CN109942012B - Nanoscale flaky boehmite and preparation method thereof - Google Patents
Nanoscale flaky boehmite and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of inorganic nano materials, and particularly relates to nano flaky boehmite, and further discloses a preparation method of the nano flaky boehmite. The preparation method of the nanoscale flaky boehmite takes an aluminum salt material as an aluminum source raw material, takes ammonia water as a precipitator to carry out bidirectional precipitation, and carries out hydrothermal synthesis treatment on the prepared precursor slurry, so that the prepared boehmite is in a nanoscale flaky structure. The method for preparing the nano-scale flaky boehmite can realize the preparation of the boehmite under the condition of not adding a surfactant or a template agent, has the advantages of simple process, safety and low cost, and is suitable for large-scale industrial production. The nanoscale flaky boehmite prepared by the method has the advantages of regular flaky shape, high crystallinity, good dispersibility and narrow particle size distribution, and has wider application prospect.
Description
Technical Field
The invention belongs to the technical field of inorganic nano materials, and particularly relates to nano flaky boehmite, and further discloses a preparation method of the nano flaky boehmite.
Background
Boehmite (Boehmite), also known as Boehmite or Boehmite, has a chemical formula of gamma-Al2O3·H2O or gamma-AlOOH. The gamma-AlOOH is composed of a plurality of AlOs6The octahedron is composed of Al in the center of the octahedron and O at the vertex of the octahedron, and the octahedron forms a double chain through coplane and then forms a three-dimensional framework structure by sharing the vertex. Gamma-AlOOH belongs to an orthorhombic system, is a layered structure, and is widely applied to the fields of ceramic materials, optical materials, semiconductor materials, composite materials, catalysts, carrier materials and coatings by virtue of unique mechanical, chemical and optical properties.
In the prior art, boehmite is prepared by a plurality of methods, which mainly comprise a precipitation method (acid and alkali precipitation), a carbonization method, an aluminum alkoxide hydrolysis method, a hydrothermal method, a sol-gel method, an ionic liquid method, a hard template method and the like. Boehmite with various shapes such as wrinkled sheet, needle, chain, boat, cube, diamond sheet and the like and different grain sizes is prepared by different methods in Stiles et al (Stiles A B. catalyst Supports and Supported catalysts. Theroretic and Applied Concepts [ M ]. USA: Butterworth, Boston, Mass, 1987: 158-; and Liu et al (Qian Liu, Aiqin, Wang, Xiaoodong, Wang, Tao Zhuang. Morphologica controlled synthesis of meso pore aluminum, micro pore and meso pore Materials, 100(2007)35-44.) various Mesoporous aluminas with special morphologies, including spherical, bone, rod, fiber, 3D dumbbell, were synthesized using different surfactants in combination with hydrothermal method using aluminum nitrate as aluminum source, ammonia and urea as precipitants.
However, although the above methods can prepare boehmites with different morphologies, each preparation method requires the addition of a large amount of surfactant or template, which not only increases the production cost due to high price, but also has a certain toxicity, and is not suitable for large-scale industrial production.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide nanoscale flaky boehmite, which has the advantages of regular flaky shape, high crystallinity, good dispersibility and narrow particle size distribution;
the second technical problem to be solved by the present invention is to provide the method for preparing the nano-scale sheet boehmite, wherein the method can realize the preparation of boehmite without adding a surfactant/template, has the advantages of simple process, safety and low cost, and is suitable for large-scale industrial production.
In order to solve the technical problems, the preparation method of the nanoscale flaky boehmite comprises the following steps:
(1) preparing an aluminum source material to obtain an aluminum salt solution, adding a precipitator to carry out bidirectional precipitation, and adjusting the pH value of the system to be more than 11 to obtain precursor slurry; continuously washing the obtained precursor slurry to remove impurity ions in the solution;
(2) spray drying the washed precursor slurry, and carrying out high-temperature calcination treatment on the obtained powder;
(3) and (3) performing dispersion treatment on the calcined powder, performing hydrothermal synthesis reaction at the temperature of 150-250 ℃, and drying the obtained reactant slurry to obtain the catalyst.
In the step (1), the aluminum source material includes aluminum nitrate and/or aluminum sulfate.
In the step (1), the concentration of the aluminum salt solution is 0.5mol/L-10 mol/L.
In the step (1), the precipitant includes ammonia water.
Preferably, the mass concentration of the ammonia water is 20-30 wt%.
In the step (1), the continuous washing step is continuous washing by ceramic membrane washing equipment. In the washing process, the water flux is controlled to be 10-1000kg/h, and the washing pressure is controlled to be 0.1-1.5 Mpa.
In the step (2), in the spray drying step, the solid content of the feed of the spray dryer is controlled to be 20-30%, and the outlet temperature is controlled to be 120-150 ℃.
In the step (2), the temperature of the calcination step is 400-600 ℃.
In the step (3), the dispersion step adopts a planetary mill for dispersion, the solid content is controlled to be 40 +/-5%, and the rotating speed is 300 +/-20 r/1 h.
