CN111620361A - Preparation method of thorium dioxide nano material - Google Patents
Preparation method of thorium dioxide nano material Download PDFInfo
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- CN111620361A CN111620361A CN202010464235.1A CN202010464235A CN111620361A CN 111620361 A CN111620361 A CN 111620361A CN 202010464235 A CN202010464235 A CN 202010464235A CN 111620361 A CN111620361 A CN 111620361A
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 22
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- VGBPIHVLVSGJGR-UHFFFAOYSA-N thorium(4+);tetranitrate Chemical compound [Th+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VGBPIHVLVSGJGR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 8
- 239000000919 ceramic Substances 0.000 abstract description 7
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000011858 nanopowder Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 15
- 229910004369 ThO2 Inorganic materials 0.000 description 12
- 239000000843 powder Substances 0.000 description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 229910052768 actinide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F15/00—Compounds of thorium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/12—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of actinides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/51—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on compounds of actinides
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
- G21C3/42—Selection of substances for use as reactor fuel
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- G21C3/62—Ceramic fuel
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method of a thorium dioxide nano material, belonging to the technical field of nano materials. The preparation method comprises the steps of uniformly mixing thorium nitrate solution and sodium hydroxide solution, adding the mixture into a reaction kettle for hydrothermal reaction, cooling the reaction product to room temperature, and then adding waterWashing until the pH value is 7.5-8.5, drying and grinding to obtain the thorium dioxide nano material. By using the preparation method of the thorium dioxide nano material, the ThO with controllable appearance, lighter agglomeration, uniform particle size, higher specific surface area and good catalytic activity can be prepared on a large scale2Ceramic nano-powder.
Description
Technical Field
The invention belongs to the technical field of thorium dioxide nano materials, and relates to a preparation method of a thorium dioxide nano material.
Background
Thorium dioxide (ThO)2) Actinide metal oxides are not only important nuclear fuels, but also have been widely used in the fields of adsorption, catalysis, and the like. In order to obtain ThO with better comprehensive performance2Scientists have tried different preparation methods and raw materials.
Chen et al use oxalic acid precipitation to react thorium nitrate solution with oxalic acid and then calcine to make ThO2And (3) powder. Liu et al, using radiation method, with soluble thorium complex (NH)4)4Th(C2O4)4Is used as reactant to obtain micron-sized insoluble precursor, and is sintered at 600 ℃ to obtain ThO2Micron particles. Mishra et al synthesized ThO containing water of crystallization by precipitation2It was found to be specific for Ba in radioactive waste liquid2+And Sr2+The cation has better adsorption effect.
Liu and the like are prepared by a hydrothermal method by taking thorium nitrate, urea and glycerol as raw materials2Ceramic powder is used for adsorption. Cui and the like are subjected to mixed reaction of thorium nitrate solution and urea solution by using a microwave-assisted hydrothermal method to obtain ThO with a sheet-shaped surface structure2A ceramic nanomaterial.
Although there are already many ThO' s2The preparation method, however, prepares ThO with controllable morphology, lighter agglomeration, uniform particle size, higher specific surface area and good catalytic activity on a large scale2Efforts are still needed for ceramic nanopowders.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a method for preparing thorium dioxide nano material, so as to prepare ThO with controllable appearance, lighter agglomeration, uniform particle size, higher specific surface area and good catalytic activity in a large scale2Ceramic nano-powder.
In order to realize the purpose, in a basic embodiment, the invention provides a preparation method of thorium dioxide nano material, which comprises the steps of uniformly mixing a thorium nitrate solution and a sodium hydroxide solution, adding the mixture into a reaction kettle for hydrothermal reaction, cooling a reaction product to room temperature, washing the reaction product with water until the pH value is 7.5-8.5, drying and grinding the reaction product, and thus obtaining the thorium dioxide nano material.
In a preferred embodiment, the invention provides a preparation method of thorium dioxide nano-material, wherein the concentration of the thorium nitrate solution is 0.5-1.0mol/L, the concentration of the sodium hydroxide solution is 5-8mol/L, and the mixing volume ratio of the thorium nitrate solution and the sodium hydroxide solution is 1:20-1: 10.
In a preferred embodiment, the invention provides a preparation method of thorium dioxide nano-material, wherein the reaction kettle is a stainless steel high-temperature high-pressure reaction kettle taking polytetrafluoroethylene as a lining.
In a preferred embodiment, the invention provides a preparation method of thorium dioxide nano-material, wherein the temperature of the hydrothermal reaction is 80-100 ℃, the pressure is 0.6-0.8MPa, and the time is 18-48 hours.
The preparation method of the thorium dioxide nano material has the beneficial effects that (1) sodium hydroxide is used as a precipitator, and the sodium hydroxide is widely used, cheap and easy to prepare. (2) Hydrothermal method for preparing ThO2The ceramic powder does not need high-temperature calcination treatment, and the growth of crystal grains, defect formation and impurity introduction caused in the calcination process are avoided, so that the prepared powder has higher sintering activity. (3) The sodium hydroxide is matched with a hydrothermal method, and the ThO with controllable appearance, lighter agglomeration, uniform particle size, higher specific surface area and good catalytic activity can be prepared on a large scale2Ceramic nano-powder.
Drawings
FIG. 1 is an XRD detection spectrum of thorium dioxide nano-materials prepared in examples 1-3.
FIG. 2 is a scanning electron microscope detection spectrum of the thorium dioxide nanomaterial prepared in example 1.
FIG. 3 is a scanning electron microscope detection spectrum of the thorium dioxide nanomaterial prepared in example 2.
