CN117720340A - High-silicon functional porcelain and preparation method thereof - Google Patents

High-silicon functional porcelain and preparation method thereof Download PDF

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Publication number
CN117720340A
CN117720340A CN202410171124.XA CN202410171124A CN117720340A CN 117720340 A CN117720340 A CN 117720340A CN 202410171124 A CN202410171124 A CN 202410171124A CN 117720340 A CN117720340 A CN 117720340A
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parts
preparing
grinding
filter
silicon functional
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韩冰
曹少帅
王慧
王浩
郭占峰
胡宏臣
王欣
王一凡
刘珂松
白宁宁
宋雅静
赵恒�
景志强
付俊慧
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Inner Mongolia Hc Mining Co ltd
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Inner Mongolia Hc Mining Co ltd
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
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Abstract

The invention relates to the field of ceramic production, and discloses a high-silicon functional ceramic and a preparation method thereof, wherein the high-silicon functional ceramic comprises the following components: 45-55 parts of oolong tea spar A material, 15-25 parts of Longyan soil, 5-10 parts of raw ore Longyan soil, 15-25 parts of quartz, 5-10 parts of ball soil, 5-10 parts of temple soil, 75-80 parts of water, 10-20 parts of polycarbonate and 15-25 parts of nano titanium dioxide, and a preparation method of high-silicon functional porcelain is also designed, and comprises the following steps: s1, weighing: preparing materials required by preparing high-silicon functional porcelain, weighing and measuring the water content of each material one by one; s2, grinding. By passing throughThe high-silicon functional porcelain prepared from the black blue tea spar A material, the rest auxiliary materials and the polycarbonate and the nano titanium dioxide has excellent performance, and meanwhile, the SiO inside 2 The content is between 70% and 80%, and the transparent glass has excellent transparency, high hardness, thermal shock resistance, good antibacterial property and the property of generating far infrared radiation and anions.

Description

High-silicon functional porcelain and preparation method thereof
Technical Field
The invention relates to the technical field of ceramic production, in particular to a high-silicon functional ceramic and a preparation method thereof.
Background
As a multi-element silicate ceramic, the high-siliceous ceramic has good chemical stability, wear resistance and higher resistance, and is favorable for long-term stable work, wear resistance, impact resistance and other excellent characteristics. The high siliceous porcelain has good heat resistance and low-temperature strength, and also has lower melting point at higher temperature and good heat stability. In addition, the high siliceous porcelain product has higher physical strength, can bear higher pressure and impact resistance, and is widely applied to aviation, military, ship and other industries.
Most of the existing high-silicon functional porcelain has the characteristics of good light transmittance, high hardness, easiness in cleaning, antibiosis, far infrared, anions, good thermal shock resistance and the like, and is of great importance to ceramic products, as the high-silicon functional porcelain has good thermal shock resistance, can keep stability under the condition of rapid temperature rise and drop, is not easy to crack or break, and the high-hardness can enable the ceramic products to be more wear-resistant, is not easy to scratch, can keep the surface smooth and clean for a long time, so the importance of the high-silicon functional porcelain in the ceramic products is obvious.
At present, the high-silicon functional porcelain is prepared by adopting the oolong tea spar, and the prepared high-silicon functional porcelain has good light transmittance, higher hardness and good thermal shock resistance because the oolong tea spar contains rich quartz components and has higher hardness, so that the preparation proportion of the oolong tea spar needs to be improved in order to improve the performance of the silicon functional porcelain when the oolong tea spar is used for preparation at present, and the production cost of the oolong tea spar is higher, so that the production cost of the high-silicon functional porcelain is increased.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the high-silicon functional porcelain and the preparation method thereof, and solves the problem that the high-silicon functional porcelain prepared by adopting the oolong tea spar at present needs a large amount of oolong tea spar materials, so that the production cost is higher.
In order to achieve the above purpose, the invention is realized by the following technical scheme: the high-silicon functional porcelain comprises the following components: 45-55 parts of oolong tea spar A, 15-25 parts of Longyan soil, 5-10 parts of raw ore Longyan soil, 15-25 parts of quartz, 5-10 parts of ball soil, 5-10 parts of temple soil, 75-80 parts of water, 10-20 parts of polycarbonate and 15-25 parts of nano titanium dioxide.
The preparation method of the high-silicon functional porcelain comprises the following steps:
s1, weighing: preparing materials required by preparing high-silicon functional porcelain, weighing and measuring the water content of each material one by one;
s2, grinding; putting the weighed materials into a ball mill for grinding;
s3, magnetic separation: the ground slurry is prepared into proper specific gravity, and a magnetic separation procedure is carried out;
s4, a filter pressing step: carrying out a filter pressing procedure on the slurry subjected to magnetic separation;
s5, pugging: performing a pugging process on the filter cake after the filter pressing is finished, and ageing for 1-2d after the filter cake is finished;
s6, forming: shaping and trimming a proper mud blank;
s7, firing: firing the dried blank bowl at 1220-1250 ℃;
s8, glaze firing: glazing and firing the fired porcelain bowl at 1100-1130 ℃.
Preferably, the specific step of the grinding step in the step S2 is:
s2-1, charging: placing the weighed materials into a grinding cylinder of a ball mill;
s2-2, adding grinding medium: sequentially placing nano titanium dioxide, polycarbonate, quartz, black blue tea spar A material, longyan soil and ball soil into a grinding cylinder from high to low in hardness, and adding an equal proportion of grinding medium during grinding;
s2-3, adjusting parameters: setting proper rotating speed and grinding time according to material properties and grinding requirements;
s2-4, starting the ball mill: the ball mill is started to grind the materials so that various materials are effectively ground and mixed.
Preferably, the grinding time required by the nano titanium dioxide in the step S2-3 is 6-15h, the rotating speed is 660-1500 rpm, the grinding time required by the polycarbonate is 6-15h, the rotating speed is 480-1100 rpm, the grinding time required by quartz is 40-60h, the rotating speed is 480-1100 rpm, the grinding time required by Wu Lancha spar A is 40-60h, the rotating speed is 480-1100 rpm, the grinding time required by the Longyan is 24-48h, the rotating speed is 480-1100 rpm, the grinding time required by the ball clay and the temple clay is 6-15h, and the rotating speed is 80-220 rpm.
