CN112744853A - Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora - Google Patents
Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora Download PDFInfo
- Publication number
- CN112744853A CN112744853A CN202011642895.0A CN202011642895A CN112744853A CN 112744853 A CN112744853 A CN 112744853A CN 202011642895 A CN202011642895 A CN 202011642895A CN 112744853 A CN112744853 A CN 112744853A
- Authority
- CN
- China
- Prior art keywords
- cerium
- boat
- sterculia
- cerium dioxide
- swollen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title claims abstract description 41
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 title claims abstract description 24
- 230000001699 photocatalysis Effects 0.000 title abstract description 6
- 241001412228 Scaphium lychnophorum Species 0.000 title description 9
- 238000007146 photocatalysis Methods 0.000 title description 2
- 241000934878 Sterculia Species 0.000 claims abstract description 48
- 235000021282 Sterculia Nutrition 0.000 claims abstract description 48
- 229940059107 sterculia Drugs 0.000 claims abstract description 48
- 241001571446 Scaphium scaphigerum Species 0.000 claims abstract description 27
- 150000000703 Cerium Chemical class 0.000 claims abstract description 23
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 230000008961 swelling Effects 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012266 salt solution Substances 0.000 claims abstract description 12
- 238000004108 freeze drying Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000000643 oven drying Methods 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 239000007783 nanoporous material Substances 0.000 claims abstract description 3
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 24
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 12
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 29
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 6
- 229910000420 cerium oxide Inorganic materials 0.000 description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 5
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 210000000582 semen Anatomy 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 239000013025 ceria-based material Substances 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 159000000021 acetate salts Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 210000003278 egg shell Anatomy 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Images
Classifications
-
- 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
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- 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
-
- 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
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analytical Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method for preparing a nano-porous cerium dioxide material based on boat-fruited sterculia seed, which comprises the following steps: dissolving cerium salt in water to prepare a cerium salt solution; adding boat-fruited sterculia seed into the cerium salt solution for swelling, and removing the core after complete swelling; and (3) washing the swollen sterculia scaphigera, drying in an oven or freeze drying, and calcining in a muffle furnace to obtain the swollen sterculia scaphigera-based cerium dioxide nano porous material. The preparation method of the nano-porous cerium dioxide prepared by the method is rapid, and the prepared cerium dioxide has high photocatalytic activity and can effectively improve the additional value of the cerium dioxide powder material.
Description
Technical Field
The invention belongs to the technical field of rare earth material application, and particularly relates to a method for preparing a nano-porous cerium dioxide material based on sterculia lychnophora.
Background
In rare earth, the price of cerium is low, the 99.9 percent of cerium oxide in 2020 is only about 13 yuan/kg, the price of nano cerium oxide is generally 100 yuan/kg or more, and the nano cerium oxide is beneficial to improving the added value of the cerium oxide. The existing method for preparing nano powder comprises the following steps: 1. gas phase method: the common methods include inert gas condensation, sputtering, vacuum vapor deposition on a flowing liquid surface, energization heating, wire explosion, chemical vapor reaction, and the like. 2. Liquid phase method: precipitation methods, hydrolysis methods, hydrothermal methods, spraying methods, sol-gels, and the like are common. 3. Solid phase method: the thermal decomposition method, the solid phase reaction method, the spark discharge method, the dissolution method, the ball milling method, etc. are commonly used.
The preparation method of the nano cerium dioxide mainly comprises a precipitation method, a hydrothermal method and a sol-gel method. Wherein, the technological conditions (dripping speed and reaction temperature) for preparing the nano cerium dioxide by the precipitation method are difficult to control, the reaction time is long, and the particle size distribution of the prepared powder is wide; the hydrothermal method for preparing the nano cerium dioxide has long reaction time and complex process; the sol-gel method for preparing the nano cerium dioxide has long reaction time, complex process and large particle size of the prepared powder.
The prior literature reports that the template agent is obtained by treating petals, eggshell inner membrane and the like with acid and alkali or by calcining starch and glucose at high temperature. Precipitating a cerium source in a template agent in a solution, drying and calcining to obtain the nano cerium dioxide. The methods obtain the template agent through pretreatment, and simultaneously need to add a precipitator, and then obtain the nano cerium dioxide through drying and calcining.
