CN109336161A - A kind of preparation method of CeO2 nanotube, CeO2 nanotube and application - Google Patents
A kind of preparation method of CeO2 nanotube, CeO2 nanotube and application Download PDFInfo
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- CN109336161A CN109336161A CN201811342597.2A CN201811342597A CN109336161A CN 109336161 A CN109336161 A CN 109336161A CN 201811342597 A CN201811342597 A CN 201811342597A CN 109336161 A CN109336161 A CN 109336161A
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- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a kind of CeO2The preparation method of nanotube.The present invention, using simple hydro-thermal reaction, prepares Cerium Oxide Nanotubes using carbonate, formic acid, highly basic and trivalent solubility cerium salt as raw material.Synthesized Cerium Oxide Nanotubes have surface richness cerium, mainly exist in the form of the cerium ion of tetravalence, potentially act as the adsorbent for removing pollution organic compound in water, this is an important application in water treatment system.
Description
Technical field
The invention belongs to nano materials and field of waste water treatment, are related to a kind of CeO2The preparation method of nanotube, CeO2Nanometer
Pipe and application.
Background technique
Ceria is the most abundant rare earth element and the most abundant rare earth resources of China's reserves in the earth's crust, because of its tool
There are excellent oxygen storage capacity, higher thermal stability, good optical property etc., has attracted extensive research interest, and
Be applied to the fields such as catalysis, fuel cell, sensor [A.Trovarelli, C.de Leitenburg, M.Boaro,
G.Dolcetti, Catal.Today 1999,50,353；S.D.Park, J.M.Vohs, R.J.Gorte, Nature 2000,
404,265；E.L.Brosha, R.Mukundan, D.R.Brown, F.H.Garzon, J.H.Visser, Solid State
Ionics 2002,148,61；S.Yabe, T.J.Sato, Solid State Chem.2003,171,7.].With nano material
The development of controlledly synthesis technology to develop there is the ceria functional material of excellent structural characteristic to provide new opportunity.So
And rare earth cerium oxide because have cubic fluorite structure, cannot in the solution direct anisotropic growth at one-dimensional rare earth cerium oxide
Nano-tube material.Therefore, hydro-thermal method synthesizing one-dimensional rare earth cerium oxide nanotube is utilized in the solution, it is necessary to find suitable close
At scheme.Common solution is by means of the physics such as porous aluminium, carbon nanotube, nano wire, nanometer rods or chemical mould
Plate recycles the synthetic technologys such as electrochemical deposition or liquid deposition to realize one-dimensional rare earth cerium oxide nanotube
[R.Inguanta, S.Piazza, C.Sunseri, Nanotechnology 18 (2007) 485605；D.Zhang, H.Fu,
L.Shi, J.Fang, Q.Li, J.Solid State Chem.180 (2007) 654-660；T.Wang, L.Zhang, J.Zhang,
G.Hua, Micropor.Mesopor.Mat.171 (2013) 196-200；J.Wu, J.Wang, Y.Du, H.Li, Y.Yang,
X.Jia, Appl.Catal.B-Environ.174-175 (2015) 435-444；Y.Feng, L.Liu, X.Wang,
J.Mater.Chem.21(2011)15442-15448；K.Lin, S.Chowdhury, Int.J.Mol.Sci.11 (2010)
3226-3251].It can also be in such a way that self-template methods be combined with Ostwald ripening process come synthesizing one-dimensional rare earth
Cerium Oxide Nanotubes [K.Zhou, Z.Yang, S.Yang, Chem.Mater.19 (2007) 1215-1217；X.Wu, S.Kawi,
Cryst.Growth Des.10(2010)1833-1841；Z.Wang, J.Qi, K.Zhao, L.Zong, Z.Tang, L.Wang,
R.Yu, Mater.Chem.Front.1 (2017) 1629-1634].Although template method being capable of synthesizing one-dimensional Rare-Earth Ce O2Nanometer
Pipe, but it has the characteristics that complicated for operation, higher cost and energy consumption is larger.Another solution is the synthesis of two steps
Method designs and constructs first the one-dimensional Rare-Earth Ce O with anisotropic structure2Then nanotube precursor passes through calcining conversion
At required CeO2Nanotube.The key for realizing two-step synthesis method is searched out suitably, with anisotropic one-dimensional CeO2It receives
Mitron precursor.Once it is determined that the nanotube precursor of anisotropic structure, it can be using easy to operate, at low cost, investment
Few hydrothermal synthesis route is realized.The most important point is can to control and adjust CeO by control hydrothermal reaction condition2
The appearance structure and physicochemical properties of nanotube.However, in reported work, only only Ce (0H) 3 be used as it is each to
The one-dimensional CeO of anisotropic approach2Nanotube precursor [G.Chen, C.Xu, X.Song, W.Zhao, Y.Ding, S.Sun,
Inorg.Chem.47(2008)723-728；W.-Q.Han, L.Wu, Y.Zhu, J.Am.Chem.Soc.127 (2005) 12814-
12815；C.C.Tang, Y.Bando, B.D.Liu, D.Golberg, Adv.Mater.17 (2005) 3005-3009].This is limited
Synthetic method and means greatly limit Rare-Earth Ce O2The development and application of nanotube.Therefore, it needs to develop a kind of easy, low
Cost and the synthetic route being easily mass produced prepare the one-dimensional Rare-Earth Ce O with excellent physical chemical property2Nanotube comes
It is developed in the application in the fields such as Industrial Wastewater Treatment, Industrial Catalysis, electrochemistry, optical engineering, it is promoted to send out in national economy
Needs in exhibition and big industrialized production.
