KR102347575B1 - Manufacturing method of high fluidity granule powder for ceramic tile and manufacturing method of ceramic tile - Google Patents

Abstract

The present invention relates to the steps of preparing granular powder for ceramic tile, preparing a saturated fatty acid coating solution, and coating the saturated fatty acid coating solution on the surface of the granular powder for ceramic tile and surface-treated with the saturated fatty acid coating solution. The present invention relates to a method for producing a high-fluidity granular powder for ceramic tiles, comprising obtaining a powder, and a method for producing a ceramic tile using the high-flowability granular powder for ceramic tiles. According to the present invention, excellent fluidity can be uniformly distributed in a molding mold for manufacturing a porcelain tile having a three-dimensional surface, and flowability can be secured to cope with local stress.

Description

The manufacturing method of high fluidity granule powder for ceramic tile and manufacturing method of ceramic tile

The present invention relates to a method for producing a high-flowing granular powder for ceramic tile and a method for producing a ceramic tile, and more particularly, it has excellent fluidity so that it can be uniformly distributed in a molding mold for producing a ceramic tile having a three-dimensional surface. The present invention relates to a method for producing a high-flowability granular powder for ceramic tile, which can secure flowability to cope with local stress, and a method for manufacturing a ceramic tile using the high-flowability granular powder for ceramic tile.

Tiles are products that are widely used in daily life.

Tiles may be classified into interior tiles, exterior tiles, floor tiles, and mosaic tiles according to their use. In general, interior tiles are manufactured using porcelain, stone substrates or ceramic substrates, exterior tiles are manufactured using porcelain or stone substrates, floor tiles are manufactured using porcelain or stone substrates, and mosaic tiles are It can be manufactured using a magnetic material.

Tiles may be classified into porcelain tiles, stone-based tiles, and ceramic tiles according to their materials and characteristics. In general, porcelain tile is transparent, hard and dense, and has the characteristic of making a metallic clear sound when struck. It is highly absorbent and has the characteristic of making a dull sound when struck.

Recently, with the improvement of quality of life, the demand for high-end design architectural ceramic tiles in residential spaces is increasing. Therefore, products of architectural ceramic tiles with a three-dimensional surface texture are being released, and product development centered on CMF (Color-Material-Finishing, Color-Material-Finishing) is becoming active.

In order to complete the three-dimensional surface of architectural ceramic tiles, a metal forming mold with a three-dimensional design reflected in the dry forming process of the tile manufacturing process is required, and the development of a substrate capable of withstanding the local stress in the intaglio/embossed parts during the pressing process is necessary. very important.

As the most important property for manufacturing ceramic tile having a three-dimensional surface, the powder for manufacturing ceramic tile must have high flowability. should be able to obtain

Republic of Korea Patent Publication No. 10-1906155

The problem to be solved by the present invention is high fluidity for porcelain tile that has excellent fluidity, can be uniformly distributed in a molding mold for manufacturing porcelain tile having a three-dimensional surface, and can secure flowability to cope with local stress An object of the present invention is to provide a method for producing a granular powder and a method for producing a ceramic tile using the highly fluid granular powder for ceramic tiles.

The present invention relates to the steps of preparing granular powder for ceramic tile, preparing a saturated fatty acid coating solution, and coating the saturated fatty acid coating solution on the surface of the granular powder for ceramic tile and surface-treated with the saturated fatty acid coating solution. Comprising the step of obtaining a powder, the saturated fatty acid coating solution is palmitic acid, butyric acid (C ₄ H ₈ O ₂ , Butyric acid), stearic acid (C ₁₈ H36O ₂ , Stearic acid), valeric acid ( C ₅ H ₁₀ O ₂ , Valeric acid), caproic acid (C ₆ H ₁₂ O ₂ , Caproic acid), caprylic acid (C ₈ H ₁₆ O ₂ , Carrylic acid), pelargonic acid (C ₉ H ₁₈ O _{2 )} , Pelargonic acid), lauric acid (C ₁₂ H ₂₄ O ₂ , Lauric acid) _{, tridecylic acid (C 13} H ₂₆ O ₂ , Tridecylic acid), myristic acid (C ₁₄ H ₂₈ O ₂ , Myristic acid), Margaric acid (C ₁₇ H ₃₄ O ₂ , Margaric acid), arachidic acid (C ₆ H ₁₂ O ₂ , Arachidic acid), behenic acid (C ₁₁ H ₂₂ O, Behenic acid), lignoceric acid (C ₁₂ H ₂₄ O, Lignoceric acid), cerotic acid (C ₂₆ H ₅₂ O ₂ , Cerotic acid), montanic acid (C ₂₈ H ₅₆ O ₂ , Montanic acid) and hentriacontylic acid (C ₃₁ H ₆₂ O ₂ , Hentriacontylic acid) ) provides a method for producing a high-flowing granular powder for porcelain tile comprising at least one saturated fatty acid selected from the group consisting of.

The step of preparing the granular powder for porcelain tile includes 10-15 wt% of limestone powder, 20-25 wt% of clay powder, 35-45 wt% of porcelain powder, 10-15 wt% of pyrophyllite powder and 8 clay powder as starting materials. It may include the steps of preparing and mixing ∼13% to make a slurry, and spray drying the mixture in the slurry state to obtain a granular powder for ceramic tiles.

In the step of making the slurry state, 0.1 to 2 parts by weight of PVP (Polyvinylpyrrolidone) may be further mixed with respect to 100 parts by weight of the starting material.

In the step of making the slurry state, 0.1 to 2 parts by weight of PVA (polyvinyl alcohol) may be further mixed with respect to 100 parts by weight of the starting material.

In the step of making the slurry state, 0.1 to 2 parts by weight of sodium silicate may be further mixed with respect to 100 parts by weight of the starting material.

In the step of making the slurry state, 0.1 to 2 parts by weight of gelatin may be further mixed with respect to 100 parts by weight of the starting material.

In the step of making the slurry state, 0.1 to 2 parts by weight of sugar water may be further mixed with respect to 100 parts by weight of the starting material.

The saturated fatty acid coating solution may be prepared by mixing saturated fatty acid with a solvent, and the solvent may include water (H ₂ O).

Preferably, the coating is carried out so that the content of the saturated fatty acid coating solution is 1 to 10 parts by weight based on 100 parts by weight of the granular powder for ceramic tiles.

In addition, the present invention comprises the steps of molding and drying the high-fluidity granular powder for porcelain tile into a desired shape; There is provided a method of manufacturing a ceramic tile comprising the steps of forming a secondary glaze layer, forming a secondary glaze layer on the first glaze layer, and secondary firing the resultant product on which the secondary glaze layer is formed. .

According to the present invention, the fluidity of the granular powder for ceramic tiles is excellent.

Since the granular powder for ceramic tile has excellent fluidity, it can be uniformly distributed in a molding mold for producing a ceramic tile having a three-dimensional surface, and flowability can be secured to cope with local stress.

Because the granular powder for ceramic tiles has excellent fluidity, it is possible to manufacture ceramic tile substrates that can withstand the stress generated locally in the intaglio/embossed parts during the molding process.