FIG. 4 is a scanning electron microscope detection spectrum of the thorium dioxide nanomaterial prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Example 1:
5mL of a 0.5mol/L thorium nitrate solution was added dropwise to 75mL of a 5mol/L sodium hydroxide solution, and the mixture was stirred at room temperature for 30 min. Subsequently, the mixed solution was transferred to a 100mL stainless steel reaction vessel lined with Teflon and placed in an oven at 80 ℃ under 0.6MPa for 48 hours. Cooling to room temperature, washing with ultrapure water to pH 7.5, drying at 60 deg.C, and grinding to obtain ThO2White powder.
To obtain ThO2White powder was measured, XRD pattern and ThO2Standard PDF cards 65-0291 correspond (see fig. 1); the scanning electron microscope detection result shows that (see figure 2) the particle size is relatively uniform, the average grain size is 8.7nm, and the dispersibility is good.
Example 2:
5mL of a 0.8mol/L thorium nitrate solution was added dropwise to 75mL of a 6.4mol/L sodium hydroxide solution, and the mixture was stirred at room temperature for 30 min. Subsequently, the mixed solution was transferred to a 100mL stainless steel reaction vessel lined with Teflon and placed in an oven at 90 ℃ under 0.7MPa for 30 hours. Cooling to room temperature, washing with ultrapure water to pH 8.0, drying at 60 deg.C, and grinding to obtain ThO2White powder.
To obtain ThO2White powder was measured, XRD pattern and ThO2Standard PDF cards 65-0291 correspond (see fig. 1); the scanning electron microscope test result shows (see figure 3), the particle diameter is relatively uniform, the average grain size is 8.9nm, and the dispersibility is good。
Example 3:
5mL of a 1.0mol/L thorium nitrate solution was added dropwise to 75mL of an 8mol/L sodium hydroxide solution, and the mixture was stirred at room temperature for 30 min. Subsequently, the mixed solution was transferred to a stainless steel reaction vessel with a 100mL inner liner of polytetrafluoroethylene, and the vessel was placed in an oven at 100 ℃ and 0.8MPa for 18 hours. Cooling to room temperature, washing with ultrapure water to pH 8.5, drying at 60 deg.C, and grinding to obtain ThO2White powder.
To obtain ThO2White powder was measured, XRD pattern and ThO2Standard PDF cards 65-0291 correspond (see fig. 1); the scanning electron microscope detection result shows (see figure 4), the particle size is relatively uniform, the average grain size is 9.6nm, and the dispersibility is good.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (4)
1. A preparation method of thorium dioxide nano material is characterized by comprising the following steps: the preparation method comprises the steps of uniformly mixing a thorium nitrate solution and a sodium hydroxide solution, adding the mixture into a reaction kettle for hydrothermal reaction, cooling a reaction product to room temperature, washing the reaction product with water until the pH value is 7.5-8.5, drying and grinding the reaction product to obtain the thorium dioxide nano material.
2. The method of claim 1, wherein: the concentration of the thorium nitrate solution is 0.5-1.0mol/L, the concentration of the sodium hydroxide solution is 5-8mol/L, and the mixing volume ratio of the thorium nitrate solution to the sodium hydroxide solution is 1:20-1: 10.
3. The method of claim 1, wherein: the reaction kettle is a stainless steel high-temperature high-pressure reaction kettle taking polytetrafluoroethylene as a lining.
4. The method of claim 1, wherein: the temperature of the hydrothermal reaction is 80-100 ℃, the pressure is 0.6-0.8MPa, and the time is 18-48 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4687601A (en) * | 1983-11-25 | 1987-08-18 | Comurhex | Process for the preparation of pulverulent metallic oxides from metallic nitrates |
| CN105132682A (en) * | 2015-09-10 | 2015-12-09 | 中国科学院长春应用化学研究所 | Method for extracting and separating cerium, fluorine and phosphorus from sulfuric acid leaching solution of Baotou rare earth mine |
| CN108083315A (en) * | 2018-02-08 | 2018-05-29 | 中国科学院上海应用物理研究所 | A kind of preparation method of the spherical thorium anhydride nano material of sheet surface structure and thus obtained spherical thorium anhydride particle |
| CN110386618A (en) * | 2019-08-20 | 2019-10-29 | 福建省长汀金龙稀土有限公司 | A kind of preparation method of the low thorium of PET, low uranium luteium oxide |
| CN111439772A (en) * | 2020-03-10 | 2020-07-24 | 中国原子能科学研究院 | Preparation method of thorium dioxide nano material |
-
2020
- 2020-05-27 CN CN202010464235.1A patent/CN111620361A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4687601A (en) * | 1983-11-25 | 1987-08-18 | Comurhex | Process for the preparation of pulverulent metallic oxides from metallic nitrates |
| CN105132682A (en) * | 2015-09-10 | 2015-12-09 | 中国科学院长春应用化学研究所 | Method for extracting and separating cerium, fluorine and phosphorus from sulfuric acid leaching solution of Baotou rare earth mine |
| CN108083315A (en) * | 2018-02-08 | 2018-05-29 | 中国科学院上海应用物理研究所 | A kind of preparation method of the spherical thorium anhydride nano material of sheet surface structure and thus obtained spherical thorium anhydride particle |
| CN110386618A (en) * | 2019-08-20 | 2019-10-29 | 福建省长汀金龙稀土有限公司 | A kind of preparation method of the low thorium of PET, low uranium luteium oxide |
| CN111439772A (en) * | 2020-03-10 | 2020-07-24 | 中国原子能科学研究院 | Preparation method of thorium dioxide nano material |
Non-Patent Citations (1)
| Title |
|---|
| 李英杰等: "溶剂热法合成微纳米介孔ThO_2的研究", 《硅酸盐通报》, vol. 35, no. 11, 30 November 2016 (2016-11-30), pages 3724 - 3728 * |
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