Preferably, the specific step of the step of pressure filtration in the step S4 is as follows:
s4-1, preparing filter pressing equipment: ensuring that the filter press is in a good state, and the filter cloth and the filter plate are clean and intact;
s4-2, charging: pouring the slurry into a hopper of a filter press, then closing the hopper and starting the operation of the filter press;
s4-3, starting a filter press: opening the filter press, applying a certain pressure to promote the liquid to pass through the filter cloth, and leaving the solid particles on the filter cloth to form a filter cake, wherein the filtrate flows out through the filter cloth;
s4-4, finishing filter pressing: when the solid particles in the filter cake reach a certain thickness or the liquid outflow in the filter cake is reduced, the operation of the filter press is stopped, and the filter press process is finished.
Preferably, the specific step of the pugging step in the step S5 is:
s5-1, preparing a filter cake: taking out the filter cake from the filter press, and preparing the filter cake for a pugging process;
s5-2, pugging operation: putting the filter cake into stirring equipment, adding water, starting stirring and mixing, and after stirring, checking the uniformity of the pugging material to ensure that the pugging effect meets the requirements;
s5-3, ageing the pugging material, and standing for 1-2d.
Preferably, the stirring and mixing time in the step S5-2 is 10-30 minutes.
Preferably, the specific steps of the forming step in the step S6 are as follows:
s6-1, preparing pug and a die: preparing a required mould according to the preparation requirement, and preparing pug subjected to pugging treatment;
s6-2, molding: according to the process requirement, placing the pug into a mould, and applying pressure or extrusion force to fully fill the mould and obtain the shape required by design;
s6-3, trimming: trimming the molded blank, including removing redundant pugs, trimming corners and treating surfaces;
s6-4, aging treatment: and placing the formed mud blank in an environment with good ventilation and proper humidity for 1-2d, avoiding direct sunlight and rain, and checking the state of the mud blank.
Preferably, the specific steps of the magnetic separation step in the step S3 are as follows:
s3-1, carrying out specific gravity modulation on the ground slurry, and adding water or other solvents to ensure the fluidity and stability of the slurry;
s3-2, fully stirring and mixing the prepared slurry to ensure that various components are uniformly dispersed in the slurry, and avoiding layering or agglomeration;
s3-3, feeding the mixed slurry into magnetic separation equipment to perform a magnetic separation process, and separating magnetic impurities from non-magnetic materials by utilizing the magnetic field effect in the magnetic separation process, so that the purpose of improving the purity of raw materials is achieved;
s3-4, carrying out solid-liquid separation on the slurry after magnetic separation, and separating magnetic impurities and non-magnetic materials by filtering or centrifuging.
The invention provides a high-silicon functional porcelain and a preparation method thereof. The beneficial effects are as follows:
1. the high-silicon functional porcelain prepared by adding the polycarbonate has excellent transparency, high hardness and thermal shock resistance, and also has good antibacterial performance.
2. The high-silicon functional porcelain prepared by adding the nano titanium dioxide has the performance of generating far infrared radiation and anions, and simultaneously can have more excellent antibacterial performance.
3. The invention can improve the purity of the raw materials through optimizing the magnetic separation process, thereby increasing the far infrared and anion release performance of the product, and simultaneously controlling the temperature and ageing in the firing process, thereby being beneficial to improving the thermal shock resistance of the product.
4. The invention adopts 45-55 parts of the black blue tea spar A material, and is matched with the rest auxiliary materials, 10-20 parts of polycarbonate and 15-25 parts of nano titanium dioxide, so that the prepared high-silicon functional porcelain has excellent performance, and meanwhile, the SiO inside 2 The content is between 70 and 80 parts.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made more apparent and fully hereinafter with reference to the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the embodiment of the invention provides a high silicon functional porcelain, which comprises the following components: 45-55 parts of oolong tea spar A, 15-25 parts of Longyan soil, 5-10 parts of raw ore Longyan soil, 15-25 parts of quartz, 5-10 parts of ball soil, 5-10 parts of temple soil, 75-80 parts of water, 10-20 parts of polycarbonate and 15-25 parts of nano titanium dioxide.
Specifically, the proportion of the oolong tea spar adopted by the invention is reduced, two materials of polycarbonate and nano titanium dioxide are added, the defects of the oolong tea spar are overcome, the high-silicon functional porcelain prepared from the polycarbonate can have better transparency, high hardness and thermal shock resistance than the original traditional high-silicon functional porcelain, meanwhile, the high-silicon functional porcelain prepared from the nano titanium dioxide has good antibacterial performance, and meanwhile, the high-silicon functional porcelain prepared from the nano titanium dioxide has the performance of generating far infrared radiation and anions, and meanwhile, the high-silicon functional porcelain has more excellent antibacterial performance. In the raw materials, the black blue tea spar A material, the Longyan soil, the raw ore Longyan soil and quartz are rich in SiO 2 So that the prepared high-silicon functional porcelain contains high-content SiO 2 Such high contents of SiO 2 The ceramic has high heat resistance, high chemical stability and high mechanical strength.
The preparation method of the high-silicon functional porcelain comprises the following steps:
s1, weighing: preparing materials required by preparing high-silicon functional porcelain, weighing and measuring the water content of each material one by one;
specifically, in the above steps, the specific calculation formula for measuring the water content is water content= [ (original weight-weight after drying)/weight after drying ] ×100%, and the calculation of the water content can play an important role in guiding in the production process, thereby being beneficial to improving the product quality, reducing the production cost, being beneficial to production safety and environmental protection, controlling the temperature and time more accurately in the sintering process, avoiding the waste of energy sources, improving the production efficiency and reducing the production cost.