1 and 2 are scanning electron microscope (SEM) pictures showing the granular powder for porcelain tile prepared according to Experimental Example 4.
3 is a view showing an X-ray diffraction (XRD) pattern of the granular powder for porcelain tile prepared according to Experimental Example 4.
4 is a graph showing the particle size distribution of the granular powder for porcelain tile prepared according to Experimental Example 4.
5 is a photograph showing the granular powder for porcelain tile prepared according to Experimental Example 4.
6 is a photograph showing the granular powder for ceramic tiles coated with hydrophobic silica solution according to Experimental Example 7 and surface-coated with hydrophobic silica.
7 is a view illustrating a method for measuring the fluidity of granular powder for ceramic tiles.

Hereinafter, preferred embodiments according to the present invention will be described in detail with reference to the accompanying drawings. However, the following examples are provided so that those of ordinary skill in the art can fully understand the present invention, and can be modified in various other forms, and the scope of the present invention is limited to the examples described below it is not going to be

When it is said that any one component "includes" another component in the detailed description or claims of the invention, it is not construed as being limited to only the component, unless otherwise stated, and other components are further added. It should be understood as being able to include

Tiles may be classified into interior tiles, exterior tiles, floor tiles, and mosaic tiles according to their use. In general, interior tiles are manufactured using porcelain, stone substrates or ceramic substrates, exterior tiles are manufactured using porcelain or stone substrates, floor tiles are manufactured using porcelain or stone substrates, and mosaic tiles are It can be manufactured using a magnetic material.

Tiles may be classified into porcelain tiles, stone-based tiles, and ceramic tiles according to their materials and characteristics. In general, porcelain tile is transparent, hard and dense, and has the characteristic of making a metallic clear sound when struck. It is highly absorbent and has the characteristic of making a dull sound when struck. In general, porcelain tiles are fired at a temperature of 1000°C or higher, and exhibit a water absorption rate of 3% or less. Stone-based tiles are fired at a temperature of about 1200° C. and exhibit a water absorption rate of 5% or less. The ceramic tile is fired at a temperature of 1000°C or higher, and exhibits a water absorption rate of 18% or less.

Hereinafter, the term 'porcelain tile' is used to include a ceramic tile and a porcelain tile.

According to a preferred embodiment of the present invention, the method for producing a high-flowing granular powder for ceramic tile includes the steps of: preparing a granular powder for ceramic tile; preparing a saturated fatty acid coating solution; and coating a fatty acid coating solution to obtain a granular powder for ceramic tiles surface-treated with a saturated fatty acid coating solution, wherein the saturated fatty acid coating solution is palmitic acid, butyric acid (C ₄ H ₈ O ₂ , Butyric acid) ), stearic acid (C ₁₈ H36O ₂ , Stearic acid), valeric acid (C ₅ H ₁₀ O ₂ , Valeric acid), caproic acid (C ₆ H ₁₂ O ₂ , Caproic acid), caprylic acid (C ₈ H ₁₆ O ₂ , Carrylic acid), pelargonic acid (C ₉ H ₁₈ O ₂ , Pelargonic acid), lauric acid (C ₁₂ H ₂₄ O ₂ , Lauric acid) _{, tridecylic acid (C 13} H ₂₆ O ₂ , Tridecylic acid) , Myristic acid (C ₁₄ H ₂₈ O ₂ , Myristic acid), margaric acid (C ₁₇ H ₃₄ O ₂ , Margaric acid), arachidic acid (C ₆ H ₁₂ O ₂ , Arachidic acid), behenic acid (C ₁₁ H ₂₂ O, Behenic acid), lignoceric acid (C ₁₂ H ₂₄ O, Lignoceric acid), cerotic acid (C ₂₆ H ₅₂ O ₂ , Cerotic acid), montanic acid (C ₂₈ H ₅₆ O ₂ , Montanic acid) ) and _{hentriacontylic acid (C 31} H ₆₂ O ₂ , Hentriacontylic acid), and includes at least one saturated fatty acid selected from the group consisting of.

The step of preparing the granular powder for porcelain tile includes 10-15 wt% of limestone powder, 20-25 wt% of clay powder, 35-45 wt% of porcelain powder, 10-15 wt% of pyrophyllite powder and 8 clay powder as starting materials. It may include the steps of preparing and mixing ∼13% to make a slurry, and spray drying the mixture in the slurry state to obtain a granular powder for ceramic tiles.

In the step of making the slurry state, 0.1 to 2 parts by weight of PVP (Polyvinylpyrrolidone) may be further mixed with respect to 100 parts by weight of the starting material.

In the step of making the slurry state, 0.1 to 2 parts by weight of PVA (polyvinyl alcohol) may be further mixed with respect to 100 parts by weight of the starting material.

In the step of making the slurry state, 0.1 to 2 parts by weight of sodium silicate may be further mixed with respect to 100 parts by weight of the starting material.

In the step of making the slurry state, 0.1 to 2 parts by weight of gelatin may be further mixed with respect to 100 parts by weight of the starting material.

In the step of making the slurry state, 0.1 to 2 parts by weight of sugar water may be further mixed with respect to 100 parts by weight of the starting material.

The saturated fatty acid coating solution may be prepared by mixing saturated fatty acid with a solvent, and the solvent may include water (H ₂ O).

Preferably, the coating is carried out so that the content of the saturated fatty acid coating solution is 1 to 10 parts by weight based on 100 parts by weight of the granular powder for ceramic tiles.

A method of manufacturing a ceramic tile according to a preferred embodiment of the present invention comprises the steps of molding and drying the high-fluidity granular powder for ceramic tile into a desired shape, and first firing the dried resultant to form a ceramic tile base layer; , forming a first glaze layer on the ceramic tile base layer, forming a second glaze layer on the first glaze layer, and secondary firing the resultant product on which the second glaze layer is formed do.

Hereinafter, a method for producing a high-fluidity granular powder for porcelain tile according to a preferred embodiment of the present invention will be described in more detail.

With the improvement of the quality of life, the demand for high-end design architectural ceramic tiles in residential spaces is increasing. Therefore, products of architectural ceramic tiles with a three-dimensional surface texture are being released, and product development centered on CMF (Color-Material-Finishing, Color-Material-Finishing) is becoming active.

In order to complete the three-dimensional surface of architectural ceramic tiles, a metal forming mold with a three-dimensional design reflected in the dry forming process of the tile manufacturing process is required, and the development of a substrate capable of withstanding the local stress in the intaglio/embossed parts during the pressing process is necessary. very important.

As the most important property for manufacturing ceramic tile having a three-dimensional surface, the powder for manufacturing ceramic tile must have high flowability. should be able to obtain

A powder for producing a ceramic tile having a three-dimensional surface is prepared in the form of a granule powder by using a spray dryer.

To prepare granular powder for porcelain tile, 10-15 wt% of limestone powder, 20-25 wt% of clay powder, 35-45 wt% of ceramic powder, 10-15 wt% of pyrophyllite powder, and 8-13% of clay powder Prepare and mix to make a slurry.

The mixing may use a ball milling process or the like.

When describing the ball milling process, a starting material is charged into a ball milling machine together with a solvent such as water. It is mechanically mixed by rotating it at a constant speed using a ball mill. The ball used for the ball milling is preferably a ball made of a ceramic material such as alumina or zirconia. Adjust the size of the ball, the milling time, and the rotation speed per minute of the ball mill. For example, the size of the ball can be set in the range of about 1 mm to 50 mm, and the rotation speed of the ball mill can be set in the range of about 50 to 500 rpm. Ball milling is preferably performed for 10 minutes to 48 hours for uniform mixing. The mixture that has been subjected to the wet mixing process as described above is pulverized to form a slurry.