The invention also discloses the nanoscale flaky boehmite prepared by the method.
The preparation method of the nanoscale flaky boehmite takes an aluminum salt material as an aluminum source raw material, takes ammonia water as a precipitator to carry out bidirectional precipitation, and carries out hydrothermal synthesis treatment on the prepared precursor slurry, so that the prepared boehmite is in a nanoscale flaky structure. The method for preparing the nano-scale flaky boehmite can realize the preparation of the boehmite under the condition of not adding a surfactant or a template agent, has the advantages of simple process, safety and low cost, and is suitable for large-scale industrial production.
The nanoscale flaky boehmite prepared by the method has the advantages of regular flaky shape, high crystallinity, good dispersibility and narrow particle size distribution, and has wider application prospect.
Drawings
In order that the present disclosure may be more readily and clearly understood, the following detailed description of the present disclosure is provided in connection with specific embodiments thereof and the accompanying drawings, in which,
FIG. 1 is a scanning electron micrograph of a nanoscale, flaky boehmite sample prepared according to example 1 of the present invention;
figure 2 is an XRD pattern of a sample of nano-scale flaky boehmite prepared according to example 1 of the present invention.
Detailed Description
Example 1
The preparation method of nanoscale flaky boehmite described in this example includes the following steps:
(1) taking aluminum nitrate as an aluminum source material, adding water to prepare an aluminum nitrate solution with the concentration of 0.5mol/L, adding ammonia water with the mass concentration of 30 wt% as a precipitator to perform bidirectional precipitation treatment until precipitation is not increased any more, and adjusting the pH value of a reaction system to 11.5 to obtain precursor slurry; continuously washing the obtained precursor slurry by ceramic membrane washing equipment, controlling the water flux in the washing process to be 10-1000kg/h and the washing pressure to be 0.1-1.5Mpa so as to remove impurity ions in the solution until the concentration of the impurity ions in the solution is less than 600 ppm;
(2) carrying out spray drying treatment on the washed precursor slurry by using a spray dryer, controlling the solid content of the feed of the spray dryer to be 20-30%, and controlling the outlet temperature to be 120-; then, carrying out high-temperature calcination treatment on the obtained powder at 500 ℃ to obtain calcined powder;
(3) dispersing the calcined powder by adopting a planetary mill, and controlling the solid content to be 40 +/-5% and the rotating speed to be 300 +/-20 r/1 h; and then placing the dispersed powder in a synthesis kettle, controlling the filling degree to be 70-80%, adding water at 200 ℃ to perform hydrothermal synthesis (controlling the reaction temperature rise speed to be 3 ℃/min) to react for 6h, and performing spray drying treatment on the obtained reactant slurry (controlling the inlet temperature to be 270 ℃, the outlet temperature to be 120 ℃ and the rotation speed of an atomizing disc to be 8000r/min), thus obtaining the catalyst.
The scanning electron micrograph of the boehmite sample prepared in this example is shown in fig. 1, and it can be seen that the boehmite prepared by the method of this example has a lamellar structure, and is shown as a boehmite phase through the XRD pattern analysis shown in fig. 2, and the particle size is in the nanometer level.
Example 2
The preparation method of nanoscale flaky boehmite described in this example includes the following steps:
(1) taking aluminum sulfate as an aluminum source material, adding water to prepare an aluminum sulfate solution with the concentration of 2mol/L, adding ammonia water (with the mass concentration of 30 wt%) as a precipitator to carry out bidirectional precipitation treatment until precipitation is not increased any more, and adjusting the pH value of a reaction system to be 12.2 to obtain precursor slurry; continuously washing the obtained precursor slurry by ceramic membrane washing equipment, controlling the water flux in the washing process to be 10-1000kg/h and the washing pressure to be 0.1-1.5Mpa so as to remove impurity ions in the solution until the concentration of the impurity ions in the solution is less than 600 ppm;
(2) carrying out spray drying treatment on the washed precursor slurry by using a spray dryer, controlling the solid content of the feed of the spray dryer to be 20-30%, and controlling the outlet temperature to be 120-; then, carrying out high-temperature calcination treatment on the obtained powder at 400 ℃ to obtain calcined powder;
(3) dispersing the calcined powder by adopting a planetary mill, and controlling the solid content to be 40 +/-5% and the rotating speed to be 300 +/-20 r/1 h; and then placing the dispersed powder in a synthesis kettle, controlling the filling degree to be 70-80%, adding water at 150 ℃ for hydro-thermal synthesis (controlling the heating rate to be 3 ℃/min) for reaction for 6h, and performing spray drying treatment on the obtained reactant slurry, wherein the inlet temperature is controlled to be 270 ℃, the outlet temperature is controlled to be 120 ℃, and the rotating speed of an atomizing disc is 8000r/min, so as to obtain the nano-composite powder.
The boehmite samples produced in this example were determined to have platelet structures and particle sizes on the order of nanometers.
