Disclosure of Invention
The invention solves the technical problem of providing a preparation method of a lanthanum carbonate micro-nano material with a multi-core nested structure, which is simple to operate, green, mild, economical and environment-friendly.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the lanthanum carbonate micro-nano material with the multi-core nested structure is characterized by comprising the following specific steps:
step S1: dissolving 4-8g of sugar source in 30mL of secondary water, and magnetically stirring for 20min to form a solution, wherein the sugar source is galactose, lactose, sucrose or maltose;
step S2: dissolving 0.01-0.04mol of lanthanum source in 20mL of secondary water, adding the solution obtained in the step S1 after magnetic stirring for 20min, and magnetically stirring for 10-30min, wherein the lanthanum source is lanthanum chloride or lanthanum sulfate;
step S3: adding 0.1-0.5g of urea into the solution obtained in the step S2, magnetically stirring for 30min, then performing ultrasonic treatment for 10-30min, transferring into a 100mL polytetrafluoroethylene reaction kettle, heating to 180 ℃ at a heating rate of 5 ℃/min, keeping for 12-15h, then naturally cooling to room temperature, centrifugally washing, and drying at 80 ℃ for 12h to obtain a compound of carbon spheres and lanthanum ions;
step S4: and (4) grinding the compound of the carbon spheres and the lanthanum ions obtained in the step (S3), heating to 500-550 ℃ at the heating rate of 1-5 ℃/min in the air atmosphere, calcining for 3h, and naturally cooling to room temperature to obtain the lanthanum carbonate micro-nano material with the multi-core nested structure.
The lanthanum carbonate micro-nano material with the multi-core nested structure has 2-3 cores, the multi-core is formed by self-assembling small nano-particles, and the average particle size of the lanthanum carbonate micro-nano material with the multi-core nested structure is 2-3 mu m.
The invention has the following beneficial effects: (1) the method has the advantages of simple experimental operation, mild conditions and environmental protection; (2) the method has low reaction cost, the shape structure of the synthesized sample has certain controllability, and the urea is added so that the synthesized sample is easier to self-assemble to generate a multi-core structure under the calcining condition; (3) the lanthanum carbonate micro-nano material with the multi-core nested structure has larger specific surface area and abundant active sites, so that the lanthanum carbonate micro-nano material has good application prospect in the aspect of sewage treatment.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
Step S1: dissolving 4g of galactose in 30mL of secondary water, and magnetically stirring for 20min to form a solution;
step S2: dissolving 0.01mol of lanthanum chloride in 20mL of secondary water, magnetically stirring for 20min, adding the solution obtained in the step S1, and magnetically stirring for 10 min;
step S3: adding 0.1g of urea into the solution obtained in the step S2, magnetically stirring for 30min, then performing ultrasonic treatment for 10min, transferring the solution into a 100mL polytetrafluoroethylene reaction kettle, heating to 180 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 12h, naturally cooling to room temperature, centrifugally washing, and drying at 80 ℃ for 12h to obtain a compound of carbon spheres and lanthanum ions;
step S4: and (4) grinding the compound of the carbon spheres and the lanthanum ions obtained in the step (S3), heating to 500 ℃ at a heating rate of 1 ℃/min in an air atmosphere, calcining for 3h, and naturally cooling to room temperature to obtain the lanthanum carbonate micro-nano material with the multi-core nested structure.
Fig. 1 is a TEM image of the lanthanum carbonate micro-nano material with a multi-core nested structure prepared in this embodiment, and it can be known from the TEM image that the number of multi-core in the lanthanum carbonate micro-nano material with a multi-core nested structure is 3, the multi-core is formed by self-assembling small nanoparticles, and the average particle size of the lanthanum carbonate micro-nano material with a multi-core nested structure is 2-3 μm.
Example 2
Step S1: dissolving 5g of galactose in 30mL of secondary water, and magnetically stirring for 20min to form a solution;
step S2: dissolving 0.02mol of lanthanum chloride in 20mL of secondary water, magnetically stirring for 20min, adding the solution obtained in the step S1, and magnetically stirring for 10 min;
step S3: adding 0.2g of urea into the solution obtained in the step S2, magnetically stirring for 30min, then performing ultrasonic treatment for 10min, transferring the solution into a 100mL polytetrafluoroethylene reaction kettle, heating to 180 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 12h, naturally cooling to room temperature, centrifugally washing, and drying at 80 ℃ for 12h to obtain a compound of carbon spheres and lanthanum ions;
step S4: and (4) grinding the compound of the carbon spheres and the lanthanum ions obtained in the step (S3), heating to 500 ℃ at a heating rate of 1 ℃/min in an air atmosphere, calcining for 3h, and naturally cooling to room temperature to obtain the lanthanum carbonate micro-nano material with the multi-core nested structure.