In the step of making the slurry state, 0.1 to 2 parts by weight of PVP (Polyvinylpyrrolidone) may be further mixed with respect to 100 parts by weight of the starting material. When PVP (Polyvinylpyrrolidone) is mixed with the starting material, the fluidity of the obtained granular powder for ceramic tiles can be increased.

In the step of making the slurry state, 0.1 to 2 parts by weight of PVA (polyvinyl alcohol) may be further mixed with respect to 100 parts by weight of the starting material. When polyvinyl alcohol (PVA) is mixed with the starting material, the fluidity of the obtained granular powder for ceramic tiles can be increased.

In the step of making the slurry state, 0.1 to 2 parts by weight of sodium silicate may be further mixed with respect to 100 parts by weight of the starting material. When sodium silicate is mixed with the starting material, the fluidity of the obtained granular powder for ceramic tiles can be increased.

In the step of making the slurry state, 0.1 to 2 parts by weight of gelatin may be further mixed with respect to 100 parts by weight of the starting material. When gelatin is mixed with the starting material, the fluidity of the obtained granular powder for porcelain tile can be increased.

In the step of making the slurry, 0.1 to 2 parts by weight of sugar water (preferably having a concentration of 90% or more) may be further mixed with respect to 100 parts by weight of the starting material. When sugar water is mixed with the starting material, the fluidity of the obtained granular powder for porcelain tile can be increased.

The mixture in the slurry state is spray dried to obtain a granular powder for ceramic tiles. Since the spray drying is generally well known, a detailed description thereof will be omitted here.

To ensure that the granular powder for ceramic tile has high fluidity, the surface of the granular powder for ceramic tile is hydrophobic surface treated with a hydrophobic silica solution by applying a fluidized bed coating process, or surface treated with a saturated fatty acid coating solution (coating) process).

Hereinafter, a method for preparing the hydrophobized silica solution will be described in detail.

The hydrophobized silica solution is a solution containing silica exhibiting hydrophobicity.

The hydrophobized silica solution may be a solution containing silica surface-treated with a silane coupling agent. The silica is surface-treated by the silane coupling agent to exhibit hydrophobicity.

For the preparation of the hydrophobized silica solution, an _{acid is added to a mixed solution of silica, alcohol, and water (H 2} O) to adjust the pH to 1 to 5, and a silane coupling agent is added to the pH-adjusted solution, and the It can be prepared by stirring at a temperature of 40 to 70 ℃ lower than the boiling point of alcohol.

As the silica, it is preferable to use particles having an average particle diameter of 2 to 100 nm.

The acid may include at least one material selected from the group consisting of hydrochloric acid (HCl), nitric acid (HNO ₃ ), and sulfuric acid (H ₂ SO _{4 ).}

The silane coupling agent is glycidoxypropyl methyldimethoxy silane, glycidoxypropyl trimethoxy silane, glycidoxypropyl triethoxy silane, methacryloxy Methacryloxypropyl methydimethoxy silane, methacryloxypropyl trimethoxy silane, Methacryloxypropyl triethoxy silane and Acryloxypropyl trimethoxy silan ) may include one or more substances selected from the group consisting of.

Hereinafter, a method for preparing a saturated fatty acid coating solution will be described in detail.

A saturated fatty acid coating solution is prepared by mixing a saturated fatty acid with a solvent. The mixing is preferably performed at a temperature lower than the boiling point of the solvent. Preferably, the solvent and the saturated fatty acid are mixed in a weight ratio of 1:1 to 3:1.

The solvent may include water (H ₂ O).

The saturated fatty acid is palmitic acid, butyric acid (C ₄ H ₈ O ₂ , Butyric acid), stearic acid (C ₁₈ H36O ₂ , Stearic acid), valeric acid (C ₅ H ₁₀ O ₂ , Valeric acid) , caproic acid (C ₆ H ₁₂ O ₂ , Caproic acid), caprylic acid (C ₈ H ₁₆ O ₂ , Carrylic acid), pelargonic acid (C ₉ H ₁₈ O ₂ , Pelargonic acid), lauric acid (C ₁₂ H ₂₄ O ₂ , Lauric acid), _{tridecylic acid (C 13} H ₂₆ O ₂ , Tridecylic acid), myristic acid (C ₁₄ H ₂₈ O ₂ , Myristic acid), margaric acid (C ₁₇ H ₃₄ O _{2 )} , Margaric acid), arachidic acid (C ₆ H ₁₂ O ₂ , Arachidic acid), behenic acid (C ₁₁ H ₂₂ O, Behenic acid), lignoceric acid (C ₁₂ H ₂₄ O, Lignoceric acid), serotic acid (C ₂₆ H ₅₂ O ₂ , Cerotic acid), montanic acid (C ₂₈ H ₅₆ O ₂ , Montanic acid), and hentriacontylic acid (C ₃₁ H ₆₂ O ₂ , Hentriacontylic acid) At least one substance selected from the group consisting of may include

In order to improve hardness while surface-treating the granular powder for ceramic tile, the hydrophobized silica solution is coated on the surface of the granular powder for ceramic tile to obtain a granular powder for ceramic tile surface-coated with silica having hydrophobicity, or The surface of the granular powder for tiles is coated with the saturated fatty acid coating solution to obtain a granular powder for ceramic tiles surface-treated with the saturated fatty acid coating solution.

The surface coating process of the granular powder for ceramic tiles using the hydrophobic silica solution or the saturated fatty acid coating solution may be performed using a fluidized bed coater. The temperature inside the coating tank is raised to about 40-70° C. and maintained, the granular powder is circulated, and the hydrophobized silica solution or the saturated fatty acid coating solution is sprayed at a rate of about 1-5 ml/min. The content of the hydrophobized silica solution is preferably 1 to 10 parts by weight based on 100 parts by weight of the granular powder to perform the coating. It is preferable to carry out the coating with the content of the saturated fatty acid coating solution being 1 to 10 parts by weight based on 100 parts by weight of the granular powder.

The granular powder for ceramic tiles surface-treated with a hydrophobized silica solution or a saturated fatty acid coating solution has the advantage of excellent fluidity. Accordingly, it can be uniformly distributed in a molding mold for manufacturing a ceramic tile having a three-dimensional surface, and flowability can be secured to cope with local stress.

Because the granular powder for ceramic tiles has excellent fluidity, it is possible to manufacture ceramic tile substrates that can withstand the stress generated locally in the intaglio/embossed parts during the molding process.

Hereinafter, a method for manufacturing a ceramic tile using the highly fluid granular powder for ceramic tile according to a preferred embodiment of the present invention will be described in more detail.

1 is a view showing the structure of a ceramic tile.

Referring to FIG. 1 , the ceramic tile is made into a compact using the above-described high-fluidity granular powder for ceramic tile, and the first glaze composition is applied on the base layer 10 formed by primary firing to form a first glaze layer 20. The second glaze layer 30 is formed by applying a second glaze composition on the first glaze layer 20 and then secondary firing. The first glaze layer 20 is called an engobe layer, and serves as an intermediate layer that can hide the color of the base layer 10 and control the thermal expansion of the base layer 10 and the second glaze layer 30 . . The secondary glaze layer 30 has a function of strengthening (protecting) and decorating the surface of the ceramic tile.

High-flowing granular powder for ceramic tiles is molded into a desired shape, and a drying process is performed. The molding may use various methods, such as generally known injection molding (slip casting), pressure molding, and the like. The drying process is preferably performed for 10 minutes to 48 hours at a temperature of room temperature to 150 ℃.