Summary of the invention
The purpose of the present invention, for industrialization demand and above-mentioned technical problem, develop it is a kind of easily to operate, cost is relatively low
Hydro-thermal synthesis process route, prepare Rare-Earth Ce O2Nano-tube material, preferably to develop CeO2The physical and chemical performance of nanotube and latent
Technical support is provided in application.
The present invention from practical angle design scheme, using cheap inorganic raw material and easy to operate, cost compared with
Low hydro-thermal route prepares Rare-Earth Ce O2Nanotube.The purpose of the present invention can be achieved through the following technical solutions:
CeO2The hydrothermal synthesis method of nanotube carries out in accordance with the following steps:
(1) dissolution of trivalent cerium soluble-salt is formed into clear solution in deionized water.
(2) formic acid is added in the solution that step (1) obtains with vigorous stirring, is uniformly mixed.
(3) ammonium hydroxide of specified rate is added in the solution that step (2) obtains with vigorous stirring, is uniformly mixed.
(4) sodium bicarbonate of specified rate is added to vigorous stirring in the suspension that step (3) obtains, mixing is equal
It is even.
(5) mixed liquor that step (4) obtains is transferred in closed reactor, is placed in baking oven, heated at 100-160 DEG C,
Reaction gained sediment is washed with distilled water, is dried to obtain CeO2Precursor body of Nano tube.
(6) presoma for obtaining step (5) under air draught in 350-800 DEG C heating 5-10 hours, obtain CeO2
Nanotube.
Further, formates prepared in step (2) can be replaced by formates reagent.
Further, the mass ratio between the trivalent cerium soluble-salt and deionized water is 1: 20-30.
Further, the trivalent cerium soluble-salt, formic acid, ammonium hydroxide, the mass ratio between sodium bicarbonate be 1: 2-3:
3-4.8∶0.5-1.5。
A kind of CeO2Nanotube is made by above-mentioned preparation method.
The resulting CeO of the present invention2Nanotube is the nano material that performance is removed with absorption, is the oxygen with rich cerium surface
Change cerium nanotube.
The pattern of product of the present invention is observed by scanning electron microscope (SEM) and transmission electron microscope (TEM), and composed structure passes through red
External spectrum (FT-IR) and thermogravimetric analysis (TG) analysis, object phase component pass through X-ray powder diffraction (XRD) identification, surface group
It is detected at by photoelectron spectroscopy (XPS).Technical solution through the invention, the cerium dioxide nano of available surface richness cerium
Pipe, target product purity is high.
The present invention, by hydro-thermal method, realizes one-dimensional using carbonate, aqueous formic acid, alkali and soluble cerium salt as raw material
The preparation of RE CeO 2 nanotube, easy to operate, easily-controlled reaction conditions, product purity are high.Raw material is inexpensively easy in method
, reaction is simple, is not necessarily to complex device, has the characteristics that at low cost, application is strong.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the resulting Cerium Oxide Nanotubes presoma of embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of 1 resulting Cerium Oxide Nanotubes presoma end of embodiment；
Fig. 3 is the infrared spectrogram of the resulting Cerium Oxide Nanotubes presoma of embodiment 1；
Fig. 4 is the hot weight curve of the resulting Cerium Oxide Nanotubes presoma of embodiment 1；
Fig. 5 is the scanning electron microscope (SEM) photograph of the resulting Cerium Oxide Nanotubes of embodiment 1；
Fig. 6 is the transmission electron microscope picture of the resulting Cerium Oxide Nanotubes of embodiment 1；
Fig. 7 is the XRD diagram of the resulting Cerium Oxide Nanotubes of embodiment 1；
Fig. 8 is that the photoelectron spectroscopy 01s of Cerium Oxide Nanotubes schemes；
Fig. 9 is that the photoelectron spectroscopy Ce3d of Cerium Oxide Nanotubes schemes；
Figure 10 is that Cerium Oxide Nanotubes remove Congo red absorption, and the quality of Cerium Oxide Nanotubes is 25mg, solution body
Product is 50ml, and Congo red concentration is 50mg/l；
Figure 11 is the loop test of Cerium Oxide Nanotubes, and the quality of Cerium Oxide Nanotubes is 25mg, liquor capacity 50ml,
Congo red concentration is 50mg/l.
