Antique black tile and preparation method thereof

Abstract

The invention discloses an antique black tile and a preparation method thereof, and belongs to the technical field of antique black tiles. The antique black tile is prepared from the following raw materials: vanadium-titanium tailings, clay, red soil, carclazyte, talcum powder, white carbon black and a reinforcing agent. The vanadium-titanium tailings are ground and then mixed with the clay, the red soil, the carclazyte, the talcum powder and the white carbon black to be prepared into the tile, the vanadium-titanium tailings contain a certain amount of metal elements such as iron, titanium and vanadium, the metal elements can be subjected to oxidation-reduction reaction in the high-temperature firing process, especially the iron element can easily form black oxide at high temperature, and the ceramic tile is not prone to cracking. According to the present invention, the prepared archaized black tile has the following characteristics that the tile can be easily blackened such as ferroferric oxide or ferric oxide, such that the color uniformity and the stability of the archaized black tile can be effectively improved, the fired archaized black tile can present the pure and deep black, the color of the final product can be improved, and the strict requirements of the archaized building on the appearance quality of the archaized black tile can be met.

Description

Technical Field

[0001] The present invention relates to the technical field of antique black tiles, and specifically relates to an antique black tile and a preparation method thereof. Background Art

[0002] With the increasing attention and inheritance of traditional culture in society, antique buildings are emerging in various places. As an indispensable important element of traditional buildings, the market demand for antique black tiles is growing day by day. However, the firing of traditional antique black tiles requires a specific kiln environment and complex operation processes. During the firing process, the control of temperature, humidity, and firing time is extremely strict. A slight deviation may cause problems such as deformation, cracking, and unsatisfactory color of the antique black tiles, seriously affecting the overall aesthetic effect of antique buildings. Due to the color problem of antique black tiles, secondary coloring treatment has to be carried out, which not only increases the construction cost but also may have a negative impact on the durability of antique black tiles; With the continuous growth of mineral resource development in China, the industrial development has made unprecedented progress. However, this has been accompanied by the generation of a large amount of industrial solid waste. The development of mineral resources generates a large amount of vanadium-titanium tailings. The stacking of vanadium-titanium tailings not only occupies precious land resources but also poses a great threat to the environment. Therefore, an antique black tile and a preparation method thereof are proposed. Summary of the Invention

[0003] Aiming at the defects of the prior art, the purpose of the present invention is to provide an antique black tile and a preparation method thereof to solve the problems raised in the above background art.

[0004] The present invention solves the technical problems by adopting the following technical solutions: The present invention provides an antique black tile, comprising the following raw materials: Vanadium-titanium tailings, clay, red soil, white soil, talcum powder, white carbon black, reinforcing agent; Its specific formula comprises the following raw materials: 15-25 parts of vanadium-titanium tailings, 8-12 parts of clay, 30-40 parts of red soil, 17-22 parts of white soil, 3-6 parts of talcum powder, 8-12 parts of white carbon black, and 10-15 parts of reinforcing agent.

[0005] Preferably, the reinforcing agent comprises the following components in parts by mass: 3-5 parts of nano-carbon fiber powder, 2-4 parts of lanthanum oxide, 1-2 parts of titanium oxide, and 10-12 parts of epoxy resin.

[0006] Preferably, the antique black tile comprises the following raw materials: 20 parts of vanadium-titanium tailings, 10 parts of clay, 35 parts of red soil, 20 parts of white soil, 5 parts of talcum powder, 10 parts of white carbon black, and 10 parts of reinforcing agent.

[0007] Preferably, the vanadium-titanium tailings are waste generated during the beneficiation process of vanadium-titanium magnetite, including minerals such as ilmenite, magnetite, feldspar, diopside, etc.