Therefore, there is a need for a novel method for preparing cerium dioxide nanopowder.
Disclosure of Invention
In view of the above, the invention provides a method for preparing a nano-porous cerium dioxide material based on sterculia lychnophora, aiming at the problems of complex process, long time consumption and high production cost.
In order to solve the technical problems, the invention discloses a method for preparing a nano-porous cerium dioxide material based on sterculia lychnophora, which comprises the following steps:
step 1, preparing a cerium salt solution: dissolving cerium salt in water to prepare a cerium salt solution;
Optionally, the cerium salt in step 1 is one of cerium nitrate, cerium sulfate or cerium acetate.
Optionally, the dissolution temperature in step 1 is 50 ℃ to 80 ℃.
Optionally, the mass ratio of the cerium salt to the water in the step 1 is 1:1-1: 10.
Optionally, the sterculia scaphigera in the step 2 accounts for 5-50% of the total mass of the cerium salt.
Optionally, the swelling rotation speed in the step 2 is 50-150r/min, and the swelling time is 0.5-1.5 h.
Optionally, the oven drying time in the step 2 is 1.5-2.5h, and the oven drying temperature is 75-85 ℃.
Optionally, the freeze-drying time in the step 2 is 1.5-2.5h, and the freeze-drying temperature is-25 ℃ to-40 ℃.
Alternatively, the calcination temperature in step 2 is 550 ℃ to 1050 ℃.
Compared with the prior art, the invention can obtain the following technical effects:
1) the cerium dioxide prepared by the invention can be widely applied to photocatalytic materials, cerium dioxide polishing powder materials, glass industrial additives, cosmetic ultraviolet absorbers and the like.
2) The method is simple, controllable, low in cost and suitable for industrial production, and can effectively improve the additional value of the cerium dioxide.
Of course, it is not necessary for any one product in which the invention is practiced to achieve all of the above-described technical effects simultaneously.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is an XRD diffraction pattern of cerium oxide powder based on swollen calcination of boat-fruited sterculia seed prepared in example 1 of the present invention;
FIG. 2 is a graph showing the degradation of methylene blue by photocatalytic degradation of nano-ceria based on swollen calcined ceria powder prepared in example 1 and purchased from a manufacturer;
FIG. 3 is an electron microscope picture of the swollen calcined ceria powder based on sterculia lychnophora prepared in example 1 of the present invention.
Detailed Description
The following embodiments are described in detail with reference to the accompanying drawings, so that how to implement the technical features of the present invention to solve the technical problems and achieve the technical effects can be fully understood and implemented.
The invention discloses a method for preparing a nano-porous cerium dioxide material based on boat-fruited sterculia seed, which comprises the following steps:
step 1, preparing a cerium salt solution: dissolving cerium salt in water at the temperature of 50-80 ℃ according to the mass ratio of 1:1-10 to prepare a cerium salt solution; wherein, the cerium salt is one of cerium nitrate, ammonium ceric nitrate, cerium sulfate or cerium acetate;
wherein, nitrate salt, sulfate salt and acetate salt can be decomposed at high temperature to generate oxide, if the oxide is directly decomposed at high temperature, the particle size of the generated oxide is extremely large and often reaches micron level, and the nano effect of materials is avoided. When preparing the nano oxide material, the nano oxide is generally sintered by utilizing the morphology inheritance of the precipitate which is generated in advance, such as nano hydroxide, nano oxalate, nano carbonate and the like, and is sintered at high temperature. The method prepares cerium dioxide by directly calcining cerium nitrate, cerium sulfate, cerium acetate and ammonium ceric nitrate solution without adding a precipitator and using the boat-fruited sterculia seed as a template.
Wherein, the calcining temperature is lower than 550 ℃ and can not decompose nitrate radical, sulfate radical and acetate radical, the sintering temperature is too high and exceeds 1050 ℃, the size of the produced powder is enlarged, and simultaneously, the energy consumption is too high.
The ratio of the solution to the boat-fruited sterculia seed is too high, the boat-fruited sterculia seed can not completely absorb the solution, the ratio of the solution to the boat-fruited sterculia seed is too low, and the boat-fruited sterculia seed is greatly wasted.