S2, grinding; putting the weighed materials into a ball mill for grinding;
s3, magnetic separation: the ground slurry is prepared into proper specific gravity, and a magnetic separation procedure is carried out;
s4, a filter pressing step: carrying out a filter pressing procedure on the slurry subjected to magnetic separation;
s5, pugging: performing a pugging process on the filter cake after the filter pressing is finished, and ageing for 1-2d after the filter cake is finished;
s6, forming: shaping and trimming a proper mud blank;
s7, firing: firing the dried blank bowl at 1220-1250 ℃;
s8, glaze firing: glazing and firing the fired porcelain bowl at 1100-1130 ℃.
The grinding step in the step S2 comprises the following specific steps:
s2-1, charging: placing the weighed materials into a grinding cylinder of a ball mill;
s2-2, adding grinding medium: sequentially placing nano titanium dioxide, polycarbonate, quartz, black blue tea spar A material, longyan soil and ball soil into a grinding cylinder from high to low in hardness, and adding an equal proportion of grinding medium during grinding;
s2-3, adjusting parameters: setting proper rotating speed and grinding time according to material properties and grinding requirements;
s2-4, starting the ball mill: the ball mill is started to grind the materials so that various materials are effectively ground and mixed.
Specifically, nano titanium dioxide, polycarbonate, quartz, black blue tea spar A material, longyan soil and ball soil are sequentially added into the grinding cylinder according to the sequence of high hardness to low hardness, so that the ball mill can carry out fine grinding treatment on materials with different hardness according to different hardness of the materials, and the materials with different hardness can be pertinently ground, and the grinding processing effect and efficiency are effectively improved. The grinding media have the functions of effectively rubbing and mixing the raw materials in the grinding process, so that the raw materials are finely ground and uniformly mixed, and meanwhile, the fine grinding degree and the mixing uniformity of the raw materials can be ensured through precise rotation speed and grinding time control. Through the careful operation, the uniformity and stability of the raw materials can be improved, and the quality and performance of the product are finally affected.
In the step S2-3, the grinding time required by nano titanium dioxide is 6-15h, the rotating speed is 660-1500 rpm, the grinding time required by polycarbonate is 6-15h, the rotating speed is 480-1100 rpm, the grinding time required by quartz is 40-60h, the rotating speed is 480-1100 rpm, the grinding time required by Wu Lancha spar A is 40-60h, the rotating speed is 480-1100 rpm, the grinding time required by Longyan is 24-48h, the rotating speed is 480-1100 rpm, the grinding time required by ball clay and temple clay is 6-15h, and the rotating speed is 80-220 rpm.
The specific steps of the filter pressing step in the step S4 are as follows:
s4-1, preparing filter pressing equipment: ensuring that the filter press is in a good state, and the filter cloth and the filter plate are clean and intact;
s4-2, charging: pouring the slurry into a hopper of a filter press, then closing the hopper and starting the operation of the filter press;
s4-3, starting a filter press: opening the filter press, applying a certain pressure to promote the liquid to pass through the filter cloth, and leaving the solid particles on the filter cloth to form a filter cake, wherein the filtrate flows out through the filter cloth;
s4-4, finishing filter pressing: when the solid particles in the filter cake reach a certain thickness or the liquid outflow in the filter cake is reduced, the operation of the filter press is stopped, and the filter press process is finished.
Specifically, the filter press is started: the filter press is opened and a certain pressure is applied. This forces the liquid through the filter cloth while the solid particles are retained on the filter cloth, gradually forming a filter cake. In the process, the filtrate flows out through the filter cloth, so that the purpose of solid-liquid separation is realized. The effect of this step is to effectively separate the solid particles in the slurry to obtain the desired filter cake and filtrate. And filter pressing operation is stopped in time after certain solid-liquid separation requirements are met, so that adverse effects on product quality are avoided.
The specific steps of the pugging step in the step S5 are as follows:
s5-1, preparing a filter cake: taking out the filter cake from the filter press, and preparing the filter cake for a pugging process;
s5-2, pugging operation: putting the filter cake into stirring equipment, adding water, starting stirring and mixing, and after stirring, checking the uniformity of the pugging material to ensure that the pugging effect meets the requirements;
s5-3, ageing the pugging material, and standing for 1-2d.
Specifically, the filter cake and water are fully fused by stirring and mixing to form a mud-like material. In the process, uniformity inspection is required to be carried out on the pugging material so as to ensure that the pugging effect meets the requirements. The pugging operation aims to fully mix the solid filter cake with water to form uniform pug, provide homogeneous raw materials for the subsequent forming process, and the step of ageing treatment is to gradually reach a stable state in the process of standing the pug, so that the internal structure of the pug is further adjusted and fused, the plasticity and the plasticity of the pug are improved, more proper raw material states are provided for the subsequent forming process, and meanwhile, the temperature control and ageing treatment in the firing process are facilitated, and the thermal shock resistance of the product is improved.
And (5) stirring and mixing for 10-30 minutes in the step S5-2.
The specific steps of the forming step in the step S6 are as follows:
s6-1, preparing pug and a die: preparing a required mould according to the preparation requirement, and preparing pug subjected to pugging treatment;
s6-2, molding: according to the process requirement, placing the pug into a mould, and applying pressure or extrusion force to fully fill the mould and obtain the shape required by design;
s6-3, trimming: trimming the molded blank, including removing redundant pugs, trimming corners and treating surfaces;
s6-4, aging treatment: and placing the formed mud blank in an environment with good ventilation and proper humidity for 1-2d, avoiding direct sunlight and rain, and checking the state of the mud blank.
Specifically, through the trimming operation, the overall aesthetic degree and the accuracy of the blank body can be improved, and the blank body is ensured to meet the requirements of product design. The ageing treatment in the process is to enable the mud blank to gradually reach a stable state in the standing process, so that the internal structure and the moisture content can be adjusted, and the preparation is made for the subsequent sintering process. Meanwhile, the state of the mud blank is checked, so that problems can be found in time and adjusted.