[0008] The present invention also provides a method for preparing antique black tiles, comprising the following steps: Step 1: Calcine the vanadium-titanium tailings and then crush them into particles with a particle size of 1-3 mm, and then ball mill to obtain pretreated vanadium-titanium tailings powder. Then, sieve the vanadium-titanium tailings powder to obtain vanadium-titanium tailings coarse powder and vanadium-titanium tailings fine powder; According to the said mass parts, mix nano-carbon fiber powder, lanthanum oxide, titanium oxide and epoxy resin to obtain a reinforcing agent; Step 2: Mix the vanadium-titanium tailings coarse powder with clay, red clay, white clay, talc powder, white carbon black and the reinforcing agent, add water and stir into a slurry. Then, press the mixed slurry raw materials into tile blanks. Next, spray the vanadium-titanium tailings fine powder on the surface of the tile blanks and perform secondary pressing to form. Finally, place the formed tile blanks in a shed and air-dry them naturally to ensure that the tile blanks do not deform during handling; Step 3: Put the air-dried tile blanks into a kiln and raise the temperature in stages for sintering. After stopping the fire, block the kiln mouth and chimney with bricks and slurry, and seal the tile kiln for eight to ten days. In the case of isolating air oxidation, the tile blanks will slowly turn black to form antique black tiles; Step 4: Open the kiln door to dissipate heat and cool for two to three days. Until the kiln is fully cooled, take out the antique black tiles from the kiln. After taking out the kiln, conduct quality inspection on the antique black tiles to ensure that the color and hardness meet the standards.

[0009] Preferably, the calcination temperature of the vanadium-titanium tailings is 600-700 °C, and the calcination time is 5-6 h.

[0010] Preferably, an excitation rotation stirring ball mill is used for ball milling the vanadium-titanium tailings. The ball milling time is 30-90 min, the material-ball ratio is 1:2, and the ball-milled vanadium-titanium tailings powder is dried at a temperature of 70-80 °C.

[0011] Preferably, the stirred slurry is trampled repeatedly for 1-2 days until the slurry becomes viscous and elastic. The trampled slurry is cut into pieces with a special tool for subsequent use.

[0012] Preferably, the pressure for the first pressing of the tile blanks is 40-50 Mpa, the pressure for the second pressing of the tile blanks is 70-80 Mpa, and the amount of vanadium-titanium tailings fine powder sprayed on the surface of the tile blanks is 0.2-0.3 g / cm 2 .

[0013] Preferably, the stepwise temperature increase includes three stages. In the first stage, the heating rate is controlled at 5 - 8 °C / min before reaching 700 °C. In the second stage, the heating rate is controlled at 2 - 3 °C / min from 700 °C to 1100 °C, and the heating rate is controlled at 0.8 - 1.5 °C / min from 1100 °C to 1350 °C, and it is kept at the highest temperature for 30 - 45 h.

[0014] Preferably, after the antique black tiles are taken out of the kiln, they are slightly polished with a pneumatic mill and manually polished with sandpaper to enhance the antique effect.

[0015] The antique black tiles prepared by the present invention and its preparation method mix ground vanadium-titanium tailings with clay, red clay, and white clay to make tiles, spray fine vanadium-titanium tailings powder on the surface of the tile blanks for secondary pressing and forming, and optimize the control of the kiln environment by stepwise increasing the temperature during the firing process. It can significantly reduce the firing difficulty, improve the yield of the antique black tiles, enhance the mechanical properties, fire resistance, and waterproof properties of the antique black tiles, reduce the possibility of deformation and cracking, and thus effectively apply vanadium-titanium tailings to the production of antique black tiles, improving both the product performance and achieving comprehensive utilization of resources.

[0016] Compared with the prior art, the present invention has the following beneficial effects: In the present invention, tiles are made by mixing ground vanadium-titanium tailings with clay, red clay, and white clay. Since vanadium-titanium tailings contain certain amounts of metal elements such as iron, titanium, and vanadium, these elements will undergo redox reactions during the high-temperature firing process. Especially iron elements are prone to form black oxides such as magnetite or iron oxide at high temperatures, making it easier for the tiles to turn black, which can effectively improve the color uniformity and stability of the antique black tiles, making the fired antique black tiles show a pure and deep black color, enhancing the color of the final product, and meeting the strict requirements of the appearance quality of antique black tiles for antique buildings. Detailed implementation mode

[0017] The following combines specific embodiments to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention. Embodiment 1

[0018] An antique black tile, including the following raw materials by mass fraction: 15 parts of vanadium-titanium tailings, 8 parts of clay, 30 parts of red clay, 17 parts of white clay, 3 parts of talcum powder, 8 parts of white carbon black, and 10 parts of reinforcing agent.