Example 1
Dissolving cerium nitrate in water according to the mass ratio of 1:5 at the temperature of 65 ℃ to prepare a cerium nitrate solution; weighing boat-fruited sterculia seed, wherein the boat-fruited sterculia seed accounts for 30% of the total mass of the cerium nitrate solution, and adding dried boat-fruited sterculia seed into the cerium nitrate solution to swell for 2 hours at the rotating speed of 100 r/min; and (3) washing the swollen sterculia scaphigera, drying the swollen sterculia scaphigera in an oven at 80 ℃ for 2h, and calcining the swollen sterculia scaphigera in a muffle furnace at 800 ℃ to prepare the swollen and calcined cerium dioxide material based on the sterculia scaphigera.
Example 2
Dissolving ammonium ceric nitrate in water at the temperature of 50 ℃ according to the mass ratio of 1:10 to prepare ammonium ceric nitrate solution; weighing dry boat-fruited sterculia seeds, wherein the dry boat-fruited sterculia seeds account for 5 percent of the mass of the ammonium cerium nitrate solution, and adding the dry boat-fruited sterculia seeds into the ammonium cerium nitrate solution to swell for 0.5 hour at the rotating speed of 150 r/min; and (3) washing the swollen sterculia scaphigera, drying the swollen sterculia scaphigera in an oven at 85 ℃ for 1.5h, and calcining the swollen sterculia scaphigera in a muffle furnace at 1050 ℃ to prepare the cerium dioxide material based on swollen and calcined sterculia scaphigera.
Example 3
Dissolving cerium sulfate in water according to the mass ratio of 1:1 at the temperature of 80 ℃ to prepare a cerium sulfate solution; weighing dried boat-fruited sterculia seed, wherein the dried boat-fruited sterculia seed accounts for 50% of the total mass of the cerium sulfate solution, and adding the dried boat-fruited sterculia seed into the cerium sulfate solution to swell for 1.5h at the rotating speed of 50 r/min; and (3) washing the swollen sterculia scaphigera, drying the swollen sterculia scaphigera in a 75 ℃ oven for 2.5h, and calcining the swollen sterculia scaphigera in a muffle furnace at 550 ℃ to prepare the swollen and calcined cerium dioxide material based on the sterculia scaphigera.
Example 4
Dissolving cerium acetate in water according to the mass ratio of 1:3 at the temperature of 60 ℃ to prepare a cerium acetate solution; weighing dry boat-fruited sterculia seed, wherein the boat-fruited sterculia seed accounts for 10 percent of the total mass of the cerium acetate solution, and adding the dry boat-fruited sterculia seed into the cerium acetate solution to swell for 0.8h at the rotating speed of 120 r/min; and (3) washing and denucleating the swollen sterculia scaphigera, drying in an oven at 78 ℃ for 2.2h, and calcining in a muffle furnace at 750 ℃ to prepare the cerium dioxide material based on swollen and calcined sterculia scaphigera.
Example 5
Dissolving cerium nitrate in water according to the mass ratio of 1:8 at the temperature of 70 ℃ to prepare a cerium nitrate solution; weighing boat-fruited sterculia seed, wherein the boat-fruited sterculia seed accounts for 40 percent of the total mass of the cerium nitrate solution, and adding dry boat-fruited sterculia seed into the cerium nitrate solution to swell for 1.2 hours at the rotating speed of 80 r/min; after removing the kernels of the swollen boat-fruited sterculia seeds and washing, carrying out freeze drying for 2h at the temperature of minus 30 ℃, and calcining in a muffle furnace at the temperature of 850 ℃ to prepare the cerium dioxide material based on the swollen and calcined boat-fruited sterculia seeds.
Example 6
Dissolving ammonium ceric nitrate in water according to the mass ratio of 1:6 at the temperature of 55 ℃ to prepare ammonium ceric nitrate solution; weighing boat-fruited sterculia seed, wherein the boat-fruited sterculia seed accounts for 30 percent of the total mass of the ammonium cerium nitrate solution, and adding the boat-fruited sterculia seed into the ammonium cerium nitrate solution to swell for 1.5 hours at the rotating speed of 90 r/min; after the swollen sterculia lychnophora is washed, the swollen sterculia lychnophora is frozen and dried for 1.5h at the temperature of minus 25 ℃, and calcined at the temperature of 550 ℃ in a muffle furnace to prepare the cerium dioxide material based on the swollen and calcined sterculia lychnophora.