The molded result is first fired.

Hereinafter, the primary firing process will be described in detail.

The molded result is charged into a furnace such as an electric furnace and a primary firing process is performed. The primary firing process is preferably performed at a temperature of about 1000 to 1250° C. for about 1 to 48 hours. It is desirable to keep the pressure inside the furnace constant during the first firing.

The primary firing is preferably made at a temperature of about 1000 to 1250 ℃. If the firing temperature is less than 1000°C, the thermal or mechanical properties of the ceramic tile may be poor due to incomplete firing.

It is preferable to increase the temperature up to the firing temperature at a temperature increase rate of 1 to 50 °C/min. If the temperature increase rate is too slow, it takes a long time to decrease productivity. Therefore, it is preferable to raise the temperature at a temperature increase rate in the above range.

In addition, the primary firing is preferably maintained for 1 to 48 hours at the firing temperature. If the firing time is too long, energy consumption is high, which is uneconomical, and it is difficult to expect further firing effects. If the firing time is too short, the properties of the ceramic tile may be poor due to incomplete firing.

In addition, the primary firing is preferably performed in an oxidizing atmosphere (eg, oxygen (O ₂ ) or air (air) atmosphere).

After performing the primary firing process, the furnace temperature is lowered to unload the primary firing result. The furnace cooling may be performed in a natural state by shutting off the furnace power, or may be cooled by arbitrarily setting a temperature drop rate (eg, 10° C./min). It is desirable to keep the pressure inside the furnace constant even while the furnace temperature is lowered.

A first glaze layer (Engobe layer) is formed on top of the first fired ceramic tile base layer. A first glaze composition is prepared to form a first glaze layer on the first fired ceramic tile base layer, and the first glaze composition is applied to the first fired ceramic tile base surface and dried. The first glaze layer is preferably formed to a thickness of about 50 to 300㎛. Preferably, the first glaze composition is in a slurry state including a solid content and a solvent, and the solvent is contained in an amount of 30 to 80 parts by weight based on 100 parts by weight of the solid content in the first glaze composition.

A second glaze composition is applied on top of the first glaze layer and dried to form a second glaze layer. The second glaze composition is in a slurry state including a solid content and a solvent, and the solvent is preferably contained in an amount of 30 to 80 parts by weight based on 100 parts by weight of the solid content in the second glaze composition. The second glaze layer is preferably formed to a thickness of about 70 to 500 ㎛.

As an example, the solid content of the first glaze composition is SiO ₂ 55 to 67 wt%, Al ₂ O _{3 8 to} 14.5 wt%, Fe ₂ O ₃ 0.01 to 0.8 wt%, TiO ₂ 0.1 to 6 wt%, CaO 3 -9 wt%, MgO 0.01-1.5 wt%, Na ₂ O ₃ 0.1-4 wt%, K ₂ O 0.1-4 wt%, P ₂ O ₅ 0.01-0.8 wt% and ZrO _{2 1.5-7.5 wt%} The solid content of the second glaze composition is SiO ₂ 41-53 wt%, Al ₂ O ₃ 8-20 wt%, K ₂ O 0.1-4 wt%, ZrO ₂ 2-12 wt%, Fe ₂ O _{3 3 to 13} % by weight, B ₂ O ₃ 5 to 17% by weight, CaO 0.1 to 8% by weight, and P 2 O _{5 2 to} 12% by weight may be included.

The glaze layer forms a vitreous film on the tile surface where micropores exist, increasing strength and reducing absorption, and expressing unique color and texture. The glazing method can be carried out in various ways, for example, by immersing the porcelain tile substrate (or porcelain tile substrate with the Enkobe layer formed thereon) that has been fired in the glaze composition, or by applying the glaze composition to the surface of the porcelain tile substrate layer with a tool such as a brush. (or the upper part of the engobe layer), or a method of spraying the glaze composition on the surface of the porcelain tile base layer (or the upper part of the engobe layer) with a spray device, etc. can be used.

The porcelain tile on which the second glaze layer is formed is charged into a furnace such as an electric furnace, and a secondary firing (chaebol) process is performed.

Hereinafter, the secondary firing process will be described in detail.

The resultant (porcelain tile) formed with the second glaze layer is charged into a furnace such as an electric furnace, and a secondary firing process is performed. The secondary firing process is preferably performed at a temperature of about 1000 to 1100° C. for a predetermined time (eg, about 2 to 10 minutes). It is desirable to keep the pressure inside the furnace constant during the secondary firing.

The secondary firing is preferably made at a temperature of about 1000 to 1100 ℃. If the firing temperature is less than 1000℃, the solid content of the glaze composition is incompletely melted, so the surface of the porcelain tile may not be smooth or the gloss (gloss) characteristics may be poor. to be.

It is preferable to increase the temperature up to the firing temperature at a temperature increase rate of 1 to 50 °C/min. If the temperature increase rate is too slow, it takes a long time to decrease productivity. The surface of the ceramic tile may not be smooth due to the rapid temperature rise.

In addition, the secondary firing is preferably maintained at the firing temperature for 1 to 48 hours. If the firing time is too long, energy consumption is high, which is uneconomical, and it is difficult to expect further firing effects. If the firing time is too short, the properties of the ceramic tile may be poor due to incomplete firing.

In addition, the secondary firing is preferably performed in an oxidizing atmosphere (eg, oxygen (O ₂ ) or air (air) atmosphere).

After performing the secondary firing process, the furnace temperature is lowered to unload the secondary firing result. The furnace cooling may be performed in a natural state by shutting off the furnace power, or may be cooled by arbitrarily setting a temperature drop rate (eg, 10° C./min). It is desirable to keep the pressure inside the furnace constant even while the furnace temperature is lowered.

Hereinafter, experimental examples according to the present invention are specifically presented, and the present invention is not limited to the experimental examples presented below.

<Experimental Example 1>

As starting materials, 12 wt% of limestone powder, 24 wt% of clay powder, 40 wt% of ceramic powder, 13 wt% of pyrophyllite powder and 11 wt% of white clay powder were prepared and mixed.

The starting materials were mixed using a ball milling process. The starting materials were charged into a ball milling machine together with water, and mechanically mixed by rotating at a constant speed using the ball milling machine. The ball used for the ball milling was a zirconia ball, the size of the ball was about 3 mm, the rotation speed of the ball mill was set to about 100 rpm, and the ball milling was performed for 24 hours for uniform mixing, etc. . The mixture subjected to the wet mixing process as described above was in a slurry state having a moisture content of 40%.

The mixture in the slurry state was spray dried to obtain a granular powder for ceramic tiles. For the spray drying, a nozzle having a size of 2.5 mm was used, and the inlet temperature was 160°C.

<Experimental Example 2>

12% by weight of limestone powder, 24% by weight of clay powder, 40% by weight of porcelain powder, 13% by weight of pyrophyllite powder and 11% by weight of clay powder were prepared as starting materials, and PVP (Polyvinylpyrrolidone) 0.5% by weight based on 100 parts by weight of the starting material After preparing parts, the starting material and the PVP were mixed.

A ball milling process was used for mixing the starting material and the PVP. The starting material and PVP were charged into a ball milling machine together with water, and mechanically mixed by rotating at a constant speed using the ball milling machine. The ball used for the ball milling was a zirconia ball, the size of the ball was about 3 mm, the rotation speed of the ball mill was set to about 100 rpm, and the ball milling was performed for 24 hours for uniform mixing, etc. . The mixture subjected to the wet mixing process as described above was in a slurry state having a moisture content of 40%.