Example 3
Step S1: dissolving 4g of lactose in 30mL of secondary water, and magnetically stirring for 20min to form a solution;
step S2: dissolving 0.02mol of lanthanum chloride in 20mL of secondary water, magnetically stirring for 20min, adding the solution obtained in the step S1, and magnetically stirring for 10 min;
step S3: adding 0.4g of urea into the solution obtained in the step S2, magnetically stirring for 30min, then performing ultrasonic treatment for 10min, transferring the solution into a 100mL polytetrafluoroethylene reaction kettle, heating to 180 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 13h, naturally cooling to room temperature, centrifugally washing, and drying at 80 ℃ for 12h to obtain a compound of carbon spheres and lanthanum ions;
step S4: and (4) grinding the compound of the carbon spheres and the lanthanum ions obtained in the step (S3), heating to 500 ℃ at a heating rate of 3 ℃/min in an air atmosphere, calcining for 3h, and naturally cooling to room temperature to obtain the lanthanum carbonate micro-nano material with the multi-core nested structure.
Example 4
Step S1: dissolving 7g of lactose in 30mL of secondary water, and magnetically stirring for 20min to form a solution;
step S2: dissolving 0.03mol of lanthanum sulfate in 20mL of secondary water, magnetically stirring for 20min, adding the solution obtained in the step S1, and magnetically stirring for 20 min;
step S3: adding 0.4g of urea into the solution obtained in the step S2, magnetically stirring for 30min, then performing ultrasonic treatment for 20min, transferring the solution into a 100mL polytetrafluoroethylene reaction kettle, heating to 180 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 13h, naturally cooling to room temperature, centrifugally washing, and drying at 80 ℃ for 12h to obtain a compound of carbon spheres and lanthanum ions;
step S4: and (4) grinding the compound of the carbon spheres and the lanthanum ions obtained in the step (S3), heating to 550 ℃ at a heating rate of 3 ℃/min in an air atmosphere, calcining for 3h, and naturally cooling to room temperature to obtain the lanthanum carbonate micro-nano material with the multi-core nested structure.
Example 5
Step S1: dissolving 7g of sucrose in 30mL of secondary water, and magnetically stirring for 20min to form a solution;
step S2: dissolving 0.035mol of lanthanum sulfate in 20mL of secondary water, magnetically stirring for 20min, adding into the solution obtained in the step S1, and magnetically stirring for 30 min;
step S3: adding 0.45g of urea into the solution obtained in the step S2, magnetically stirring for 30min, then performing ultrasonic treatment for 10min, transferring the solution into a 100mL polytetrafluoroethylene reaction kettle, heating to 180 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 14h, naturally cooling to room temperature, centrifugally washing, and drying at 80 ℃ for 12h to obtain a compound of carbon spheres and lanthanum ions;
step S4: and (4) grinding the compound of the carbon spheres and the lanthanum ions obtained in the step (S3), heating to 550 ℃ at a heating rate of 5 ℃/min in an air atmosphere, calcining for 3h, and naturally cooling to room temperature to obtain the lanthanum carbonate micro-nano material with the multi-core nested structure.
Example 6
Step S1: dissolving 8g of maltose in 30mL of secondary water, and magnetically stirring for 20min to form a solution;
step S2: dissolving 0.04mol of lanthanum sulfate in 20mL of secondary water, magnetically stirring for 20min, adding the solution obtained in the step S1, and magnetically stirring for 30 min;
step S3: adding 0.5g of urea into the solution obtained in the step S2, magnetically stirring for 30min, then performing ultrasonic treatment for 30min, transferring the solution into a 100mL polytetrafluoroethylene reaction kettle, heating to 180 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 15h, naturally cooling to room temperature, centrifugally washing, and drying at 80 ℃ for 12h to obtain a compound of carbon spheres and lanthanum ions;
step S4: and (4) grinding the compound of the carbon spheres and the lanthanum ions obtained in the step (S3), heating to 550 ℃ at a heating rate of 5 ℃/min in an air atmosphere, calcining for 3h, and naturally cooling to room temperature to obtain the lanthanum carbonate micro-nano material with the multi-core nested structure.
The embodiment of the preparation method of the lanthanum carbonate micro-nano material with the multi-core nested structure is introduced in detail and the basic principle, the main characteristics and the advantages of the invention are described. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, and that several variations and modifications of the present invention are possible without departing from the scope of the principles of the present invention, and that such variations and modifications are within the scope of the invention as expressed in the appended claims.