Example 7
Dissolving cerium sulfate in water according to the mass ratio of 1:4 at the temperature of 75 ℃ to prepare a cerium sulfate solution; weighing boat-fruited sterculia seed, wherein the boat-fruited sterculia seed accounts for 35% of the total mass of the cerium sulfate solution, and adding the boat-fruited sterculia seed into the cerium sulfate solution to swell for 1.1h at the rotating speed of 80 r/min; and washing and denucleating the swollen sterculia scaphigera, freeze-drying the swollen sterculia scaphigera at the temperature of minus 40 ℃ for 2.5 hours, and calcining the swollen sterculia scaphigera in a muffle furnace at the temperature of 950 ℃ to prepare the cerium dioxide material based on swollen and calcined sterculia scaphigera.
Example 8
Dissolving cerium acetate in water according to the mass ratio of 1:5 at the temperature of 65 ℃ to prepare a cerium acetate solution; weighing semen Scaphii Lychnophori, wherein the weight of semen Scaphii Lychnophori accounts for 25% of the total weight of cerium acetate solution, adding semen Scaphii Lychnophori into the cerium acetate solution at a rotation speed of 100r/min, and swelling for 1 hr; and washing and removing the kernels of the swollen scaphium scaphigerum, freeze-drying the swollen scaphium scaphigerum for 2 hours at the temperature of minus 35 ℃, and calcining the swollen scaphium scaphigerum at the temperature of 1050 ℃ in a muffle furnace to prepare the cerium dioxide material based on the swollen and calcined scaphium scaphigerum.
As can be seen from FIG. 1, the XRD diffraction pattern of the boat-fruited sterculia seed swelling calcined ceria-based material prepared in example 1, compared with the standard PDF card #43-1002 of ceria, shows that the calcined product has no impurities, the ceria is formed, and the crystallinity of the product is high. As can be seen from fig. 2, the ceria material prepared in example 1 based on swelling calcination of sterculia scaphigera has a significantly improved photocatalytic efficiency compared to the photocatalytic degradation methylene blue curve of the photocatalytic nano-ceria purchased from a certain manufacturer. As can be seen from fig. 3, the boat sterculia seed swelling calcined ceria-based material prepared by example 1 has a porous structure, and the particle size reaches the nanometer level.
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A method for preparing a nano-porous cerium dioxide material based on boat-fruited sterculia seeds is characterized by comprising the following steps:
step 1, preparing a cerium salt solution: dissolving cerium salt in water to prepare a cerium salt solution;
step 2, weighing the boat-fruited sterculia seeds, adding the boat-fruited sterculia seeds into the cerium salt solution for swelling; removing kernels of the swelled boat-fruited sterculia seeds, washing, drying in an oven or freeze drying, and calcining in a muffle furnace to prepare the swelling and roasting cerium dioxide nano porous material based on the boat-fruited sterculia seeds.
2. The method according to claim 1, wherein the cerium salt in step 1 is one of cerium nitrate, cerium sulfate or cerium acetate.
3. The method according to claim 1, wherein the dissolution temperature in the step 1 is 50 ℃ to 80 ℃.
4. The method according to claim 1, wherein the cerium salt and water in step 1 are in a mass ratio of 1:1 to 1: 10.
5. The method as claimed in claim 1, wherein the sterculia scaphigera seeds in the step 2 account for 5-50% of the cerium salt.
6. The preparation method according to claim 1, wherein the swelling speed in step 2 is 50-150r/min, and the swelling time is 0.5-1.5 h.
7. The preparation method according to claim 1, wherein the oven drying time in the step 2 is 1.5-2.5h, and the oven drying temperature is 75-85 ℃.
8. The method according to claim 1, wherein the freeze-drying time in step 2 is 1.5 to 2.5 hours, and the freeze-drying temperature is-25 ℃ to-40 ℃.