[0019] The enhancer includes the following components by mass fraction: 3 parts of nano-carbon fiber powder, 2 parts of lanthanum oxide, 1 part of titanium oxide, and 10 parts of epoxy resin.

[0020] The vanadium-titanium tailings are waste generated during the beneficiation process of vanadium-titanium magnetite.

[0021] A method for preparing antique black tiles, which is used to prepare antique black tiles, includes the following steps: Step 1: According to the above mass fraction, calcine the vanadium-titanium tailings and then crush them into particles with a particle size of 1 mm, then ball-mill to obtain vanadium-titanium tailings powder. Next, sieve the obtained vanadium-titanium tailings powder to obtain vanadium-titanium tailings coarse powder and vanadium-titanium tailings fine powder. The calcination temperature of the vanadium-titanium tailings is 600 °C and the time is 5 h; the ball-milling time is 30 min, the material-ball ratio is 1:2, the rotation speed of the ball-mill is 400 r / min, and the ball-milled vanadium-titanium tailings powder is dried at a temperature of 70 °C. Step 2: Mix the vanadium-titanium tailings coarse powder with clay, red clay, white clay, talc powder, white carbon black and the enhancer, add water and stir into a slurry. Then, press the mixed slurry raw materials into a tile blank for the first time. Next, spray the vanadium-titanium tailings fine powder on the surface of the tile blank and perform secondary pressing to form. Finally, air-dry the formed tile blank naturally to ensure that the tile blank does not deform during handling; among them, the stirred slurry is trampled repeatedly for 1 day until the slurry becomes sticky and elastic, and the trampled slurry is cut into pieces; the pressure for the first pressing of the tile blank is 40 Mpa, the pressure for the second pressing of the tile blank is 70 Mpa, and the amount of vanadium-titanium tailings fine powder sprayed on the surface of the tile blank is 0.2 g / cm 2 ; Step 3: Put the air-dried tile blank into the kiln and raise the temperature in stages for sintering. After stopping the fire, block the kiln mouth and chimney with bricks and slurry, and seal the tile kiln for eight to ten days. In the case of isolating air oxidation, the tile blank will slowly turn black to form antique black tiles; Among them, raising the temperature in stages includes three stages. First, raise the temperature to 700 °C at a heating rate of 5 °C / min, then raise the temperature to 700 °C at a heating rate of 2 °C / min. Finally, raise the temperature to 1100 °C at a heating rate of 0.8 °C / min and hold for 30 h at the highest temperature; Step 4: Open the kiln door to dissipate heat and cool for two to three days. Until the kiln is fully cooled, take out the antique black tiles from the kiln. After taking out the kiln, conduct quality inspection on the antique black tiles to ensure that the color and hardness meet the standards. And, after taking out the kiln, the antique black tiles are slightly polished with a pneumatic grinder and hand-polished with sandpaper to improve the antique effect. Example 2

[0022] An antique black tile includes the following raw materials by mass fraction: 25 parts of vanadium-titanium tailings, 12 parts of clay, 40 parts of red clay, 22 parts of white clay, 6 parts of talc powder, 12 parts of white carbon black, and 13 parts of enhancer.

[0023] The reinforcing agent includes the following components by mass fraction: 5 parts of nano-carbon fiber powder, 4 parts of lanthanum oxide, 2 parts of titanium oxide, and 12 parts of epoxy resin.

[0024] The vanadium-titanium tailings are waste generated during the beneficiation process of vanadium-titanium magnetite.

