CN115028441A - Green and environment-friendly leucite preparation method - Google Patents

Green and environment-friendly leucite preparation method Download PDF

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CN115028441A
CN115028441A CN202210678923.7A CN202210678923A CN115028441A CN 115028441 A CN115028441 A CN 115028441A CN 202210678923 A CN202210678923 A CN 202210678923A CN 115028441 A CN115028441 A CN 115028441A
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leucite
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corundum
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崔为成
崔紫萌
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Rizhao Maoyuan Electronics Co ltd
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Abstract

The invention provides a green and environment-friendly leucite preparation method, which comprises the following steps: (1) weighing raw materials according to the formula of the leucite, grinding uniformly, and sieving to obtain a batch; (2) putting the batch obtained in the step (1) into a container for sintering, cooling, crushing and sieving to obtain an intermediate; (3) and (3) putting the intermediate obtained in the step (2) into a container for heat treatment, cooling, crushing and sieving to obtain the leucite. The leucite prepared by the method has the advantages of high purity, simple process, low cost, greenness, no pollution and suitability for batch production.

Description

Green and environment-friendly leucite preparation method
Technical Field
The invention relates to the technical field of ceramics, in particular to a green and environment-friendly leucite preparation method.
Background
The leucite ceramics have been widely used in various fields such as biomedical (CN108742904A), architectural decoration (CN108727840A), automobile decoration (CN107619598A), and fire-resistant material (CN106278208A) due to its excellent mechanical properties, acid and alkali corrosion resistance, high refractive index, low density, and high expansion characteristics.
The leucite has good mechanical property and acid and alkali corrosion resistance, and in the cooling process, the crystal phase of the leucite is changed from a cubic phase to a tetragonal phase, and the accompanying volume shrinkage can generate compressive stress, thereby improving the strength of the matrix. Such as dental ceramic powder with thermal expansion coefficient of 8.5-9X10 -6 /° c) coefficient of thermal expansion compared to that of the commercial zirconia ceramic crown (10.5X 10) -6 /° c), reduces the mismatch of thermal expansion coefficients, has large brittleness of the porcelain powder, can improve the thermal expansion coefficients, the strength and the acid and alkali resistance of the porcelain powder by adding a small amount of leucite into the porcelain powder, and has basically consistent refractive index with the veneer porcelain, so the white garnet has the advantages of low thermal expansion coefficient, high strength, high acid and alkali resistance, and good heat resistance, heat resistance and the like heat resistance, heat resistanceStrong diffuse reflection can not be generated in the porcelain powder, namely, the light transmission (beauty) of the porcelain powder can not be influenced. In addition, the leucite can be co-fired with the zirconia powder to synthesize, and the thermal expansion coefficient of the leucite is adjusted. Other applications of leucites can be found in the exemplified patents, which are not listed here.
The application of the leucite mainly comprises directly using the leucite, and separating the leucite crystal phase (CN105837047B) in the glass phase or synthesizing the leucite and other crystal phases or materials into a composite crystal phase material (CN 110256063A). The quantity of leucite in nature is small, so artificial synthesis is needed. The synthesis method of leucite mainly comprises a solid phase method, a hydrothermal method, a sol-gel method, a coprecipitation method and the like. The solid phase method is mainly characterized in that the white garnet is melted into glass, then water quenched and then thermally treated for crystallization, so that the purity of the obtained white garnet is not very high, and the energy consumption is high; the hydrothermal method, the coprecipitation method and the sol-gel method can obtain the leucite with high powder granularity, high surface activity and high purity, but the raw material cost is higher, the synthesis process is complex, high-temperature calcination is also needed, and the comprehensive cost is higher. Compared with the prior art, the solid phase method has the advantages of simple, controllable and adjustable process, short process period, low cost and high energy consumption, can be reduced by adjusting the formula and the process, and is suitable for batch production.
Disclosure of Invention
The invention aims to provide a green and environment-friendly leucite preparation method to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of green environment-friendly leucite comprises the following steps:
(1) the composition comprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 55.02 percent, the sum of the weight percent of the components is 100 percent, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 4-7 wt% of TiO, based on the total weight of the aforementioned components 2 0.5 wt% of the total weight of the foregoing components, B 2 O 3 Is 0.5 wt% of the total weight of the componentsWeighing raw materials, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) putting the batch obtained in the step (1) into a corundum sagger, melting for 2h at 1500-;
(3) and (3) preserving the heat of the intermediate obtained in the step (2) at 900-.
The invention has the advantages that: the leucite prepared by the method has the advantages of high purity, simple process, low cost, greenness, no pollution and suitability for batch production.
Drawings
FIG. 1 is an XRD pattern of leucite incubated at 900-;
FIG. 2 is an XRD pattern of leucite incubated at 900-;
FIG. 3 is an XRD contrast of leucites incubated at 900-.
Detailed Description
The technical solutions of the present invention are described below by specific examples, which are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention.
Example 1
A preparation method of green environment-friendly leucite comprises the following steps:
(1) the composition comprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 : 55.02 t%, the sum of the weight percentages of the components is 100%, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 4 wt% of the total weight of the aforementioned components, TiO 2 0.5 wt% of the total weight of the aforementioned components, B 2 O 3 Weighing raw materials in 0.5 wt% of the total weight of the above components, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) and (2) putting the batch obtained in the step (1) into a corundum sagger, melting for 2 hours at 1600 ℃, cooling along with a furnace, taking out porous loose melt in the corundum sagger, putting the porous loose melt into a ball milling bottle of corundum medium or zirconia medium, performing roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain an intermediate.
(3) And (3) preserving the heat of the intermediate obtained in the step (2) at 900 ℃ for 2 hours, cooling the intermediate along with a furnace, taking the intermediate out, putting the intermediate into a ball milling bottle of corundum medium or zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain leucite.
Example 2
A preparation method of green environment-friendly leucite comprises the following steps:
(1) the composition comprises the following components in percentage by weight: k is 2 O21.58％，Al 2 O 3 23.40％，SiO 2 : 55.02 t%, the sum of the weight percentages of the components is 100%, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 5 wt% of the total weight of the aforementioned components, TiO 2 0.5 wt% of the total weight of the aforementioned components, B 2 O 3 Weighing raw materials in 0.5 wt% of the total weight of the above components, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) putting the batch obtained in the step (1) into a corundum sagger, melting for 2 hours at 1600 ℃, cooling along with a furnace, taking out porous loose melt in the corundum sagger, putting the porous loose melt into a ball milling bottle of corundum medium or zirconia medium, performing roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain an intermediate;
