CN110698188A - Method for preparing mullite powder from waste diatomite and mullite powder prepared based on method - Google Patents
Method for preparing mullite powder from waste diatomite and mullite powder prepared based on method Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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Abstract
The invention discloses a method for preparing mullite powder by using waste diatomite and the mullite powder prepared by the method, wherein the mullite powder is prepared by using the waste diatomite as a main raw material, adding a proper amount of solution containing aluminum ions and adopting a high-temperature self-propagating combustion method; the mullite powder is prepared by taking the waste diatomite as a main raw material, so that waste is changed into valuable, the waste diatomite is not a waste polluting the environment any more, and the mullite powder is a high-value resource and has obvious economic and social benefits; the preparation method is simple, and the obtained mullite powder is a nonmetal powder material with good crystallization performance, has good uniformity and small crystal grains, and can be widely applied to preparation of refractory materials and ceramic materials.
Description
Technical Field
The invention relates to the technical field of preparing ceramic powder materials by using solid wastes, in particular to a method for preparing mullite powder by using waste diatomite and the mullite powder prepared based on the method.
Background
Mullite (3 Al)2O3·2SiO2) Is Al2O3-SiO2The system is a unique and stable crystalline compound under normal pressure, has high refractoriness, good thermal shock resistance, chemical erosion resistance and creep resistance, high refractoriness under load, good volume stability, strong electrical insulation and the like, is an ideal high-grade refractory material, and is widely applied to the fields of metallurgy, glass, ceramics, chemistry, electric power, national defense and the like. However, natural mullite minerals are rare in nature, and industrial mullite is mainly usedAnd (4) artificial synthesis.
At present, the methods for synthesizing mullite for industrial use mainly include an electric melting method and a sintering method. The electric melting method is formed by melting the mixed raw materials in an electric arc, and has the defects of high power consumption and strict requirements on synthesis conditions; sintering processes are classified into inorganic silica-alumina gel processes, organic silica-alumina gel processes, and mineral phase change processes according to the nature of the raw materials used. Wherein, the inorganic silicon-aluminum gel method and the organic silicon-aluminum gel method are respectively prepared by adopting inorganic and organic raw materials according to certain chemical compositions and then are calcined at high temperature, and have the defects of higher energy consumption and expensive price of the organic raw materials used in the organic gel method; the mineral phase transition method is formed by placing natural minerals such as high bauxite, kaolin, pyrophyllite and the like in a kiln and calcining at high temperature, and has the defects of high energy consumption, low mullite conversion rate and resource waste due to the fact that the mineral composition of the mullite is greatly different from that of the mullite.
Diatomite is a natural mineral raw material deposited from dead bodies of ancient biological diatoms, has the characteristics of light weight, good chemical stability, high porosity, wear resistance, acid resistance, heat resistance, strong adsorbability and the like, is used as a filter aid, a filling agent, a catalyst carrier and the like, and is widely applied to various industrial departments. A large amount of diatomite loses activity after being used and is stacked near a factory building or in a drainage ditch, so that the environment is polluted, and the renewable resources which can be used are wasted. Therefore, it is an important content of the present invention to research a method for preparing mullite powder from waste diatomite.
Disclosure of Invention
The invention aims to provide a method for preparing mullite powder by using waste diatomite and mullite prepared based on the method, aiming at solving the problems that the mullite synthesized by using a capacitance method at present has large power consumption and strict requirements on synthesis conditions, and a sintering method has high energy consumption, high cost, low mullite conversion rate and the like.
In order to realize the purpose, the invention is realized by the following technical scheme:
the mullite powder provided by the invention is prepared by taking waste diatomite as a main raw material, adding a proper amount of solution containing aluminum ions and adopting a high-temperature self-propagating combustion method.
Preferably, the mass ratio of the silicon element in the waste diatomite to the aluminum ion added in the aluminum ion solution is 1: 3.
The invention relates to a method for preparing mullite powder by using waste diatomite, which comprises the following steps:
(1) mixing waste diatomite and a solution containing aluminum ions, wherein the mass ratio of silicon elements in the waste diatomite to substances added with the aluminum ions in the aluminum ion solution is 1:3, putting the mixture into a planetary ball mill for wet ball milling, controlling the ball-material ratio of grinding balls to raw materials to be 2 ~ 3:1, controlling the rotating speed to be 300r/min, and ball milling for 4h 4 ~ 6h to obtain slurry;
(2) adding fuel into the slurry, stirring, transferring into a heating furnace at 500 ~ 800 deg.C, igniting, and burning to obtain fluffy powder;
(3) and (3) carrying out heat treatment on the fluffy powder for 2 ~ 4h at 1200 ~ 1350 ℃ in an air atmosphere to obtain the mullite powder.
Preferably, the solution containing aluminum ions in the present invention is obtained by dissolving one or more of aluminum nitrate or aluminum sulfate or aluminum chloride in water.
Preferably, the fuel in the present invention is one or more of urea or citric acid or ethanol.
Preferably, the fluffy powder is heat treated at 1350 ℃ for 3h in an air atmosphere.