The mixture in the slurry state was spray dried to obtain a granular powder for ceramic tiles. For the spray drying, a nozzle having a size of 2.5 mm was used, and the inlet temperature was 160°C.

<Experimental Example 3>

12% by weight of limestone powder, 24% by weight of clay powder, 40% by weight of ceramic powder, 13% by weight of pyrophyllite powder and 11% by weight of clay powder were prepared as starting materials, and 1 weight of PVP (Polyvinylpyrrolidone) based on 100 parts by weight of the starting material After preparing parts, the starting material and the PVP were mixed.

A ball milling process was used to mix the starting material and the PVP. The starting material and PVP were charged into a ball milling machine together with water, and mechanically mixed by rotating at a constant speed using the ball milling machine. The ball used for the ball milling was a zirconia ball, the size of the ball was about 3 mm, the rotation speed of the ball mill was set to about 100 rpm, and the ball milling was performed for 24 hours for uniform mixing, etc. . The mixture subjected to the wet mixing process as described above was in a slurry state having a moisture content of 40%.

The mixture in the slurry state was spray dried to obtain a granular powder for ceramic tiles. For the spray drying, a nozzle having a size of 2.5 mm was used, and the inlet temperature was 160°C.

<Experimental Example 4>

12% by weight of limestone powder, 24% by weight of clay powder, 40% by weight of porcelain powder, 13% by weight of pyrophyllite powder and 11% by weight of clay powder were prepared as starting materials, and PVP (Polyvinylpyrrolidone) 1.5% by weight based on 100 parts by weight of the starting material After preparing parts, the starting material and the PVP were mixed.

A ball milling process was used for mixing the starting material and the PVP. The starting material and PVP were charged into a ball milling machine together with water, and mechanically mixed by rotating at a constant speed using the ball milling machine. The ball used for the ball milling was a zirconia ball, the size of the ball was about 3 mm, the rotation speed of the ball mill was set to about 100 rpm, and the ball milling was performed for 24 hours for uniform mixing, etc. . The mixture subjected to the wet mixing process as described above was in a slurry state having a moisture content of 40%.

The mixture in the slurry state was spray dried to obtain a granular powder for ceramic tiles. For the spray drying, a nozzle having a size of 2.5 mm was used, and the inlet temperature was 160°C.

<Experimental Example 5>

12% by weight of limestone powder, 24% by weight of clay powder, 40% by weight of porcelain powder, 13% by weight of pyrophyllite powder and 11% by weight of clay powder were prepared as starting materials, and 2 weights of PVP (Polyvinylpyrrolidone) with respect to 100 parts by weight of the starting material After preparing parts, the starting material and the PVP were mixed.

A ball milling process was used for mixing the starting material and the PVP. The starting material and PVP were charged into a ball milling machine together with water, and mechanically mixed by rotating at a constant speed using the ball milling machine. The ball used for the ball milling was a zirconia ball, the size of the ball was about 3 mm, the rotation speed of the ball mill was set to about 100 rpm, and the ball milling was performed for 24 hours for uniform mixing. . The mixture subjected to the wet mixing process as described above was in a slurry state having a moisture content of 40%.

The mixture in the slurry state was spray dried to obtain a granular powder for ceramic tiles. For the spray drying, a nozzle having a size of 2.5 mm was used, and the inlet temperature was 160°C.

<Experimental Example 6>

A granular powder for ceramic tiles prepared according to Experimental Example 4 was prepared.

For the hydrophobization surface treatment of the granular powder for ceramic tiles, a silica (SiO ₂ , 50 nm, 30%) solution (hydrophobized silica solution) surface-treated with Glycidoxypropyl trimethoxy silane (GPTMS) was prepared.

The hydrophobized silica solution was mixed with colloidal silica (50 nm, 20 g), ethanol (10 g), and distilled water (20 g) in a weight ratio of 2: 1: 2, followed by stirring for 10 minutes, and hydrochloric acid (HCl, 36.5%) After addition, the pH was adjusted to 2-3, followed by further stirring at a temperature of 60 °C for 30 minutes, and GPTMS (Glycidoxypropyl trimethoxy silane) was added to the solution at a concentration of 0.01M and stirred at a temperature of 60 °C for 24 hours. was prepared.

The surface coating process of the granular powder for ceramic tiles using the hydrophobic silica solution was performed using a fluidized bed coater. The temperature inside the coating tank was raised to 60° C. and maintained, and the hydrophobic silica solution was sprayed at a rate of 2.3 ml/min while circulating the granular powder under ^{air flow @ 45 m 3 /h in consideration of the density of the granular powder.} The content of the hydrophobized silica solution was 2 parts by weight based on 100 parts by weight of the granular powder, and coating was performed. The total coating process time was carried out in 50 minutes.

<Experimental Example 7>

A granular powder for ceramic tiles prepared according to Experimental Example 4 was prepared.

For the hydrophobization surface treatment of the granular powder for ceramic tiles, a silica (SiO ₂ , 50 nm, 30%) solution (hydrophobized silica solution) surface-treated with Glycidoxypropyl trimethoxy silane (GPTMS) was prepared.

The hydrophobized silica solution was mixed with colloidal silica (50 nm, 20 g), ethanol (10 g), and distilled water (20 g) in a weight ratio of 2: 1: 2, followed by stirring for 10 minutes, and hydrochloric acid (HCl, 36.5%) After addition, the pH was adjusted to 2-3, followed by further stirring at a temperature of 60 °C for 30 minutes, and GPTMS (Glycidoxypropyl trimethoxy silane) was added to the solution at a concentration of 0.01M and stirred at a temperature of 60 °C for 24 hours. was prepared.

The surface coating process of the granular powder for ceramic tiles using the hydrophobic silica solution was performed using a fluidized bed coater. The temperature inside the coating tank was raised to 60° C. and maintained, and the hydrophobic silica solution was sprayed at a rate of 2.3 ml/min while circulating the granular powder under ^{air flow @ 45 m 3 /h in consideration of the density of the granular powder.} The content of the hydrophobized silica solution was 5 parts by weight based on 100 parts by weight of the granular powder, and coating was performed. The total coating process time was carried out in 50 minutes.

<Experimental Example 8>

A granular powder for ceramic tiles prepared according to Experimental Example 4 was prepared.

For the hydrophobization surface treatment of the granular powder for ceramic tiles, a silica (SiO ₂ , 50 nm, 30%) solution (hydrophobized silica solution) surface-treated with Glycidoxypropyl trimethoxy silane (GPTMS) was prepared.

The hydrophobized silica solution was mixed with colloidal silica (50 nm, 20 g), ethanol (10 g), and distilled water (20 g) in a weight ratio of 2: 1: 2, followed by stirring for 10 minutes, and hydrochloric acid (HCl, 36.5%) After addition, the pH was adjusted to 2-3, followed by additional stirring at a temperature of 60°C for 30 minutes, and GPTMS (Glycidoxypropyl trimethoxy silane) was added to this solution at a concentration of 0.01M and stirred at a temperature of 60°C for 24 hours. was prepared.