(3) and (3) preserving the heat of the intermediate obtained in the step (2) at 1000 ℃ for 2 hours, cooling the intermediate along with a furnace, taking the intermediate out, putting the intermediate into a ball milling bottle of corundum medium or zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain leucite.
Example 3
A preparation method of green environment-friendly leucite comprises the following steps:
(1) the composition comprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 : 55.02 t%, the sum of the weight percentages of the components is 100%, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 TiO accounting for 6wt percent of the total weight of the components 2 0.5 wt% of the total weight of the foregoing components, B 2 O 3 Weighing raw materials in 0.5 wt% of the total weight of the above components, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) putting the batch mixture obtained in the step (1) into a corundum sagger, melting for 2 hours at 1600 ℃, cooling along with a furnace, taking out porous loose melt in the corundum sagger, putting the porous loose melt into a ball milling bottle of corundum medium or zirconia medium, performing roll milling, and performing ball milling and sieving by using industrial alcohol as a grinding aid to obtain an intermediate;
(3) and (3) preserving the heat of the intermediate obtained in the step (2) at 1100 ℃ for 2 hours, cooling the intermediate along with a furnace, taking the intermediate out, putting the intermediate into a ball milling bottle made of corundum medium or zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain leucite.
Example 4
A preparation method of green environment-friendly leucite comprises the following steps:
(1) the composition comprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 : 55.02 t%, the sum of the weight percentages of the components is 100%, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 7 wt% of the total weight of the aforementioned components, TiO 2 0.5 wt% of the total weight of the aforementioned components, B 2 O 3 Weighing raw materials in 0.5 wt% of the total weight of the above components, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) putting the batch obtained in the step (1) into a corundum sagger, melting for 2 hours at 1600 ℃, cooling along with a furnace, taking out porous loose melt in the corundum sagger, putting the porous loose melt into a ball milling bottle of corundum medium or zirconia medium, performing roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain an intermediate;
(3) and (3) preserving the heat of the intermediate obtained in the step (2) at 1200 ℃ for 2h, cooling along with the furnace, taking out, putting into a ball milling bottle of corundum medium or zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain leucite.
Example 5
A preparation method of green environment-friendly leucite comprises the following steps:
(1) the composition comprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 : 55.02 t%, the sum of the weight percentages of the components is 100%, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 4 wt% of the total weight of the aforementioned components, TiO 2 Is 0 of the total weight sum of the components.5wt％，B 2 O 3 Weighing the raw materials in 0.5 wt% of the total weight of the components, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) putting the batch mixture obtained in the step (1) into a corundum sagger, melting for 2 hours at 1500 ℃, cooling along with a furnace, taking out porous loose melt in the corundum sagger, putting the porous loose melt into a ball milling bottle of corundum medium or zirconia medium, performing roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain an intermediate;
(3) and (3) preserving the heat of the intermediate obtained in the step (2) at 900 ℃ for 2 hours, cooling along with a furnace, taking out, putting into a ball milling bottle of a corundum medium or a zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain leucite.
Example 6
A preparation method of green environment-friendly leucite comprises the following steps:
(1) the composition comprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 : 55.02 t%, the sum of the weight percentages of the components is 100%, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 5 wt% of the total weight of the aforementioned components, TiO 2 0.5 wt% of the total weight of the foregoing components, B 2 O 3 Weighing raw materials in 0.5 wt% of the total weight of the above components, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) putting the batch obtained in the step (1) into a corundum sagger, melting for 2 hours at 1500 ℃, cooling along with a furnace, taking out porous loose melt in the corundum sagger, putting the porous loose melt into a ball milling bottle of corundum medium or zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain an intermediate;
(3) and (3) preserving the heat of the intermediate obtained in the step (2) at 1000 ℃ for 2 hours, cooling along with a furnace, taking out, putting into a ball milling bottle of a corundum medium or a zirconia medium, performing roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain leucite.
Example 7
A preparation method of green environment-friendly leucite comprises the following steps:
(1) the composition comprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 : 55.02 t%, the sum of the weight percentages of the components is 100%, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 TiO accounting for 6wt percent of the total weight of the components 2 0.5 wt% of the total weight of the foregoing components, B 2 O 3 Weighing raw materials in 0.5 wt% of the total weight of the above components, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) putting the batch obtained in the step (1) into a corundum sagger, melting for 2 hours at 1500 ℃, cooling along with a furnace, taking out porous loose melt in the corundum sagger, putting the porous loose melt into a ball milling bottle of corundum medium or zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain an intermediate;
(3) and (3) preserving the heat of the intermediate obtained in the step (2) at 1100 ℃ for 2h, cooling along with a furnace, taking out, putting into a ball milling bottle of a corundum medium or a zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain leucite.
Example 8
A preparation method of green environment-friendly leucite comprises the following steps:
(1) according to the following weight percentageComprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 : 55.02 t%, the sum of the weight percentages of the components is 100%, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 7 wt% of the total weight of the aforementioned components, TiO 2 0.5 wt% of the total weight of the aforementioned components, B 2 O 3 Weighing the raw materials in 0.5 wt% of the total weight of the components, wherein K 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; then putting all the raw materials into a rapid grinding machine of a corundum medium or a zirconia medium, uniformly mixing, taking industrial alcohol as a grinding aid, and sieving by a 300-mesh sieve to obtain a batch;
(2) putting the batch obtained in the step (1) into a corundum sagger, melting for 2 hours at 1500 ℃, cooling along with a furnace, taking out porous loose melt in the corundum sagger, putting the porous loose melt into a ball milling bottle of corundum medium or zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain an intermediate;
(3) and (3) preserving the heat of the intermediate obtained in the step (2) at 1200 ℃ for 2h, cooling along with the furnace, taking out, putting into a ball milling bottle of corundum medium or zirconia medium for roll milling, taking industrial alcohol as a grinding aid, and performing ball milling and sieving to obtain leucite.
Table 1 case data integration
Figure BDA0003697541900000071
From the XRD patterns, it can be seen that the leucite prepared under the process conditions of example 1 has the best main crystal phase and the highest purity.