The invention has the beneficial effects that:
(1) the mullite powder is prepared by taking the waste diatomite as a main raw material, so that waste is changed into valuable, the waste diatomite is not a waste polluting the environment any more, and the mullite powder is a high-value resource and has obvious economic and social benefits.
(2) The mullite powder prepared by the method is a nonmetal powder material with good crystallization performance, and can be widely applied to preparation of refractory materials and ceramic materials.
(3) The invention adopts a high-temperature self-propagating combustion method, utilizes the characteristic that the waste diatomite contains high grease and organic matters, and additionally adds fuel, so that once the waste diatomite is ignited under the low-temperature condition, the heat generated by combustion is enough to maintain the combustion, and the waste diatomite does not need to be heated by an additional heat source. The heat released by continuous self-propagating combustion is utilized to enable the silicon source and the aluminum source to react to generate mullite, so that the method not only saves energy, but also has the advantages of high reaction speed, low reaction temperature, capability of being carried out under normal pressure and the like.
Drawings
FIG. 1 is a microscopic topography of waste diatomaceous earth;
FIG. 2 is an XRD spectrum of waste diatomaceous earth;
FIG. 3 is an XRD pattern of mullite powder prepared in example 1 of the present invention;
FIG. 4 is a microscopic morphology of mullite powder prepared in example 1 of the present invention;
FIG. 5 is an XRD pattern of mullite powder prepared in example 2 of the present invention;
FIG. 6 is an XRD pattern of mullite powder prepared in example 3 of the present invention;
fig. 7 is an XRD pattern of mullite powder prepared in example 4 of the present invention.
Detailed Description
Example 1
The mullite powder is prepared by taking waste diatomite as a main raw material, adding a proper amount of aluminum chloride solution and adopting a high-temperature self-propagating combustion method.
Preferably, the mass ratio of the silicon element in the waste diatomite to the aluminum ion added in the aluminum ion solution is 1: 3.
The method for preparing mullite powder by using waste diatomite comprises the following steps:
(1) weighing 4.0g of waste diatomite, mixing the waste diatomite with 120mL of 1mol/L aluminum chloride solution, putting the mixture into a planetary ball mill for wet ball milling, controlling the rotating speed to be 300r/min, controlling the ball-material ratio of a grinding ball to the mixture to be 3:1, and ball milling for 6 hours to obtain slurry;
(2) adding 1.0g of urea fuel into the slurry, fully stirring, transferring into a heating furnace at the temperature of 600 ℃ for ignition, and obtaining fluffy powder after the combustion is finished;
(3) and (3) carrying out heat treatment on the fluffy powder for 3h under the air atmosphere of 1350 ℃, washing the mullite powder for 1h by using distilled water, and filtering and drying to obtain the mullite powder.
The raw material, namely the waste diatomaceous earth, of this example was subjected to microscopic morphology observation and XRD analysis, referring to FIGS. 1 and 2, it can be seen from FIG. 1 that the waste diatomaceous earth had an irregular lamellar structure with a lamellar particle size of about 1 ~ 3 μm, and it can be seen from FIG. 2 that diatomaceous earth has a main crystal phase of quartz and also contains a small amount of amorphous SiO2. The mullite powder obtained in this example was subjected to XRD analysis, and the obtained result is shown in fig. 3. As can be seen from FIG. 3, the main crystal phase of the product obtained in this example is mullite, and a small amount of impurity peaks are corundum, which indicates that the waste diatomite is converted into mullite after reaction. The microstructure of the product was further observed, and as a result, as shown in fig. 4, it can be seen that the nano-sized short rod-shaped mullite grains, which are uniform in grain size and well crystallized, are the best embodiment of the present invention.
Example 2
The mullite powder is prepared by taking waste diatomite as a main raw material, adding a proper amount of aluminum sulfate solution and adopting a high-temperature self-propagating combustion method.
Preferably, the mass ratio of the silicon element in the waste diatomite to the aluminum ion added in the aluminum ion solution is 1: 3.
The method for preparing mullite powder by using waste diatomite comprises the following steps:
(1) weighing 4.0g of waste diatomite, mixing the waste diatomite with 60mL of 1mol/L aluminum sulfate solution, putting the mixture into a planetary ball mill for wet ball milling, controlling the rotating speed to be 300r/min, controlling the ball-material ratio of a milling ball to the mixture to be 2:1, and obtaining slurry after ball milling for 4 hours;
(2) adding 1.0g of citric acid fuel into the slurry, fully stirring, transferring into a heating furnace at 700 ℃ for ignition, and obtaining fluffy powder after the combustion is finished;
(3) and (3) carrying out heat treatment on the fluffy powder for 3h under the atmospheric pressure at 1300 ℃ in the air atmosphere, washing the mullite powder for 1h by using distilled water, and filtering and drying to obtain the mullite powder.
The mullite powder obtained in this example was subjected to XRD analysis, and the obtained result is shown in fig. 5. As can be seen from fig. 5, the mullite crystal phase appears in the product, but a portion of the silica and alumina phases remain. This is due to the fact that at lower calcination temperatures, the reaction does not proceed sufficiently and the mullite yield decreases.