The surface coating process of the granular powder for ceramic tiles using the hydrophobic silica solution was performed using a fluidized bed coater. The temperature inside the coating tank was raised to 60° C. and maintained, and the hydrophobic silica solution was sprayed at a rate of 2.3 ml/min while circulating the granular powder under ^{air flow @ 45 m 3 /h in consideration of the density of the granular powder.} The content of the hydrophobized silica solution was 8 parts by weight based on 100 parts by weight of the granular powder, and coating was performed. The total coating process time was carried out in 50 minutes.

<Experimental Example 9>

A granular powder for ceramic tiles prepared according to Experimental Example 4 was prepared.

For the hydrophobization surface treatment of the granular powder for ceramic tiles, a silica (SiO ₂ , 50 nm, 30%) solution (hydrophobized silica solution) surface-treated with Glycidoxypropyl trimethoxy silane (GPTMS) was prepared.

The hydrophobized silica solution was mixed with colloidal silica (50 nm, 20 g), ethanol (10 g), and distilled water (20 g) in a weight ratio of 2: 1: 2, followed by stirring for 10 minutes, and hydrochloric acid (HCl, 36.5%) After addition, the pH was adjusted to 2-3, followed by further stirring at a temperature of 60 °C for 30 minutes, and GPTMS (Glycidoxypropyl trimethoxy silane) was added to the solution at a concentration of 0.01M and stirred at a temperature of 60 °C for 24 hours. was prepared.

The surface coating process of the granular powder for ceramic tiles using the hydrophobic silica solution was performed using a fluidized bed coater. The temperature inside the coating tank was raised to 60° C. and maintained, and the hydrophobic silica solution was sprayed at a rate of 2.3 ml/min while circulating the granular powder under ^{air flow @ 45 m 3 /h in consideration of the density of the granular powder.} The content of the hydrophobized silica solution was 10 parts by weight based on 100 parts by weight of the granular powder, and coating was performed. The total coating process time was carried out in 50 minutes.

<Experimental Example 10>

A granular powder for ceramic tiles prepared according to Experimental Example 4 was prepared.

A saturated fatty acid coating solution was prepared for surface treatment of the granular powder for ceramic tiles. The saturated fatty acid coating solution was prepared by mixing palmitic acid with distilled water and stirring at room temperature for 30 minutes. The distilled water and palmitic acid were mixed in a weight ratio of 2:1.

The surface coating process of the granular powder for ceramic tiles using the saturated fatty acid coating solution was performed using a fluidized bed coater. The temperature inside the coating tank was raised to 60° C. and maintained, and the saturated fatty acid coating solution was sprayed at a rate of 2.3 ml/min while circulating the granular powder under ^{air flow @ 45 m 3 /h in consideration of the density of the granular powder.} The coating was carried out in an amount of 2 parts by weight based on 100 parts by weight of the granular powder in the content of the saturated fatty acid coating solution. The total coating process time was carried out in 50 minutes.

<Experimental Example 11>

A granular powder for ceramic tiles prepared according to Experimental Example 4 was prepared.

A saturated fatty acid coating solution was prepared for surface treatment of the granular powder for ceramic tiles. The saturated fatty acid coating solution was prepared by mixing palmitic acid with distilled water and stirring at room temperature for 30 minutes. The distilled water and palmitic acid were mixed in a weight ratio of 2:1.

The surface coating process of the granular powder for ceramic tiles using the saturated fatty acid coating solution was performed using a fluidized bed coater. The temperature inside the coating tank was raised to 60° C. and maintained, and the saturated fatty acid coating solution was sprayed at a rate of 2.3 ml/min while circulating the granular powder under ^{air flow @ 45 m 3 /h in consideration of the density of the granular powder.} Coating was carried out in an amount of the saturated fatty acid coating solution of 4 parts by weight based on 100 parts by weight of the granular powder. The total coating process time was carried out in 50 minutes.

<Experimental Example 12>

A granular powder for ceramic tiles prepared according to Experimental Example 4 was prepared.

A saturated fatty acid coating solution was prepared for surface treatment of the granular powder for ceramic tiles. The saturated fatty acid coating solution was prepared by mixing palmitic acid with distilled water and stirring at room temperature for 30 minutes. The distilled water and palmitic acid were mixed in a weight ratio of 2:1.

The surface coating process of the granular powder for ceramic tiles using the saturated fatty acid coating solution was performed using a fluidized bed coater. The temperature inside the coating tank was raised to 60° C. and maintained, and the saturated fatty acid coating solution was sprayed at a rate of 2.3 ml/min while circulating the granular powder under ^{air flow @ 45 m 3 /h in consideration of the density of the granular powder.} The coating was carried out in an amount of 6 parts by weight based on 100 parts by weight of the granular powder in the content of the saturated fatty acid coating solution. The total coating process time was carried out in 50 minutes.

1 and 2 are scanning electron microscope (SEM) photos showing the granular powder for porcelain tile prepared according to Experimental Example 4, and FIG. 3 is X of the granular powder for porcelain tile prepared according to Experimental Example 4. - It is a diagram showing an X-ray diffraction (XRD) pattern, FIG. 4 is a graph showing the particle size distribution of the granular powder for ceramic tiles prepared according to Experimental Example 4, and FIG. It is a photograph showing granular powder for ceramic tile.

6 is a photograph showing the granular powder for ceramic tiles coated with hydrophobic silica solution according to Experimental Example 7 and surface-coated with hydrophobic silica. 7 is a diagram illustrating a method for measuring the fluidity of granular powder for ceramic tiles.

Referring to FIG. 7 , the flowability evaluation of the granular powder for ceramic tiles was analyzed by measuring the angle of repose (ASTM D6393-08) of the granular powder. The angle (refer to 'φ' in FIG. 5 ) between the stage and the cone formed by the granular powder falling through a sieve installed 75 mm above the sample stage was measured.

The fluidity of the granular powder for ceramic tiles prepared according to Experimental Examples 1 to 5 was measured and shown in Table 1 below.

division Experimental Example 1 Experimental Example 2 Experimental Example 3 Experimental Example 4 Experimental Example 5 angle of repose (°) 30.2 29.1 27.6 27.3 29.8 Particle size distribution (mm) D ₁₀ : 88
D ₅₀ : 305
D ₉₀ : 910 D ₁₀ : 103
D ₅₀ : 321
D ₉₀ :915 D ₁₀ : 125
D ₅₀ : 364
D ₉₀ :927 D ₁₀ :152
D ₅₀ : 387
D ₉₀ : 920 D ₁₀ : 141
D ₅₀ : 344
D ₉₀ : 905

The fluidity of the granular powder is affected by the particle size distribution, and when PVP was added to control the particle size distribution during the preparation of the granular powder, the fluidity was improved.

The granular powder for ceramic tiles prepared according to Experimental Example 4, the granular powder for ceramic tiles coated with the hydrophobic silica solution according to Experimental Examples 6 to 9, and coated with a saturated fatty acid coating solution according to Experimental Examples 10 to 12 The angle of repose, tap density, compressibility, and flowability index of the treated granular powder for ceramic tiles were measured and shown in Table 2 below.