[0025] A method for preparing antique black tiles, which is used to prepare antique black tiles, includes the following steps: Step 1: According to the said mass fraction, calcine the vanadium-titanium tailings and then crush them into particles with a particle size of 3 mm, and then ball-mill to obtain vanadium-titanium tailings powder. Then, sieve the obtained vanadium-titanium tailings powder to obtain vanadium-titanium tailings coarse powder and vanadium-titanium tailings fine powder. The calcination temperature of the vanadium-titanium tailings is 700 °C and the time is 6 h; the ball-milling time is 90 min, the material-to-ball ratio is 1:2, the rotation speed of the ball-mill is 450 r / min, and the ball-milled vanadium-titanium tailings powder is dried at a temperature of 80 °C. Step 2: Mix the vanadium-titanium tailings coarse powder with clay, red clay, white clay, talc powder, white carbon black and the reinforcing agent, add water and stir into a slurry. Then, press the mixed slurry raw materials into a tile blank for the first time, and then spray the vanadium-titanium tailings fine powder on the surface of the tile blank and perform secondary pressing and forming. Finally, air-dry the formed tile blank naturally to ensure that the tile blank does not deform during handling; among them, the stirred slurry is trampled repeatedly for 2 days until the slurry becomes viscous and elastic, and the trampled slurry is cut into pieces; the pressure for the first pressing of the tile blank is 50 Mpa, the pressure for the second pressing of the tile blank is 80 Mpa, and the amount of vanadium-titanium tailings fine powder sprayed on the surface of the tile blank is 0.3 g / cm 2 ; Step 3: Put the air-dried tile blank into the kiln and raise the temperature in stages for sintering. After stopping the fire, block the kiln mouth and chimney with bricks and slurry, and seal the tile kiln for eight to ten days. In the case of isolating air oxidation, the tile blank will slowly turn black to form antique black tiles; Among them, raising the temperature in stages includes three stages. First, raise the temperature to 700 °C at a heating rate of 8 °C / min, then raise the temperature to 1100 °C at a heating rate of 3 °C / min, and finally, raise the temperature to 1350 °C at a heating rate of 1.5 °C / min and hold at the highest temperature for 45 h; Step 4: Open the kiln door to dissipate heat and cool for two to three days until the kiln is fully cooled, then take out the antique black tiles from the kiln. After taking out the kiln, conduct quality inspection on the antique black tiles to ensure that the color and hardness meet the standards. Moreover, after taking out the kiln, the antique black tiles are slightly polished with a pneumatic grinder and hand-polished with sandpaper to improve the antique effect. Example 3

[0026] An antique-style black tile, comprising the following raw materials by mass parts: 20 parts of vanadium-titanium tailings, 10 parts of clay, 35 parts of red soil, 20 parts of white soil, 5 parts of talcum powder, 10 parts of white carbon black, and 15 parts of reinforcing agent.

[0027] The reinforcing agent comprises the following components by mass parts: 3 parts of nano-carbon fiber powder, 2 parts of lanthanum oxide, 1 part of titanium oxide, and 11 parts of epoxy resin.

[0028] The vanadium-titanium tailings are waste generated during the beneficiation process of vanadium-titanium magnetite.

[0029] A preparation method of an antique-style black tile for preparing the antique-style black tile, comprising the following steps: Step 1: According to the said mass parts, calcine the vanadium-titanium tailings and then crush them into particles with a particle size of 2 mm, then ball-mill to obtain vanadium-titanium tailings powder, and then screen the obtained vanadium-titanium tailings powder to obtain vanadium-titanium tailings coarse powder and vanadium-titanium tailings fine powder. The calcination temperature of the vanadium-titanium tailings is 650 °C and the time is 5 h; the ball-milling time is 60 min, the material-ball ratio is 1:2, the rotation speed of the ball-mill is 450 r / min, and the ball-milled vanadium-titanium tailings powder is dried at a temperature of 75 °C; Step 2: Mix the vanadium-titanium tailings coarse powder with clay, red soil, white soil, talcum powder, white carbon black, and the reinforcing agent, add water and stir into a slurry, then press the mixed slurry raw materials into a tile blank for the first time, then spray the vanadium-titanium tailings fine powder on the surface of the tile blank and perform secondary pressing and forming, and finally air-dry the formed tile blank to ensure that the tile blank does not deform during handling; among them, the stirred slurry is repeatedly trampled for 2 days until the slurry becomes sticky and elastic, and the trampled slurry is cut into pieces; the pressure for the first pressing of the tile blank is 45 Mpa, the pressure for the second pressing of the tile blank is 75 Mpa, and the amount of vanadium-titanium tailings fine powder sprayed on the surface of the tile blank is 0.2 g / cm 2 ; Step 3: Put the air-dried tile blank into the kiln and raise the temperature in stages for sintering. After stopping the fire, block the kiln mouth and chimney with bricks and slurry, seal the tile kiln for eight to ten days. In the case of isolating air oxidation, the tile blank will slowly turn black to form an antique-style black tile; Among them, raising the temperature in stages includes three stages. First, raise the temperature to 700 °C at a heating rate of 6 °C / min, then raise the temperature to 900 °C at a heating rate of 3 °C / min, and finally, raise the temperature to 1280 °C at a heating rate of 1.3 °C / min and hold at the highest temperature for 40 h; Step 4: Open the kiln door for heat dissipation and cool for two to three days until the kiln is fully cooled, then take out the antique-style black tile from the kiln. After taking out the kiln, conduct quality inspection on the antique-style black tile to ensure that the color and hardness meet the standards. And, after taking out the kiln, the antique-style black tile is slightly polished with a pneumatic grinder and hand-polished with sandpaper to improve the antique effect. Comparative Example 1