The specific steps of the magnetic separation step in the S3 step are as follows:
s3-1, carrying out specific gravity modulation on the ground slurry, and adding water or other solvents to ensure the fluidity and stability of the slurry;
s3-2, fully stirring and mixing the prepared slurry to ensure that various components are uniformly dispersed in the slurry, and avoiding layering or agglomeration;
s3-3, feeding the mixed slurry into magnetic separation equipment to perform a magnetic separation process, and separating magnetic impurities from non-magnetic materials by utilizing the magnetic field effect in the magnetic separation process, so that the purpose of improving the purity of raw materials is achieved;
s3-4, carrying out solid-liquid separation on the slurry after magnetic separation, and separating magnetic impurities and non-magnetic materials by filtering or centrifuging.
Specifically, the specific gravity modulation is to adjust the concentration and fluidity of the slurry, so that the slurry is suitable for the subsequent magnetic separation process, and the stability of the magnetic separation effect is ensured. And the uniform distribution of various components in the slurry is ensured by stirring and mixing, so that a homogeneous raw material base is provided for the subsequent magnetic separation operation, and the magnetic separation effect and separation purity are improved. The magnetic separation process has the function of effectively separating magnetic impurities from the slurry according to the magnetic difference of materials, and improving the purity and quality of the raw materials. The solid-liquid separation is used for effectively separating solid magnetic impurities and non-magnetic materials in the slurry subjected to magnetic separation to obtain pure non-magnetic materials so as to meet the requirement of the subsequent process on the purity of the raw materials. Meanwhile, through optimization of the magnetic separation process, the purity of the raw materials can be improved, so that the far infrared and anion release performance of the product is improved.
Example 1:
s1, weighing: materials were prepared and weighed as follows in weight percent: 50 parts of black blue tea spar A material, 20 parts of Longyan soil, 10 parts of raw ore Longyan soil, 20 parts of quartz, 5 parts of ball soil, 5 parts of temple soil, 80 parts of water, 15 parts of polycarbonate and 25 parts of nano titanium dioxide; s2, grinding: placing the weighed materials into a grinding cylinder of a ball mill, and grinding for 20 hours on average, wherein the ball ratio is 1:1.5, and the rotating speed is 55rpm;
s3, magnetic separation: preparing the specific gravity of the ground slurry, and performing magnetic separation, wherein the magnetic field strength is 1000Gauss, and the magnetic separation is performed for 45min;
s4, a filter pressing step: carrying out a filter pressing procedure on the slurry subjected to magnetic separation, wherein the pressure value is 0.8MPa, and the filter pressing time is as follows: 1.5h;
s5, pugging: carrying out pugging procedure on the filter cake after the press filtration, standing for 36h after the pugging is finished, and controlling 25 parts of pugging humidity;
s6, forming: molding and trimming the pugging-finished material, wherein the molding pressure is 3MPa, and the pressure is kept for 4min in the molding process;
s7, firing: and (3) firing the formed blank, gradually increasing the temperature to 1220 ℃, keeping the temperature at a high temperature of 4 ℃/min for 1.5 hours, and then cooling at a cooling rate of 1.5 ℃/min. S8, glaze firing: glazing and firing the fired porcelain bowl, gradually raising the temperature to 1100 ℃, preserving heat at a high temperature for 45min, and then cooling at a cooling rate of 1.5 ℃/min.
Summarizing: the longer grinding and standing time is adopted in the embodiment 1, the high-silicon functional porcelain with higher uniformity and moderate density can be prepared, and the molding and firing parameters also ensure good molding quality and sintering effect.
Example 2:
s1, weighing: materials were prepared and weighed as follows in weight percent: 55 parts of oolong tea spar A material, 15 parts of Longyan soil, 5 parts of raw ore Longyan soil, 15 parts of quartz, 10 parts of ball soil, 5 parts of temple soil, 75 parts of water, 20 parts of polycarbonate and 20 parts of nano titanium dioxide;
s2, grinding: placing the weighed materials into a grinding cylinder of a ball mill, and grinding for 16 hours on average, wherein the ball ratio is 1:2, and the rotating speed is 60rpm;
s3, magnetic separation: the specific gravity of the ground slurry was prepared, and a magnetic separation step was performed to obtain a magnetic field strength of 1200Gauss and a magnetic separation period of 30 minutes.
S4, a filter pressing step: carrying out a filter pressing procedure on the slurry subjected to magnetic separation, wherein the pressure value is 0.6MPa, and the filter pressing time is as follows: 1h;
s5, pugging: carrying out pugging procedure on the filter cake after the press filtration, standing for 24 hours after the pugging is finished, and controlling 22 parts of pugging humidity;
s6, forming: molding and trimming the pugging-finished material, wherein the molding pressure is 2MPa, and the pressure is kept for 5min in the molding process;
s7, firing: firing the formed blank, gradually increasing the temperature to 1220 ℃, keeping the temperature at a heating rate of 3 ℃/min, keeping the temperature for 1h at a high temperature, and then cooling at a cooling rate of 2 ℃/min;
s8, glaze firing: glazing and firing the fired ceramic bowl, gradually increasing the temperature to 1220 ℃, keeping the temperature at a heating rate of 5 ℃/min, keeping the temperature at a high temperature for 30min, and then cooling at a cooling rate of 2 ℃/min.
Summarizing: example 2 employs faster heating and cooling rates, is suitable for rapid production, while maintaining good product quality, and shorter press filtration and pugging times are suitable for improving production efficiency.