Specific embodiment
Several specific embodiments of the invention are given below, the present invention to be described in more details.
Embodiment 1
It is raw material that the present invention, which is described using formates and carbonate etc., synthesizes CeO by hydro-thermal method2The side of nanotube
Method.Firstly, weighing 1.0g Ce (NO3)3·6H2O is dissolved into 24.5ml deionized water, forms clear solution.It is being vigorously stirred
Under, 2ml formic acid is added to above-mentioned solution, is thoroughly mixed to form solution.Mixed solution is added in 3.5ml ammonium hydroxide again, mixing is equal
It is even, form suspension.Finally 0.6g sodium bicarbonate is added in the suspension, is transferred in closed reactor, baking oven is placed in,
It is heated 20 hours at 120 DEG C, gained sediment is filtered after reaction and distilled water washing, be dried to obtain with carbonate and formate
CeO2Precursor body of Nano tube, electromicroscopic photograph such as Fig. 1 and Fig. 2, infrared spectroscopy such as Fig. 3, thermogravimetric curve such as Fig. 4.By the preceding body
Body heats 5 hours under air draught in 450 DEG C, obtains faint yellow sample.After washing, drying, acquisition width is 100-
300nm, the pure CeO that length is several microns2Nanotube, electromicroscopic photograph such as Fig. 5 and Fig. 6, XRD diffraction spectra are as shown in Figure 7.
Embodiment 2
Weigh 1.0g Ce (NO3)3·6H2O is dissolved into 24ml deionized water, forms clear solution.With vigorous stirring,
2ml formic acid is added to above-mentioned solution, is thoroughly mixed to form solution.Mixed solution is added in 4ml ammonium hydroxide again, is uniformly mixed, shape
At suspension.Finally 0.6g sodium bicarbonate is added in the suspension, is transferred in closed reactor, baking oven is placed in, 120
DEG C heating 20 hours, after reaction filter gained sediment through distillation water washing, be dried to obtain the CeO with anisotropic structure2
Precursor body of Nano tube.The precursor is heated 5 hours under air draught in 450 DEG C, faint yellow sample is obtained.By washing,
After drying, pure CeO is obtained2Nanotube.
Embodiment 3
Weigh 1.0g Ce (NO3)3·6H2O is dissolved into 24.5ml deionized water, forms clear solution.It is being vigorously stirred
Under, 2ml formic acid is added to above-mentioned solution, is thoroughly mixed to form solution.Mixed solution is added in 3.5ml ammonium hydroxide again, mixing is equal
It is even, form suspension.Finally 1g sodium bicarbonate is added in the suspension, is transferred in closed reactor, baking oven is placed in,
120 DEG C are heated 20 hours, and gained sediment is filtered after reaction and distilled water washing, be dried to obtain with anisotropic structure
CeO2Precursor body of Nano tube.The precursor is heated 5 hours under air draught in 450 DEG C, faint yellow sample is obtained.By washing
After washing, drying, pure CeO is obtained2Nanotube.
The present invention synthesizes Cerium Oxide Nanotubes using raw materials such as cheap formates and carbonate, by hydro-thermal method.It incite somebody to action this
The Cerium Oxide Nanotubes of invention are characterized by XPS photoelectron spectroscopy, the cerium oxide nano particle of discovery and traditional precipitation method preparation
Compare, cerium oxide nano pipe surface is shown containing more cerium atoms, and mainly based on the cerium ion of tetravalence, such as Fig. 8 and
Shown in Fig. 9.This rich cerium Cerium Oxide Nanotubes shows high efficiency in terms of the organic compound that absorption removes in water.