9. The method according to claim 1, wherein the calcination temperature in the step 2 is 550 ℃ to 1050 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011642895.0A CN112744853A (en) | 2020-12-30 | 2020-12-30 | Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011642895.0A CN112744853A (en) | 2020-12-30 | 2020-12-30 | Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112744853A true CN112744853A (en) | 2021-05-04 |
Family
ID=75651187
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011642895.0A Pending CN112744853A (en) | 2020-12-30 | 2020-12-30 | Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112744853A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837053A (en) * | 2006-04-12 | 2006-09-27 | 中南大学 | Process for preparing mesoporous ceria |
| CN103908933A (en) * | 2014-03-10 | 2014-07-09 | 苏州科技学院相城研究院 | Preparation method and applications of porous hollow submicron cerium oxide microcapsules |
| CN107381616A (en) * | 2017-09-15 | 2017-11-24 | 福州大学 | A kind of method that active porous nano ceric oxide is prepared based on organic formwork |
| CN107522221A (en) * | 2017-09-15 | 2017-12-29 | 福州大学 | A kind of method that active porous nano ceric oxide is prepared based on inorganic template |
-
2020
- 2020-12-30 CN CN202011642895.0A patent/CN112744853A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837053A (en) * | 2006-04-12 | 2006-09-27 | 中南大学 | Process for preparing mesoporous ceria |
| CN103908933A (en) * | 2014-03-10 | 2014-07-09 | 苏州科技学院相城研究院 | Preparation method and applications of porous hollow submicron cerium oxide microcapsules |
| CN107381616A (en) * | 2017-09-15 | 2017-11-24 | 福州大学 | A kind of method that active porous nano ceric oxide is prepared based on organic formwork |
| CN107522221A (en) * | 2017-09-15 | 2017-12-29 | 福州大学 | A kind of method that active porous nano ceric oxide is prepared based on inorganic template |
Non-Patent Citations (1)
| Title |
|---|
| 赵国峥等: "以海藻酸钠为模板制备蜂窝状纳米CeO2及其性能", 中国稀土学报, vol. 36, no. 5, pages 558 - 563 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103949193B (en) | Universal method for preparing inorganic hollow microspheres | |
| CN102295304B (en) | Preparation method of pseudo-boehmite and microcrystalline corundum abrasive | |
| JP7021795B2 (en) | Method for preparing indium oxide spherical powder with controllable grain shape | |
| CN110975795A (en) | Synthesis method of lithium extraction adsorbent | |
| CN108910932B (en) | Method for preparing narrow-distribution superfine yttrium oxide by sodium carbonate precipitation | |
| CN109019656B (en) | Method for producing nano rare earth oxide powder | |
| CN109205655B (en) | Preparation method of nano gadolinium oxide with particle size of 80-100nm | |
| CN110194480B (en) | Nano cerium oxide and preparation method thereof | |
| CN110615463B (en) | Production method of high-purity indium oxide nano powder of trace carbon element | |
| CN104944471A (en) | Tungsten doped bronze powder having high infrared shielding property and synthesis method of doped tungsten bronze powder | |
| CN101066781A (en) | Process of preparing cobalto-cobaltic oxide for lithium ion cell | |
| CN113877586B (en) | Preparation method and application of cerium-iron bimetallic composite oxide with hierarchical structure and controllable morphology | |
| JP5233007B2 (en) | Paint for transparent conductive material and method for producing transparent conductive film | |
| CN105016382A (en) | Method for preparing pure gold redstone type titanium dioxide nanorod | |
| CN113600174B (en) | Bismuth-bismuth oxide carbonate composite photocatalyst and preparation method and application thereof | |
| CN110759385B (en) | Bismuth ferrite nano cube material and preparation method and application thereof | |
| CN109485434A (en) | The method of low temperature synthesis yttrium-aluminium-garnet ceramic powder | |
| CN112744853A (en) | Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora | |
| CN111646493A (en) | Hydrothermal preparation method of yttrium oxide nano powder | |
| CN114873618B (en) | Nanoscale boehmite and preparation method and application thereof | |
| CN107352554B (en) | Preparation method and application of magnetic X-type molecular sieve | |
| CN112374524A (en) | Preparation method of cerium dioxide nano powder based on dry tremella | |
| JP2963296B2 (en) | Method for producing conductive fine powder | |
| CN109019676B (en) | Method for preparing high-purity nano-grade barium titanate by precipitation method | |
| CN112159240A (en) | Preparation method for synthesizing lanthanum hafnate powder by molten salt growth method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210504 |