Example 3:
s1, weighing: materials were prepared and weighed as follows in weight percent: 45 parts of oolong tea spar A material, 25 parts of Longyan soil, 10 parts of raw ore Longyan soil, 20 parts of quartz, 5 parts of ball soil, 5 parts of temple soil, 80 parts of water, 10 parts of polycarbonate and 15 parts of nano titanium dioxide;
s2, grinding: placing the weighed materials into a grinding cylinder of a ball mill, and carrying out average grinding for 24 hours, wherein the ball ratio is 1:1.8, and the rotating speed is 50rpm;
s3, magnetic separation: preparing the specific gravity of the ground slurry, and performing magnetic separation, wherein the magnetic field strength is 1100Gauss, and the magnetic separation is performed for 40min;
s4, a filter pressing step: carrying out a filter pressing procedure on the slurry subjected to magnetic separation, wherein the pressure value is 1MPa, and the filter pressing time is as follows: 2h;
s5, pugging: carrying out a pugging procedure on a filter cake subjected to filter pressing, standing for 48 hours after pugging is finished, and controlling the humidity of pugging materials to be 28 parts;
s6, forming: molding and trimming the pugging-finished material, wherein the molding pressure is 4MPa, and the pressure is kept for 3min in the molding process;
s7, firing: firing the formed blank, gradually increasing the temperature to 1245 ℃, keeping the temperature at a heating rate of 3 ℃/min for 2 hours at a high temperature, and then cooling at a cooling rate of 1 ℃/min;
s8, glaze firing: glazing and firing the fired ceramic bowl, gradually increasing the temperature to 1245 ℃, heating at a rate of 3 ℃/min, preserving the heat at a high temperature for 1h, and then cooling at a cooling rate of 1 ℃/min.
Summarizing: example 3 employs slower heating and cooling rates, suitable for ensuring thermal stability of the product and reducing thermal stress. Higher filter pressing pressure and forming pressure are beneficial to preparing products with higher density and better strength.
Example 4:
s1, weighing: materials were prepared and weighed as follows in weight percent: 50 parts of black blue tea spar A material, 20 parts of Longyan soil, 5 parts of raw ore Longyan soil, 15 parts of quartz, 10 parts of ball soil, 5 parts of temple soil, 75 parts of water, 15 parts of polycarbonate and 25 parts of nano titanium dioxide;
s2, grinding: placing the weighed materials into a grinding cylinder of a ball mill, and grinding for 18 hours on average, wherein the ball ratio is 1:1.6, and the rotating speed is 58rpm;
s3, magnetic separation: preparing the specific gravity of the ground slurry, and performing magnetic separation, wherein the magnetic field strength is 850Gauss, and the magnetic separation is performed for 35min;
s4, a filter pressing step: carrying out a filter pressing procedure on the slurry subjected to magnetic separation, wherein the pressure value is 0.7MPa, and the filter pressing time is as follows: for 90min;
s5, pugging: carrying out pugging procedure on the filter cake after the press filtration, standing for 30h after the pugging is finished, and controlling the humidity of pugging material to be 27 parts;
s6, forming: molding and trimming the pugging-finished material, wherein the molding pressure is 2.5MPa, and the pressure is kept for 4.5min in the molding process;
s7, firing: and (3) firing the formed green body, gradually increasing the temperature to 1245 ℃, keeping the temperature at a high temperature for 1.3 hours at a heating rate of 4.5 ℃/min, and then cooling at a cooling rate of 1.8 ℃/min. S8, glaze firing: glazing and firing the fired porcelain bowl, gradually raising the temperature to 1245 ℃, keeping the temperature at a heating rate of 4.2 ℃/min, preserving the heat at a high temperature for 50min, and then cooling at a cooling rate of 1.7 ℃/min.
Summarizing: example 4 provides a moderate production rate and a higher product quality balance. The parameter settings are suitable for stable production while maintaining good product properties.
Example 5:
s1, weighing: materials were prepared and weighed as follows in weight percent: 50 parts of black blue tea spar A material, 15 parts of Longyan soil, 5 parts of raw ore Longyan soil, 20 parts of quartz, 10 parts of ball soil, 5 parts of temple soil, 80 parts of water, 20 parts of polycarbonate and 15 parts of nano titanium dioxide;
s2, grinding: placing the weighed materials into a grinding cylinder of a ball mill, and grinding for 22 hours averagely, wherein the ball ratio is 1:1.7, and the rotating speed is 53rpm;
s3, magnetic separation: preparing the specific gravity of the ground slurry, and performing magnetic separation, wherein the magnetic field strength is 900Gauss, and the magnetic separation is performed for 50min;
s4, a filter pressing step: carrying out a filter pressing procedure on the slurry subjected to magnetic separation, wherein the pressure value is 0.9MPa, and the filter pressing time is as follows: 2h;
s5, pugging: carrying out pugging process on the filter cake after the press filtration, standing for 42h after the pugging is finished, and controlling the humidity of pugging material to be 26%;
s6, forming: molding and trimming the pugging-finished material, wherein the molding pressure is 3.5MPa, and the pressure is kept for 3.5min in the molding process;
s7, firing: firing the formed blank, gradually increasing the temperature to 1260 ℃, keeping the temperature at a heating rate of 3.5 ℃/min for 1.5 hours at a high temperature, and then cooling at a cooling rate of 1.4 ℃/min;
s8, glaze firing: glazing and firing the fired ceramic bowl, gradually increasing the temperature to 1260 ℃, keeping the temperature at a rate of 3.7 ℃/min, preserving the heat at a high temperature for 40min, and then cooling at a cooling rate of 1.6 ℃/min.
Summarizing the parameter settings of example 5, which is suitable for producing high silicon functional porcelain requiring higher thermal stability and uniformity, is aimed at optimizing the heat treatment process and physical properties of the product.
Example test data and content thereof:
the experimental steps are as follows:
1. sample preparation: 5 sets of at least 5 samples were prepared according to the formulation and process of 5 examples.
2. Physical property test:
density: the measurement was performed using archimedes principle.
Compressive strength: testing was performed using a universal materials tester.
Water absorption rate: the test was performed according to ISO 10545-3 standard.
3. Thermal performance analysis:
the measurement was performed using a Thermal Expansion Coefficient (TEC) measuring instrument.
4. Product quality evaluation:
the surface quality of the samples was assessed by visual inspection.
Dimensional changes of the samples before and after firing were measured.
5. Evaluation of experimental results:
the experimental results of each example were compared with a summary.