Example 3
The preparation method of nanoscale flaky boehmite described in this example includes the following steps:
(1) taking aluminum nitrate as an aluminum source material, adding water to prepare an aluminum nitrate solution with the concentration of 4mol/L, adding ammonia water with the mass concentration of 25 wt% as a precipitator to perform bidirectional precipitation treatment until precipitation is not increased, and adjusting the pH value of a reaction system to be 13 to obtain precursor slurry; continuously washing the obtained precursor slurry by ceramic membrane washing equipment, controlling the water flux in the washing process to be 10-1000kg/h and the washing pressure to be 0.1-1.5Mpa so as to remove impurity ions in the solution until the concentration of the impurity ions in the solution is less than 600 ppm;
(2) carrying out spray drying treatment on the washed precursor slurry by using a spray dryer, controlling the solid content of the feed of the spray dryer to be 20-30%, and controlling the outlet temperature to be 120-; then, carrying out high-temperature calcination treatment on the obtained powder at 600 ℃ to obtain calcined powder;
(3) dispersing the calcined powder by adopting a planetary mill, and controlling the solid content to be 40 +/-5% and the rotating speed to be 300 +/-20 r/1 h; and then placing the dispersed powder in a synthesis kettle, controlling the filling degree to be 70-80%, adding water at 250 ℃ to perform a hydrothermal synthesis reaction for 8 hours, and performing spray drying treatment on the obtained reactant slurry, wherein the inlet temperature is controlled to be 270 ℃, the outlet temperature is controlled to be 120 ℃, and the rotating speed of an atomizing disc is controlled to be 8000r/min, so as to obtain the catalyst.
The boehmite samples produced in this example were determined to have platelet structures and particle sizes on the order of nanometers.
Example 4
The preparation method of nanoscale flaky boehmite described in this example includes the following steps:
(1) taking aluminum sulfate as an aluminum source material, adding water to prepare an aluminum sulfate solution with the concentration of 6mol/L, adding ammonia water with the mass concentration of 20 wt% as a precipitator to carry out bidirectional precipitation treatment until precipitation is not increased, and adjusting the pH value of a reaction system to be 13.5 to obtain precursor slurry; continuously washing the obtained precursor slurry by ceramic membrane washing equipment, controlling the water flux in the washing process to be 10-1000kg/h and the washing pressure to be 0.1-1.5Mpa so as to remove impurity ions in the solution until the concentration of the impurity ions in the solution is less than 600 ppm;
(2) carrying out spray drying treatment on the washed precursor slurry by using a spray dryer, controlling the solid content of the feed of the spray dryer to be 20-30%, and controlling the outlet temperature to be 120-; then, carrying out high-temperature calcination treatment on the obtained powder at 400 ℃ to obtain calcined powder;
(3) dispersing the calcined powder by adopting a planetary mill, and controlling the solid content to be 40 +/-5% and the rotating speed to be 300 +/-20 r/1 h; and then placing the dispersed powder in a synthesis kettle, controlling the filling degree to be 70-80%, adding water at 150 ℃ to perform a hydrothermal synthesis reaction for 8 hours, and performing spray drying treatment on the obtained reactant slurry, wherein the inlet temperature is controlled to be 270 ℃, the outlet temperature is controlled to be 120 ℃, and the rotating speed of an atomizing disc is controlled to be 8000r/min, so as to obtain the catalyst.
The boehmite samples produced in this example were determined to have platelet structures and particle sizes on the order of nanometers.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (6)
1. A preparation method of nanoscale flaky boehmite is characterized by comprising the following steps:
(1) preparing an aluminum source material to obtain an aluminum salt solution, adding a precipitator to carry out bidirectional precipitation, and adjusting the pH value of the system to be more than 11 to obtain precursor slurry; continuously washing the obtained precursor slurry to remove impurity ions in the solution, wherein the aluminum source material comprises aluminum nitrate and/or aluminum sulfate, and the precipitator comprises ammonia water;
(2) spray drying the washed precursor slurry, and performing high-temperature calcination treatment on the obtained powder, wherein the temperature of the calcination step is 400-600 ℃;
(3) and dispersing the calcined powder by adopting a planetary mill, carrying out hydrothermal synthesis reaction at the temperature of 150-250 ℃, and drying the obtained reactant slurry to obtain the catalyst.
2. The method for producing nanoscale, sheet-like boehmite according to claim 1, characterized in that in the step (1), the concentration of the aluminum salt solution is 0.5mol/L to 10 mol/L.
3. The method for producing nanoscale flaky boehmite according to claim 1, characterized in that the mass concentration of aqueous ammonia is 20 to 30 wt%.
4. The method for producing nanoscale flaky boehmite according to any one of claims 1-3, characterized in that in step (1), the continuous washing step is continuous washing by a ceramic membrane washing apparatus.
5. The method for producing nanoscale flaky boehmite according to any one of claims 1-3, characterized in that in the step (2), in the spray-drying step, the feed solid content of a spray-dryer is controlled to be 20-30%, and the outlet temperature is controlled to be 120-150 ℃.
6. Nanoscale, flaky boehmite produced by the method according to any one of claims 1-5.
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