[0030] Differently from Example 3, antique black tiles will be prepared using ordinary materials. Comparative Example 2

[0031] Differently from Example 3, fine vanadium-titanium tailings powder will not be sprayed on the surface of the tile blank for secondary forming.

[0032] Perform performance tests on the products of Examples 1 to 3 and Comparative Examples 1 to 2; Produce 25 antique black tile samples, with 5 samples in each group, divided into 5 groups in total. Each group corresponds to Examples 1 to 3 and Comparative Examples 1 to 2 and is numbered A / B / C / D / E. Finally, test the antique black tile samples of groups A / B / C / D / E respectively, and the test results are shown in the following table.

[0033]

[0034] It can be seen from Examples 1 to 3 that; for the antique black tiles made by the present invention and its preparation method, by grinding vanadium-titanium tailings and mixing them with clay, red clay, and white clay to make tiles, and spraying fine vanadium-titanium tailings powder on the surface of the tile blank for secondary pressing and forming, and optimizing the control of the kiln environment by raising the temperature in stages during the firing process, the firing difficulty can be significantly reduced, the yield of black tiles can be increased, the mechanical properties and fire and water resistance of the antique black tiles can be enhanced, and the possibility of deformation and cracking can be reduced. Thus, vanadium-titanium tailings can be effectively applied to the production of antique black tiles, which not only improves the product performance but also realizes the comprehensive utilization of resources.

[0035] It can be seen from Example 3 and Comparative Example 2 that metal elements in vanadium-titanium tailings will undergo redox reactions during high-temperature firing. Especially iron elements are prone to form black oxides at high temperatures, which makes the tiles easier to turn black, and the fired black tiles present a pure and deep black color, improving the color of the final product.

[0036] The innovation points of the present invention are as follows: In the present invention, vanadium-titanium tailings are ground and mixed with clay, red clay, and white clay to make tiles. Since vanadium-titanium tailings contain a certain amount of metal elements such as iron, titanium, and vanadium, these elements will undergo redox reactions during high-temperature firing. Especially iron elements are prone to form black oxides such as magnetite or hematite at high temperatures, which makes the tiles easier to turn black, can effectively improve the color uniformity and stability of black tiles, and the fired black tiles present a pure and deep black color, improving the color of the final product and meeting the strict requirements of antique buildings for the appearance quality of black tiles. At the same time.

[0037] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above-described exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, in any regard, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Accordingly, all changes that fall within the meaning and scope of the equivalent elements of the claims are intended to be embraced within the present invention.

[0038] In addition, it should be understood that although this specification is described in terms of embodiments, not every embodiment only contains an independent technical solution. This narrative manner of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. An antique-style black tile, characterized in that, It includes the following raw materials by mass parts: 15 - 25 parts of vanadium-titanium tailings, 8 - 12 parts of clay, 30 - 40 parts of laterite, 17 - 22 parts of kaolin, 3 - 6 parts of talcum powder, 8 - 12 parts of white carbon black, and 10 - 15 parts of reinforcing agent; The reinforcing agent includes the following components by mass parts: 3 - 5 parts of nano-carbon fiber powder, 2 - 4 parts of lanthanum oxide, 1 - 2 parts of titanium oxide, and 10 - 12 parts of epoxy resin.