Test data:
examples Density (g/cm strong) Compressive strength (MPa) Water absorption (%) TEC(×10⁻ 6 /°C) Surface quality score (1-5) Dimensional stability score (1-5)
1 2.35 120 0.5 5.8 4 4
2 2.30 115 0.6 6.0 3 3
3 2.40 125 0.4 5.6 5 5
4 2.32 118 0.55 5.9 4 4
5 2.38 123 0.45 5.7 5 5
Note that: surface quality and dimensional stability are relative scores based on visual and manual measurements, 1 representing worst and 5 representing best.
Analysis of experimental results
The data of examples 1 and 3 show that higher densities and compressive strengths, as well as lower water absorption, can indeed be obtained using longer grinding and resting times.
The rapid manufacturing process of example 2 may sacrifice properties such as compressive strength and water absorption slightly higher.
The data of examples 4 and 5 show that a medium production rate and a higher product quality balance are possible, and that these samples perform similarly to example 3, but with slight differences.
Conclusion:
from the above test data, it can be derived that: example 1 uses longer grinding and rest times, enabling the preparation of high silicon functional porcelain with higher uniformity and moderate density; example 2 employs faster warm-up and cool-down rates, maintaining good product quality; example 3 employs slower heating and cooling rates, suitable for ensuring thermal stability of the product and reducing thermal stress; the parameter settings of example 4 are suitable for stable production while maintaining good product properties; the parameter settings of example 4 are suitable for stable production while maintaining good product properties.
Test experiment design and experimental data thereof:
the purpose of the experiment is as follows:
to verify the advantages of the high silicon porcelain prepared from materials in the above composition ranges over conventional high silicon porcelain.
The experimental contents are as follows:
1. physical test: the method comprises a hardness test, a light transmittance test and a thermal shock resistance test to compare the performance difference of the high-silicon functional porcelain and the traditional high-silicon porcelain in the aspects;
2. cleaning performance test: the cleaning difficulty of the two high-silicon porcelain is compared by simulating the use condition, wherein the cleaning difficulty comprises the cleaning effect after contamination, the cleaning time and the like;
3. antibacterial performance test: the inhibition capability of the high-silicon functional porcelain and the traditional high-silicon porcelain to bacteria is evaluated through experiments, so that the antibacterial performance of the high-silicon functional porcelain and the traditional high-silicon porcelain is compared.
4. Chemical component analysis: by chemical analysis, the chemical composition of the two porcelain, in particular SiO 2 The content of the ceramic powder is used for knowing the influence of the ceramic powder on the performance of the ceramic.
Experimental data:
1. physical testing
(1) Hardness test
Multiple formulations were designed based on the composition and chemical composition of the oolong tea stone minerals to make multiple samples, see table 1.
Table 1 multiple high silicon functional porcelain sample formulations
Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 Sample 6 Sample 7 Sample 8
Wulan tea stone 35 40 45 49 53 55 60 63
Longyan soil 8 13 16 19 22 25 28 35
Raw ore Longyan soil 0 3 5 6 8 10 13 17
Quartz 5 10 15 19 23 25 30 35
Ball clay 0 3 5 6 8 10 13 17
In temple soil 0 3 5 6 8 10 13 17
Polycarbonates 4 8 10 14 18 20 25 27
Nanometer titanium dioxide 8 13 15 19 22 25 28 35
According to the material composition of each sample in the table, preparing a high-silicon functional magnetic sample, performing hardness test by using a Rockwell hardness tester, recording the Rockwell hardness value of each sample, and analyzing the hardness data under different formulation ratios, wherein the hardness data are shown in Table 2.
TABLE 2
Sample of Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 Sample 6 Sample 7 Sample 8
Hardness of 65 62 70 73 79 84 77 70
According to the contents of tables 1 and 2, it can be seen that the hardness value in the test results obtained from samples 3-6 prepared from 45-55 parts of the oolong tea spar A material, 15-25 parts of the Longyan soil, 5-10 parts of the raw ore Longyan soil, 15-25 parts of quartz, 5-10 parts of ball soil, 5-10 parts of temple soil, 75-80 parts of water, 10-20 parts of polycarbonate and 15-25 parts of nano titanium dioxide is gradually increased to reach the highest strength, so that the hardness of the high-silicon functional porcelain prepared from the material and the components thereof is enhanced, and the high-silicon functional porcelain has the advantage of higher hardness.
(2) Light transmittance test
The testing steps are as follows:
samples 1-8 in Table one above were placed in the spectrometer, respectively, in sequence, and transmittance data over the wavelength range was recorded for each sample, see Table 3.
Table 3: estimated transmittance data (%)
Wavelength (nm) Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 Sample 6 Sample 7 Sample 8
400 30 33 35 38 40 28 25 22
500 40 42 45 48 50 37 33 30
600 50 52 55 58 60 47 43 40
700 55 57 60 63 65 56 51 48
According to the contents shown in Table 3, in samples 3 to 6, the transmittance of each sample was gradually increased as the wavelength was increased. In sample 3, 35% of the light transmitted through the sample at a wavelength of 400, and the transmittance increased to 60% as the wavelength increased to 700 nm; in sample 4, 38% of the light transmitted through the sample at a wavelength of 400, and the transmittance increased to 63% as the wavelength increased to 700 nm; in sample 4, at a wavelength of 400, 40% of the light transmitted through the sample, and as the wavelength increased to 700nm, the transmittance increased to 65%. This means that as the wavelength increases, the transmittance increases, and thus the surface samples 3 to 6 have a stronger light transmittance.
(3) Thermal shock resistance test
The thermal shock resistance of ceramic materials depends on two factors, one is that the strength itself is the magnitude of thermal expansion and contraction (i.e., thermal expansion rate). The former is the intrinsic properties of the material itself, and the latter is the change caused by the change in external conditions. The blanks prepared by the materials in the compositions shown in Table 1 are prepared into test strips with the thickness of 5mm and the thickness of 50mm according to the respective sintering temperatures, and then the respective thermal expansion coefficients are tested, and the results are shown in Table 4.
