CN109809464B - Preparation method of lanthanum carbonate micro-nano material with multi-core nested structure - Google Patents
Preparation method of lanthanum carbonate micro-nano material with multi-core nested structure Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 35
- 229910017569 La2(CO3)3 Inorganic materials 0.000 title claims abstract description 32
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 title claims abstract description 32
- 229960001633 lanthanum carbonate Drugs 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 27
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 9
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims abstract 3
- 238000003756 stirring Methods 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims description 5
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical group Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 4
- 229930182830 galactose Natural products 0.000 claims description 4
- 239000008101 lactose Substances 0.000 claims description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 3
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical group OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 8
- 238000005406 washing Methods 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 2
- 241000143432 Daldinia concentrica Species 0.000 abstract 2
- 150000001875 compounds Chemical class 0.000 description 14
- 238000001816 cooling Methods 0.000 description 14
- 238000000227 grinding Methods 0.000 description 7
- 238000009210 therapy by ultrasound Methods 0.000 description 7
- 238000003917 TEM image Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000002149 hierarchical pore Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- Manufacturing Of Micro-Capsules (AREA)
- Catalysts (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明公开了一种具有多核嵌套结构的碳酸镧微纳米材料的制备方法，将糖源溶于二次水中，磁力搅拌形成溶液；将镧源溶于二次水中，磁力搅拌后加入到上述溶液中；再在得到的溶液中加入尿素，磁力搅拌后超声，转入聚四氟乙烯反应釜中，以5℃/min的升温速率升温至180℃并保持12‑15h，再自然冷却至室温，离心洗涤后干燥制得碳球和镧离子的复合物；将得到碳球和镧离子的复合物经研磨后在空气气氛中以1‑5℃/min的升温速率升温至500‑550℃煅烧3h，然后自然冷却至室温得到具有多核嵌套结构的碳酸镧微纳米材料。本发明制得的具有多核嵌套结构的碳酸镧微纳米材料具有更大的比表面积及丰富的活性位点，使其在污水处理方面具有很好的应用前景。
The invention discloses a method for preparing a lanthanum carbonate micro-nano material with a multi-nuclear nested structure. A sugar source is dissolved in secondary water, and a solution is formed by magnetic stirring; Then add urea to the obtained solution, ultrasonicate after magnetic stirring, transfer to a polytetrafluoroethylene reaction kettle, heat up to 180°C at a heating rate of 5°C/min and keep it for 12-15h, and then naturally cool to room temperature , centrifugal washing and drying to obtain a composite of carbon balls and lanthanum ions; the obtained composite of carbon balls and lanthanum ions is ground and then heated to 500-550 °C at a heating rate of 1-5 °C/min in an air atmosphere for calcination 3h, and then naturally cooled to room temperature to obtain a lanthanum carbonate micro-nano material with a multi-core nested structure. The lanthanum carbonate micro-nano material with multi-nuclear nested structure prepared by the invention has larger specific surface area and abundant active sites, so that it has a good application prospect in sewage treatment.
Description
Technical Field
The invention belongs to the technical field of synthesis of inorganic functional materials, and particularly relates to a preparation method of a lanthanum carbonate micro-nano material with a multi-core nested structure.
Background
In recent years, the development of nano materials with complex structures and special morphologies is exponentially increased, and the core-shell nano materials attract wide attention due to the unique properties of low density, large surface area, easy core functionalization, good molecular load capacity of void space, adjustable void space and the like and rich application prospects thereof. The multi-core inorganic micro-nano material can effectively shorten the path of a substance or charge transmission process, provide richer multi-center active sites, increase the specific surface area and the like, and strengthen the wide application of the multi-core inorganic micro-nano material in the aspects of catalysis, drug loading, energy and the like. Based on the advantages of the multi-core nested material, the micro-nano material with both the multi-core structure and the hierarchical pore structure has good development potential and application prospect. In addition, with the rapid development of industry, water pollution becomes one of the serious problems of the environmental work in China. The lanthanum carbonate nano-particles have obvious adsorption and removal effects on phosphorus due to the chemical and physical properties of the lanthanum carbonate nano-particles, and have wide application prospects. However, due to the complexity and the uncontrollable property of the structure of the multinuclear nested lanthanum carbonate micro-nano material, few documents are reported at home and abroad at present.
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.
Drawings
Fig. 1 is a TEM image of a lanthanum carbonate micro-nano material with a multi-core nested structure prepared in embodiment 1 of the present invention.
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.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1369578A (en) * | 2001-02-13 | 2002-09-18 | 中国科学技术大学 | Alkaline rare earth-carbonate crystical film and its hydrothermal preparing process |
| CN101279757A (en) * | 2008-05-22 | 2008-10-08 | 同济大学 | A kind of double hydrolysis regulation prepares the method for basic lanthanum carbonate nano/micro crystal |
| CN102531022A (en) * | 2010-12-30 | 2012-07-04 | 中国科学院过程工程研究所 | Preparation method of monodisperse rare earth oxide nanospheres |
| CN103193258A (en) * | 2013-04-10 | 2013-07-10 | 北京科技大学 | Method for preparing multi-shell cerium oxide ball with controllable shell quantity |
| CN104129810A (en) * | 2013-05-02 | 2014-11-05 | 南京大学 | Preparation of Three-Dimensional Hierarchical Structure of La2O2CO3 in Pure Monoclinic Phase |
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| KR102158060B1 (en) * | 2015-08-21 | 2020-09-21 | 내셔날 인스티튜트 오브 어드밴스드 인더스트리얼 사이언스 앤드 테크놀로지 | Proton conductive complex oxide and fuel cell using it as electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1369578A (en) * | 2001-02-13 | 2002-09-18 | 中国科学技术大学 | Alkaline rare earth-carbonate crystical film and its hydrothermal preparing process |
| CN101279757A (en) * | 2008-05-22 | 2008-10-08 | 同济大学 | A kind of double hydrolysis regulation prepares the method for basic lanthanum carbonate nano/micro crystal |
| CN102531022A (en) * | 2010-12-30 | 2012-07-04 | 中国科学院过程工程研究所 | Preparation method of monodisperse rare earth oxide nanospheres |
| CN103193258A (en) * | 2013-04-10 | 2013-07-10 | 北京科技大学 | Method for preparing multi-shell cerium oxide ball with controllable shell quantity |
| CN104129810A (en) * | 2013-05-02 | 2014-11-05 | 南京大学 | Preparation of Three-Dimensional Hierarchical Structure of La2O2CO3 in Pure Monoclinic Phase |
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