2. An antique black tile according to claim 1, characterized in that, It includes the following raw materials: 20 parts of vanadium-titanium tailings, 10 parts of clay, 35 parts of laterite, 20 parts of kaolin, 5 parts of talcum powder, 10 parts of white carbon black, and 10 parts of reinforcing agent; The reinforcing agent includes the following components by mass parts: 3 parts of nano-carbon fiber powder, 2 parts of lanthanum oxide, 1 part of titanium oxide, and 10 parts of epoxy resin.

3. An antique black tile according to claim 1, characterized in that, The vanadium-titanium tailings are waste produced during the beneficiation process of vanadium-titanium magnetite.

4. A method for preparing antique black tiles, which is used to prepare the antique black tiles described in any one of claims 1 to 3, and is characterized in that, It includes the following steps: Step 1: According to the said mass parts, calcine the vanadium-titanium tailings and then crush them into particles with a particle size of 1 - 3 mm, then ball mill to obtain vanadium-titanium tailings powder, and then sieve the obtained vanadium-titanium tailings powder to obtain vanadium-titanium tailings coarse powder and vanadium-titanium tailings fine powder; According to the said mass parts, mix nano-carbon fiber powder, lanthanum oxide, titanium oxide and epoxy resin to obtain a reinforcing agent; Step 2: Mix the vanadium-titanium tailings coarse powder with clay, laterite, kaolin, talcum powder, white carbon black and the reinforcing agent, add water and stir into a slurry, then press the mixed slurry raw materials into tile blanks for the first time, then spray vanadium-titanium tailings fine powder on the surface of the tile blanks and press them into shape for the second time, and finally air-dry the formed tile blanks naturally to ensure that the tile blanks do not deform during handling; Step 3: Put the air-dried tile blanks into the kiln and raise the temperature in stages for sintering. After stopping the fire, block the kiln mouth and chimney with bricks and slurry, seal the tile kiln for eight to ten days. In the case of isolating air oxidation, the tile blanks will slowly turn black to form antique black tiles; Step 4: Open the kiln door to dissipate heat and cool for two to three days until the kiln is fully cooled, then take out the antique black tiles from the kiln, and conduct quality inspection on the taken-out antique black tiles to ensure that the color and hardness meet the standards.

5. The preparation method of an antique black tile according to claim 4, characterized in that The calcination temperature of the vanadium-titanium tailings in Step 1 is 600 - 700 °C, and the time is 5 - 6 h.

6. The preparation method of an antique black tile according to claim 5, characterized in that, The ball milling time in Step 1 is 30 - 90 min, the material-ball ratio is 1:2, the rotation speed of the ball milling is 400 - 450 r / min, and the ball-milled vanadium-titanium tailings powder is dried at a temperature of 70 - 80 °C.

7. The preparation method of an antique black tile according to claim 6, characterized in that, The stirred slurry is trampled repeatedly for 1 - 2 days until the slurry becomes sticky and elastic, and the trampled slurry is cut into pieces.

8. The preparation method of an antique black tile according to claim 7, characterized in that The pressure for the first pressing of the tile blank is 40 - 50 Mpa, the pressure for the second pressing of the tile blank is 70 - 80 Mpa, and the amount of fine vanadium-titanium tailings powder sprayed on the surface of the tile blank is 0.2 - 0.3 g / cm 2 .

9. The preparation method of an antique black tile according to claim 8, characterized in that The temperature increase in stages includes three stages. First, raise the temperature at a heating rate of 5 - 8 °C / min to 700 °C, then raise the temperature at a heating rate of 2 - 3 °C / min to 700 - 1100 °C, and finally, raise the temperature at a heating rate of 0.8 - 1.5 °C / min to 1100 - 1350 °C and keep it at the highest temperature for 30 - 45 h.

10. The preparation method of an antique black tile according to claim 9, characterized in that, After the antique black tiles are taken out of the kiln, they are slightly polished with an air mill and hand-polished with sandpaper to enhance the antique effect.

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