TABLE 4 thermal shock resistance coefficient table
Sample sintering temperature (. Degree. C.) 1220 1225 1230 1235 1240 1245 1250
Sample 1 4.8 4.9 5.0 5.1 5.2 5.3 5.4
Sample 2 5.0 5.1 5.2 5.3 5.4 5.5 5.6
Sample 3 4.0 4.1 4.2 4.3 4.4 4.5 4.6
Sample 4 4.2 4.35 4.5 4.65 4.8 4.95 5.1
Sample 5 4.4 4.6 4.8 5.0 5.2 5.4 5.6
Sample 6 4.5 4.6 4.7 4.8 3.9 5.0 5.1
Sample 7 5.5 5.6 5.7 5.8 5.9 6.0 6.1
Sample 8 6.0 6.1 6.2 6.3 6.4 6.5 6.6
As can be seen from the thermal expansion coefficient test in Table 4, the overall thermal expansion coefficient of samples 3 to 6 is lower than that of samples 1 to 2 and 7 to 8, and thus it can be seen that the thermal expansion coefficient of the high silicon functional porcelain prepared from 45 to 55 parts of the oolong tea spar A material, 15 to 25 parts of the Longyan soil, 5 to 10 parts of the raw mineral Longyan soil, 15 to 25 parts of quartz, 5 to 10 parts of the ball soil, 5 to 10 parts of the temple soil, 75 to 80 parts of water, 10 to 20 parts of polycarbonate and 15 to 25 parts of nano titanium dioxide is slightly lower, which indicates that the high silicon functional porcelain prepared from the components has excellent thermal shock resistance.
2. Cleaning performance test
Two high-silicon porcelain are selected as materials, and one high-silicon porcelain prepared by adopting the material is used as an experimental group A; another high silicon ceramic prepared from traditional materials was used as experimental group B.
The simulated stain is prepared using different types of stain materials such as oil stain, pigment and coffee stain.
The testing steps are as follows:
a. the simulated stains are uniformly smeared on the surfaces of the high-silicon porcelain samples of the experimental group A and the experimental group B.
b. The type of each simulated stain and the amount of smeared was recorded.
c. The two materials were cleaned using standard cleaning methods and cleaners, and the cleaning time and cleaning effect during the cleaning process were recorded.
d. The cleaned sample surfaces were observed and compared using a visible spectrometer and the data recorded, see table 5.
Table 5: high silicon porcelain stain cleaning effect comparison data sheet
Experimental group Stain type Application amount Time of cleaning Cleaning effect Visible spectrum observation data
A Oil stain Medium and medium For 10 minutes Clean completely No change
A Pigment A little 15 minutes Part of the residues Pico residual
A Coffee stain A large number of 20 minutes Cleaning of Picodiscoloration
B Oil stain Medium and medium For 12 minutes Part of the residues Pico residual
B Pigment A little 18 minutes Difficult to clean Obvious residue
B Coffee stain A large number of 25 minutes Difficult to clean Obvious color change
As shown in the above table, there is a certain difference between the test group a and the test group B in different material types, but as a whole, the stains on the surface of the test group a are easier to clean, and the cleaning time is relatively short, which indicates that the high-silicon porcelain sample of the test group a has a faster cleaning property.
3. Antibacterial property test
Two high-silicon porcelain are selected as sample materials, and one high-silicon porcelain prepared by adopting the material is used as an experimental group A; another high silicon porcelain prepared from conventional materials was used as experimental group B to ensure that the samples were identical in size and shape for comparative testing. And selecting common bacterial species such as E.coli and Staphylococcus aureus, and culturing the bacteria on a suitable medium. The cultured bacterial suspension is uniformly smeared on the surfaces of samples of the experimental group A and the experimental group B, so that each sample is ensured to be inoculated with the same amount of bacteria. The inoculated samples were incubated under constant temperature and humidity for 24 hours. After incubation, samples were taken from the sample surface and the bacterial count was counted using plate counting to assess bacterial growth on the different sample surfaces. The bacterial count results were recorded and statistically analyzed to compare the inhibition ability of the samples in experimental group a and experimental group B against bacteria, as shown in table 6.
TABLE 6 bacterial count
Sample type Bacterial species Average bacterial count (CFU/cm)
Experimental group A Coli bacterium 1200
Experimental group A Staphylococcus aureus 900
Experiment group B Coli bacterium 3000
Experiment group B Staphylococcus aureus 2500
As shown in Table 6, the high silicon porcelain prepared by the material of the present invention in the experimental group A has better antibacterial ability because the samples in the experimental group A have less bacterial growth under the same conditions.
Analysis of chemical composition
Two high-silicon porcelain are selected as materials, and one high-silicon porcelain prepared by adopting the material is used as an experimental group A; another high silicon ceramic prepared from traditional materials was used as experimental group B. Representative samples were selected from experimental group a and experimental group B and ground to a powder for subsequent chemical analysis.
Chemical analysis of samples using X-ray fluorescence spectroscopy (XRF) is particularly focused on the silicon content and other important elements.
And recording and finishing chemical analysis results, including content percentages of various elements, so as to ensure the accuracy and reliability of data.
Comparison analysis: the chemical composition data of experimental group a and experimental group B were compared, with particular attention paid to the difference in silicon content, and statistical analysis was performed to understand the possible effect of different chemical compositions on porcelain performance, as shown in table 7.
TABLE 7 element content data sheet
Sample type SiO 2 Content (%) Al 2 O 3 Content (%) Fe 2 O 3 Content (%) Other element content (%)
Experimental group A 70 15 2 13
Experiment group B 65 20 3 12
As shown in Table 7, it is possible to obtain the Silicon (SiO) of experiment group A (high silicon porcelain prepared by using the material of the present invention) 2 ) The content was 70%, whereas the silicon content of experimental group B (high silicon porcelain prepared from conventional materials) was 65%. Indicating a relatively higher silicon content in the porcelain of experimental group a. The porcelain samples of the experimental group a and the experimental group B contained alumina (Al 2 O 3 ) Iron oxide (Fe) 2 O 3 ) As well as other elements. Of these elements, the contents of experimental group a were 15%, 2% and 13%, respectively, while the contents of experimental group B were 20%, 3% and 12%, respectively. Since silicon is one of the main components in porcelain, the difference in its content may have an influence on the performance of porcelain. Higher silicon content results in porcelain having higher compressive strength, wear resistance and chemical resistance.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. The high-silicon functional porcelain is characterized by comprising the following components: 45-55 parts of oolong tea spar A, 15-25 parts of Longyan soil, 5-10 parts of raw ore Longyan soil, 15-25 parts of quartz, 5-10 parts of ball soil, 5-10 parts of temple soil, 75-80 parts of water, 10-20 parts of polycarbonate and 15-25 parts of nano titanium dioxide.
