile and preparation method and application thereof |
| CN115974411B (en) * | 2023-02-02 | 2024-03-08 | 重庆唯美陶瓷有限公司 | Ceramic tile base glaze, ceramic tile and preparation method thereof |
| CN116715539B (en) * | 2023-08-07 | 2023-11-07 | 新明珠集团股份有限公司 | High-reflection heat-insulation ceramic glaze layer, ceramic glaze, ceramic tile and preparation method thereof |
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