Angle of repose (°) Tap density (g/㎤) Compressibility (%) Flowability index Experimental Example 4 27.32 1.39 16.20 84.21 Experimental Example 6 25.21 1.52 14.71 86.22 Experimental Example 7 22.60 1.61 12.92 89.87 Experimental Example 8 26.82 1.43 15.84 85.01 Experimental Example 9 29.15 1.28 17.86 82.99 Experimental Example 10 22.85 1.60 13.83 89.05 Experimental Example 11 20.05 1.72 12.05 91.44 Experimental Example 12 23.42 1.66 13.06 88.23

Referring to Table 2, the granular powder coated with hydrophobic silica and surface-coated with hydrophobic silica solution has improved fluidity compared to the granular powder prepared according to Experimental Example 4. The best fluidity was observed when the content of the hydrophobized silica solution was 5 parts by weight (Experimental Example 7) and 8 parts by weight (Experimental Example 8) relative to 100 parts by weight of the granular powder.

The granular powder surface-treated with the saturated fatty acid coating solution had improved fluidity compared to the granular powder prepared according to Experimental Example 4. The best fluidity was observed when the content of the saturated fatty acid coating solution was 4 parts by weight (Experimental Example 11) compared to 100 parts by weight of the granular powder.

The granular powder for ceramic tiles prepared according to Experimental Example 4, the granular powder for ceramic tiles coated with a hydrophobic silica solution according to Experimental Example 7, and the granular powder for ceramic tiles coated with a saturated fatty acid coating solution according to Experimental Example 11 were prepared. The bending strength of the molded body (specimen size 30 mm × 60 mm) produced by compression molding at a pressure of 6 tons in the form of a ceramic tile using the Bending strength was measured and shown in Table 3 below.

number of experiments When using the granular powder for ceramic tiles prepared according to Experimental Example 4 When using the granular powder for ceramic tiles coated with the hydrophobic silica solution according to Experimental Example 7 When using the granular powder for ceramic tiles coated with a saturated fatty acid coating solution according to Experimental Example 11 molded body
bending strength
(N/cm) Primary 4.80 4.78 4.91 Secondary 4.72 4.88 4.82 tertiary 4.84 4.90 4.80 average 4.79 4.85 4.84 sintered compact
bending strength
(N/cm) Primary 58.60 63.22 65.05 Secondary 61.05 62.84 64.08 tertiary 58.84 63.04 67.25 average 59.50 63.03 65.46

The molded body and the sintered body manufactured using the granular powder for ceramic tiles that were coated with the hydrophobic silica solution according to Experimental Example 7 had higher bending strength than the molded body and the sintered body manufactured using the granular powder for ceramic tiles prepared according to Experimental Example 4. appeared to be excellent.

In addition, the molded body and the sintered body manufactured using the granular powder for ceramic tiles coated with the saturated fatty acid coating solution according to Experimental Example 11 were bent compared to the molded body and the sintered body manufactured using the granular powder for ceramic tiles prepared according to Experimental Example 4 The strength was found to be excellent.

As mentioned above, although preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various modifications are possible by those skilled in the art.

Claims (10)