Claims (7)

1. A green environment-friendly leucite preparation method is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing raw materials according to the formula of the leucite, grinding uniformly, and sieving to obtain a batch;
(2) putting the batch obtained in the step (1) into a container for sintering, cooling, crushing and sieving to obtain an intermediate;
(3) and (3) putting the intermediate obtained in the step (2) into a container for heat treatment, cooling, crushing and sieving to obtain the leucite.
2. The method for preparing green environment-friendly leucite according to claim 1, characterized in that: the raw material of the step (1) comprises K 2 O、Al 2 O 3 Quartz powder and sintering aid Na 2 CO 3 、TiO 2 And B 2 O 3 。
3. The method for preparing green environment-friendly leucite according to claim 1, characterized in that: the formula of the leucite comprises the following components in percentage by weight: k 2 O21.58％，Al 2 O 3 23.40％，SiO 2 55.02 percent, the sum of the weight percent of the components is 100 percent, and Na is also added 2 CO 3 、TiO 2 And B 2 O 3 ，Na 2 CO 3 4-7 wt% of TiO, based on the total weight of the aforementioned components 2 0.5 wt% of the total weight of the aforementioned components, B 2 O 3 Is 0.5 wt% of the total weight of the components; wherein K is 2 O is represented by K 2 CO 3 Introduction of Al 2 O 3 From Al (OH) 3 Introducing; preferred is Na 2 CO 3 Is added in an amount of 5 wt% based on the sum of the aforementioned components.
4. The method for preparing green environment-friendly leucite according to claim 1, characterized in that: and (2) grinding the raw materials by adopting a quick grinding machine, wherein industrial alcohol is used as a grinding aid during grinding.
5. The method for preparing green environment-friendly leucite according to claim 1, characterized in that: the sieve used in the step (1) is 300 meshes.
6. The method for preparing environment-friendly leucite according to claim 1, wherein the method comprises the following steps: the sintering container in the step (2) is a corundum sagger, the sintering temperature is 1500-1600 ℃, and the melting time is 2 h; the cooling method is furnace cooling; the grinding method is that the sintered frit is put into a ball mill bottle of corundum medium or zirconia medium for roll milling, and industrial alcohol is used as a grinding aid; the sieved sieve is 300 meshes.
7. The method for preparing green environment-friendly leucite according to claim 1, characterized in that: the heat treatment container in the step (3) is a corundum sagger, the heat treatment temperature is 900-; the cooling method is furnace cooling; the grinding method comprises the steps of putting sintered frit into a ball milling bottle of corundum medium or zirconia medium for roll milling, and taking industrial alcohol as a grinding aid; the sieved sieve is 300 meshes.
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Application publication date: 20220909