Example 3
The mullite powder is prepared by taking waste diatomite as a main raw material, adding a proper amount of aluminum nitrate solution and adopting a high-temperature self-propagating combustion method.
Preferably, the mass ratio of the silicon element in the waste diatomite to the aluminum ion added in the aluminum ion solution is 1: 3.
The method for preparing mullite powder by using waste diatomite comprises the following steps:
(1) weighing 4.0g of waste diatomite, mixing the waste diatomite with 120mL of 1mol/L aluminum nitrate solution, putting the mixture into a planetary ball mill for wet ball milling, controlling the rotating speed to be 300r/min, controlling the ball-material ratio of a grinding ball to the mixture to be 3:1, and ball milling for 5 hours to obtain slurry;
(2) adding 20.0mL of ethanol fuel into the slurry, fully stirring, transferring into a heating furnace at 500 ℃ for ignition, and obtaining fluffy powder after the combustion is finished;
(3) and (3) carrying out heat treatment on the fluffy powder for 4h under the atmospheric pressure at the temperature of 1200 ℃ in the air atmosphere, washing the mullite powder for 1h by using distilled water, and filtering and drying to obtain the mullite powder.
The mullite powder obtained in this example was subjected to XRD analysis, and the obtained result is shown in fig. 6. As can be seen from fig. 6, a portion of the mullite crystalline phase begins to appear in the product, but silica and alumina phases are present. This is because at lower calcination temperatures, the reaction does not proceed sufficiently and the mullite yield is lower.
Example 4
In the mullite powder of the embodiment, the mullite powder is prepared by using waste diatomite as a main raw material and adding a proper amount of aluminum chloride solution and adopting a high-temperature self-propagating combustion method.
Preferably, the mass ratio of the silicon element in the waste diatomite to the aluminum ion added in the aluminum ion solution is 1: 3.
The method for preparing mullite powder by using waste diatomite comprises the following steps:
(1) weighing 4.0g of waste diatomite, mixing the waste diatomite with 120mL of 1mol/L aluminum chloride solution, putting the mixture into a planetary ball mill for wet ball milling, controlling the rotating speed to be 250r/min, controlling the ball-material ratio of a grinding ball to the mixture to be 3:1, and ball milling for 5 hours to obtain slurry;
(2) adding 0.5g of urea and 10mL of ethanol fuel into the slurry, fully stirring, transferring into a heating furnace with the temperature of 500 ℃ for ignition, and obtaining fluffy powder after the combustion is finished;
(3) and (3) carrying out heat treatment on the fluffy powder for 3h under the atmospheric pressure at 1150 ℃ in the air atmosphere, washing the mullite powder for 1h by using distilled water, and filtering and drying to obtain the mullite powder.
The mullite powder obtained in this example was subjected to XRD analysis, and the obtained result is shown in fig. 7. As can be seen from fig. 7, a portion of the mullite crystalline phase begins to appear in the product, but a significant amount of silica and alumina phases are present. At lower calcination temperatures, the reaction just started and the mullite phase began to appear.
Claims (6)
1. A mullite powder is characterized in that: the mullite powder is prepared by taking waste diatomite as a main raw material, adding a proper amount of solution containing aluminum ions and adopting a high-temperature self-propagating combustion method.
2. The mullite powder of claim 1, wherein: the mass ratio of the silicon element in the waste diatomite to the aluminum ion added in the aluminum ion solution is 1: 3.
3. A method for preparing mullite powder by using waste diatomite is characterized by comprising the following steps:
(1) mixing waste diatomite and a solution containing aluminum ions, wherein the mass ratio of silicon elements in the waste diatomite to substances added with the aluminum ions in the aluminum ion solution is 1:3, putting the mixture into a planetary ball mill for wet ball milling, controlling the ball-material ratio of grinding balls to raw materials to be 2 ~ 3:1, controlling the rotating speed to be 300r/min, and ball milling for 4h 4 ~ 6h to obtain slurry;
(2) adding fuel into the slurry, stirring, transferring into a heating furnace at 500 ~ 800 deg.C, igniting, and burning to obtain fluffy powder;
(3) and (3) carrying out heat treatment on the fluffy powder for 2 ~ 4h at 1200 ~ 1350 ℃ in an air atmosphere to obtain the mullite powder.
4. The method for preparing mullite powder from waste diatomite as claimed in claim 3, wherein the method comprises the following steps: the solution containing aluminum ions is obtained by dissolving one or more of aluminum nitrate or aluminum sulfate or aluminum chloride in water.
5. The method for preparing mullite powder from waste diatomite as claimed in claim 3, wherein the method comprises the following steps: the fuel is one or more of urea, citric acid or ethanol.
6. The method for preparing mullite powder from waste diatomite as claimed in claim 3, wherein the method comprises the following steps: the fluffy powder is subjected to heat treatment for 3 hours at 1350 ℃ in an air atmosphere.
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