preparing a granular powder for ceramic tiles;
preparing a saturated fatty acid coating solution; and
coating the surface of the granular powder for ceramic tiles with the saturated fatty acid coating solution to obtain a granular powder for ceramic tiles surface-treated with the saturated fatty acid coating solution;
The saturated fatty acid coating solution is palmitic acid, butyric acid (C ₄ H ₈ O ₂ , Butyric acid), stearic acid (C ₁₈ H36O ₂ , Stearic acid), valeric acid (C ₅ H ₁₀ O ₂ , Valeric acid) ), caproic acid (C ₆ H ₁₂ O ₂ , Caproic acid), caprylic acid (C ₈ H ₁₆ O ₂ , Carrylic acid), pelargonic acid (C ₉ H ₁₈ O ₂ , Pelargonic acid), lauric acid ( C ₁₂ H ₂₄ O ₂ , Lauric acid), _{tridecylic acid (C 13} H ₂₆ O ₂ , Tridecylic acid), myristic acid (C ₁₄ H ₂₈ O ₂ , Myristic acid), margaric acid (C ₁₇ H ₃₄ O ₂ , Margaric acid), arachidic acid (C ₆ H ₁₂ O ₂ , Arachidic acid), behenic acid (C ₁₁ H ₂₂ O, Behenic acid), lignoceric acid (C ₁₂ H ₂₄ O, Lignoceric acid), vertical Tonic acid (C ₂₆ H ₅₂ O ₂ , Cerotic acid), montanic acid (C ₂₈ H ₅₆ O ₂ , Montanic acid) and hentriacontylic acid (C ₃₁ H ₆₂ O ₂ , Hentriacontylic acid) At least one selected from the group consisting of containing saturated fatty acids,
The step of preparing the granular powder for porcelain tile,
As starting materials, 10 to 15% by weight of limestone powder, 20 to 25% by weight of clay powder, 35 to 45% by weight of porcelain powder, 10 to 15% by weight of pyrophyllite powder and 8 to 13% of clay powder are prepared and mixed to form a slurry. step; and
Comprising the step of spray drying the mixture in a slurry state to obtain a granular powder for ceramic tiles,
In the step of making the slurry, 0.1 to 2 parts by weight of PVP (Polyvinylpyrrolidone) is further mixed with respect to 100 parts by weight of the starting material.
delete delete preparing a granular powder for ceramic tiles;
preparing a saturated fatty acid coating solution; and
coating the surface of the granular powder for ceramic tiles with the saturated fatty acid coating solution to obtain a granular powder for ceramic tiles surface-treated with the saturated fatty acid coating solution;
The saturated fatty acid coating solution is palmitic acid, butyric acid (C ₄ H ₈ O ₂ , Butyric acid), stearic acid (C ₁₈ H36O ₂ , Stearic acid), valeric acid (C ₅ H ₁₀ O ₂ , Valeric acid) ), caproic acid (C ₆ H ₁₂ O ₂ , Caproic acid), caprylic acid (C ₈ H ₁₆ O ₂ , Carrylic acid), pelargonic acid (C ₉ H ₁₈ O ₂ , Pelargonic acid), lauric acid ( C ₁₂ H ₂₄ O ₂ , Lauric acid), _{tridecylic acid (C 13} H ₂₆ O ₂ , Tridecylic acid), myristic acid (C ₁₄ H ₂₈ O ₂ , Myristic acid), margaric acid (C ₁₇ H ₃₄ O ₂ , Margaric acid), arachidic acid (C ₆ H ₁₂ O ₂ , Arachidic acid), behenic acid (C ₁₁ H ₂₂ O, Behenic acid), lignoceric acid (C ₁₂ H ₂₄ O, Lignoceric acid), vertical Tonic acid (C ₂₆ H ₅₂ O ₂ , Cerotic acid), montanic acid (C ₂₈ H ₅₆ O ₂ , Montanic acid) and hentriacontylic acid (C ₃₁ H ₆₂ O ₂ , Hentriacontylic acid) At least one selected from the group consisting of containing saturated fatty acids,
The step of preparing the granular powder for ceramic tiles,
As starting materials, 10 to 15% by weight of limestone powder, 20 to 25% by weight of clay powder, 35 to 45% by weight of porcelain powder, 10 to 15% by weight of pyrophyllite powder, and 8 to 13% of clay powder are prepared and mixed to form a slurry. step; and
Comprising the step of spray drying the mixture in a slurry state to obtain a granular powder for ceramic tiles,
In the step of making the slurry, 0.1 to 2 parts by weight of PVA (polyvinyl alcohol) is further mixed with respect to 100 parts by weight of the starting material.
preparing a granular powder for ceramic tiles;
preparing a saturated fatty acid coating solution; and
coating the surface of the granular powder for ceramic tiles with the saturated fatty acid coating solution to obtain a granular powder for ceramic tiles surface-treated with the saturated fatty acid coating solution;
The saturated fatty acid coating solution is palmitic acid, butyric acid (C ₄ H ₈ O ₂ , Butyric acid), stearic acid (C ₁₈ H36O ₂ , Stearic acid), valeric acid (C ₅ H ₁₀ O ₂ , Valeric acid) ), caproic acid (C ₆ H ₁₂ O ₂ , Caproic acid), caprylic acid (C ₈ H ₁₆ O ₂ , Carrylic acid), pelargonic acid (C ₉ H ₁₈ O ₂ , Pelargonic acid), lauric acid ( C ₁₂ H ₂₄ O ₂ , Lauric acid), _{tridecylic acid (C 13} H ₂₆ O ₂ , Tridecylic acid), myristic acid (C ₁₄ H ₂₈ O ₂ , Myristic acid), margaric acid (C ₁₇ H ₃₄ O ₂ , Margaric acid), arachidic acid (C ₆ H ₁₂ O ₂ , Arachidic acid), behenic acid (C ₁₁ H ₂₂ O, Behenic acid), lignoceric acid (C ₁₂ H ₂₄ O, Lignoceric acid), vertical Tonic acid (C ₂₆ H ₅₂ O ₂ , Cerotic acid), montanic acid (C ₂₈ H ₅₆ O ₂ , Montanic acid) and hentriacontylic acid (C ₃₁ H ₆₂ O ₂ , Hentriacontylic acid) At least one selected from the group consisting of containing saturated fatty acids,
The step of preparing the granular powder for porcelain tile,
As starting materials, 10 to 15% by weight of limestone powder, 20 to 25% by weight of clay powder, 35 to 45% by weight of porcelain powder, 10 to 15% by weight of pyrophyllite powder and 8 to 13% of clay powder are prepared and mixed to form a slurry. step; and
Comprising the step of spray drying the mixture in a slurry state to obtain a granular powder for ceramic tiles,
In the step of making the slurry, 0.1 to 2 parts by weight of sodium silicate is further mixed with respect to 100 parts by weight of the starting material.
preparing a granular powder for ceramic tiles;
preparing a saturated fatty acid coating solution; and
coating the surface of the granular powder for ceramic tiles with the saturated fatty acid coating solution to obtain a granular powder for ceramic tiles surface-treated with the saturated fatty acid coating solution;
The saturated fatty acid coating solution is palmitic acid, butyric acid (C ₄ H ₈ O ₂ , Butyric acid), stearic acid (C ₁₈ H36O ₂ , Stearic acid), valeric acid (C ₅ H ₁₀ O ₂ , Valeric acid) ), caproic acid (C ₆ H ₁₂ O ₂ , Caproic acid), caprylic acid (C ₈ H ₁₆ O ₂ , Carrylic acid), pelargonic acid (C ₉ H ₁₈ O ₂ , Pelargonic acid), lauric acid ( C ₁₂ H ₂₄ O ₂ , Lauric acid), _{tridecylic acid (C 13} H ₂₆ O ₂ , Tridecylic acid), myristic acid (C ₁₄ H ₂₈ O ₂ , Myristic acid), margaric acid (C ₁₇ H ₃₄ O ₂ , Margaric acid), arachidic acid (C ₆ H ₁₂ O ₂ , Arachidic acid), behenic acid (C ₁₁ H ₂₂ O, Behenic acid), lignoceric acid (C ₁₂ H ₂₄ O, Lignoceric acid), vertical Tonic acid (C ₂₆ H ₅₂ O ₂ , Cerotic acid), montanic acid (C ₂₈ H ₅₆ O ₂ , Montanic acid) and hentriacontylic acid (C ₃₁ H ₆₂ O ₂ , Hentriacontylic acid) At least one selected from the group consisting of containing saturated fatty acids,
The step of preparing the granular powder for porcelain tile,
As starting materials, 10 to 15% by weight of limestone powder, 20 to 25% by weight of clay powder, 35 to 45% by weight of porcelain powder, 10 to 15% by weight of pyrophyllite powder and 8 to 13% of clay powder are prepared and mixed to form a slurry. step; and
Comprising the step of spray drying the mixture in a slurry state to obtain a granular powder for ceramic tiles,
In the step of making the slurry, 0.1 to 2 parts by weight of gelatin is further mixed with respect to 100 parts by weight of the starting material.
preparing a granular powder for ceramic tiles;
preparing a saturated fatty acid coating solution; and
coating the surface of the granular powder for ceramic tiles with the saturated fatty acid coating solution to obtain a granular powder for ceramic tiles surface-treated with the saturated fatty acid coating solution;
The saturated fatty acid coating solution is palmitic acid, butyric acid (C ₄ H ₈ O ₂ , Butyric acid), stearic acid (C ₁₈ H36O ₂ , Stearic acid), valeric acid (C ₅ H ₁₀ O ₂ , Valeric acid) ), caproic acid (C ₆ H ₁₂ O ₂ , Caproic acid), caprylic acid (C ₈ H ₁₆ O ₂ , Carrylic acid), pelargonic acid (C ₉ H ₁₈ O ₂ , Pelargonic acid), lauric acid ( C ₁₂ H ₂₄ O ₂ , Lauric acid), _{tridecylic acid (C 13} H ₂₆ O ₂ , Tridecylic acid), myristic acid (C ₁₄ H ₂₈ O ₂ , Myristic acid), margaric acid (C ₁₇ H ₃₄ O ₂ , Margaric acid), arachidic acid (C ₆ H ₁₂ O ₂ , Arachidic acid), behenic acid (C ₁₁ H ₂₂ O, Behenic acid), lignoceric acid (C ₁₂ H ₂₄ O, Lignoceric acid), vertical Tonic acid (C ₂₆ H ₅₂ O ₂ , Cerotic acid), montanic acid (C ₂₈ H ₅₆ O ₂ , Montanic acid) and hentriacontylic acid (C ₃₁ H ₆₂ O ₂ , Hentriacontylic acid) At least one selected from the group consisting of containing saturated fatty acids,
The step of preparing the granular powder for porcelain tile,
As starting materials, 10 to 15% by weight of limestone powder, 20 to 25% by weight of clay powder, 35 to 45% by weight of porcelain powder, 10 to 15% by weight of pyrophyllite powder and 8 to 13% of clay powder are prepared and mixed to form a slurry. step; and
Comprising the step of spray drying the mixture in a slurry state to obtain a granular powder for ceramic tiles,
In the step of making the slurry, 0.1 to 2 parts by weight of sugar water is further mixed with respect to 100 parts by weight of the starting material.
The method of claim 1, wherein the saturated fatty acid coating solution is prepared by mixing saturated fatty acid with a solvent, and the solvent contains water (H ₂ O).
The method of claim 1, wherein the coating is carried out so that the content of the saturated fatty acid coating solution is 1 to 10 parts by weight based on 100 parts by weight of the granular powder for ceramic tiles.
Claims 1, 4, 5, 6 or 7, comprising the steps of molding the high-fluidity granular powder for porcelain tile prepared by the method according to any one of claims into a desired shape and drying;
forming a ceramic tile base layer by first firing the dried product;
forming a first glaze layer on the ceramic tile base layer;
forming a second glaze layer on the first glaze layer; and
A method of manufacturing a ceramic tile comprising the step of secondary firing the resultant product on which the secondary glaze layer is formed.

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