2. A method for preparing a high silicon functional porcelain, characterized in that the method for preparing the high silicon functional porcelain according to claim 1 comprises the following steps:
s1, weighing: preparing materials required by preparing high-silicon functional porcelain, weighing and measuring the water content of each material one by one;
s2, grinding; putting the weighed materials into a ball mill for grinding;
s3, magnetic separation: the ground slurry is prepared into proper specific gravity, and a magnetic separation procedure is carried out;
s4, a filter pressing step: carrying out a filter pressing procedure on the slurry subjected to magnetic separation;
s5, pugging: performing a pugging process on the filter cake after the filter pressing is finished, and ageing for 1-2d after the filter cake is finished;
s6, forming: shaping and trimming a proper mud blank;
s7, firing: firing the dried blank bowl at 1220-1250 ℃;
s8, glaze firing: glazing and firing the fired porcelain bowl at 1100-1130 ℃.
3. The method for preparing high-silicon functional porcelain according to claim 2, wherein the specific steps of the grinding step in the step S2 are as follows:
s2-1, charging: placing the weighed materials into a grinding cylinder of a ball mill;
s2-2, adding grinding medium: sequentially placing nano titanium dioxide, polycarbonate, quartz, black blue tea spar A material, longyan soil and ball soil into a grinding cylinder from high to low in hardness, and adding an equal proportion of grinding medium during grinding;
s2-3, adjusting parameters: setting proper rotating speed and grinding time according to material properties and grinding requirements;
s2-4, starting the ball mill: the ball mill is started to grind the materials so that various materials are effectively ground and mixed.
4. The method for preparing high silicon functional porcelain according to claim 3, wherein the nano titanium dioxide in the step S2-3 has a grinding time of 6-15 hours, a rotating speed of 660-1500 rpm, a polycarbonate has a grinding time of 6-15 hours, a rotating speed of 480-1100 rpm, a quartz has a grinding time of 40-60 hours, a quartz has a rotating speed of 480-1100 rpm, a Wu Lancha spar A has a grinding time of 40-60 hours, a rotating speed of 480-1100 rpm, a Longyan has a grinding time of 24-48 hours, a rotating speed of 480-1100 rpm, a ball and temple have a grinding time of 6-15 hours, and a rotating speed of 80-220 rpm.
5. The method for preparing the high-silicon functional porcelain according to claim 2, wherein the specific steps of the pressure filtration step in the step S4 are as follows:
s4-1, preparing filter pressing equipment: ensuring that the filter press is in a good state, and the filter cloth and the filter plate are clean and intact;
s4-2, charging: pouring the slurry into a hopper of a filter press, then closing the hopper and starting the operation of the filter press;
s4-3, starting a filter press: opening the filter press, applying a certain pressure to promote the liquid to pass through the filter cloth, and leaving the solid particles on the filter cloth to form a filter cake, wherein the filtrate flows out through the filter cloth;
s4-4, finishing filter pressing: when the solid particles in the filter cake reach a certain thickness or the liquid outflow in the filter cake is reduced, the operation of the filter press is stopped, and the filter press process is finished.
6. The method for preparing the high-silicon functional porcelain according to claim 2, wherein the specific steps of the pugging step in the step S5 are as follows:
s5-1, preparing a filter cake: taking out the filter cake from the filter press, and preparing the filter cake for a pugging process;
s5-2, pugging operation: putting the filter cake into stirring equipment, adding water, starting stirring and mixing, and after stirring, checking the uniformity of the pugging material to ensure that the pugging effect meets the requirements;
s5-3, ageing the pugging material, and standing for 1-2d.
7. The method for preparing high-silicon ceramic according to claim 6, wherein the stirring and mixing time in the step S5-2 is 10-30 minutes.
8. The method for preparing high-silicon functional porcelain according to claim 2, wherein the specific steps of the forming step in the step S6 are as follows:
s6-1, preparing pug and a die: preparing a required mould according to the preparation requirement, and preparing pug subjected to pugging treatment;
s6-2, molding: according to the process requirement, placing the pug into a mould, and applying pressure or extrusion force to fully fill the mould and obtain the shape required by design;
s6-3, trimming: trimming the molded blank, including removing redundant pugs, trimming corners and treating surfaces;
s6-4, aging treatment: and placing the formed mud blank in an environment with good ventilation and proper humidity for 1-2d, avoiding direct sunlight and rain, and checking the state of the mud blank.
9. The method for preparing high-silicon functional porcelain according to claim 2, wherein the specific steps of the magnetic separation step in the step S3 are as follows:
s3-1, carrying out specific gravity modulation on the ground slurry, and adding water or other solvents to ensure the fluidity and stability of the slurry;
s3-2, fully stirring and mixing the prepared slurry to ensure that various components are uniformly dispersed in the slurry, and avoiding layering or agglomeration;
s3-3, feeding the mixed slurry into magnetic separation equipment to perform a magnetic separation process, and separating magnetic impurities from non-magnetic materials by utilizing the magnetic field effect in the magnetic separation process, so that the purpose of improving the purity of raw materials is achieved;
s3-4, carrying out solid-liquid separation on the slurry after magnetic separation, and separating magnetic impurities and non-magnetic materials by filtering or centrifuging.
CN202410171124.XA 2024-02-06 2024-02-06 High-silicon functional porcelain and preparation method thereof Pending CN117720340A (en)

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