The present invention describes in the technical field of environment and water, is moved using the Cerium Oxide Nanotubes with surface richness cerium
The method of debirs in water removal.Rich cerium Cerium Oxide Nanotubes absorption of the invention, which is removed except Congo red, to be confirmed, and will
It removes effect with the absorption of the cerium oxide nano particle by traditional precipitation method preparation and is compared.It was found that with commercially available oxidation
Cerium nanoparticle is compared with the cerium oxide nano particle of traditional precipitation method preparation, and rich cerium Cerium Oxide Nanotubes of the invention are shown
Higher efficiency, as shown in Figure 10.Even if being reused many times, rich cerium Cerium Oxide Nanotubes still show that very high absorption removes
Efficiency, as shown in figure 11.
The synthetic method of Cerium Oxide Nanotubes of the present invention produces first using formic acid and ammonium hydroxide comprising as described above
Acid group, and in other embodiments, it can directly be substituted by formates using formate made from formic acid and ammonium hydroxide.
Although the detailed description and description of the specific embodiments of the present invention are given above, it should be noted that
We can carry out various equivalent changes and modification to above embodiment according to the concept of the present invention, and generated function is made
It, should all be within protection scope of the present invention when with the spirit still covered without departing from specification.
Claims (6)
1. a kind of CeO2The preparation method of nanotube, which is characterized in that carry out in accordance with the following steps:
(1) dissolution of trivalent cerium soluble-salt is formed into clear solution in deionized water；
(2) formic acid is added in the solution that step (1) obtains with vigorous stirring, is uniformly mixed；
(3) ammonium hydroxide is added in the solution that step (2) obtains with vigorous stirring, is uniformly mixed；
(4) sodium bicarbonate is added in the suspension that step (3) obtains with vigorous stirring, is uniformly mixed.；
(5) mixed liquor that step (4) obtains is transferred in closed reactor, is placed in baking oven, heated at 100-160 DEG C, reaction
Gained sediment is washed with distilled water, is dried to obtain CeO2Precursor body of Nano tube；
(6) presoma for obtaining step (5) under air draught in 350-800 DEG C heating 5-10 hours, obtain CeO2Nanometer
Pipe.
2. a kind of CeO according to claim 12The preparation method of nanotube, which is characterized in that prepared by step (2)
Formates can be replaced by formates reagent.
3. a kind of CeO according to claim 12The preparation method of nanotube, which is characterized in that the trivalent cerium is solvable
Property salt and deionized water between mass ratio be 1: 20-30.
4. a kind of CeO according to claim 12The preparation method of nanotube, which is characterized in that the trivalent cerium is solvable
Property salt, formic acid, ammonium hydroxide, the mass ratio between sodium bicarbonate be 1: 2-3: 3-4.8: 0.5-1.5.
5. a kind of CeO2Nanotube, feature are being, are made by the described in any item preparation methods of claim 1-4.
6. a kind of CeO2The application of nanotube, which is characterized in that using the CeO described in claim 52Nanotube absorption, which removes, to be had
Machine compound.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110422871A (en) * | 2019-08-20 | 2019-11-08 | 南昌大学 | The preparation method of Cerium Oxide Nanotubes |
| CN114620755A (en) * | 2021-12-30 | 2022-06-14 | 南京大学 | Cerium dioxide nanotube and preparation method thereof |
| CN115215410A (en) * | 2022-07-18 | 2022-10-21 | 山东大学 | Method for synchronously removing antibiotics and resistance genes by activating sodium hypochlorite through cerium oxide modified carbon nanotube film |
| CN115465879A (en) * | 2021-06-11 | 2022-12-13 | 四川大学 | Spherical CeO 2 Preparation method of (1) |
-
2018
- 2018-11-12 CN CN201811342597.2A patent/CN109336161B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110422871A (en) * | 2019-08-20 | 2019-11-08 | 南昌大学 | The preparation method of Cerium Oxide Nanotubes |
| CN115465879A (en) * | 2021-06-11 | 2022-12-13 | 四川大学 | Spherical CeO 2 Preparation method of (1) |
| CN115465879B (en) * | 2021-06-11 | 2023-06-02 | 四川大学 | Spherical CeO 2 Is prepared by the preparation method of (2) |
| CN114620755A (en) * | 2021-12-30 | 2022-06-14 | 南京大学 | Cerium dioxide nanotube and preparation method thereof |
| CN114620755B (en) * | 2021-12-30 | 2023-09-05 | 南京大学 | Cerium dioxide nanotube and preparation method thereof |
| CN115215410A (en) * | 2022-07-18 | 2022-10-21 | 山东大学 | Method for synchronously removing antibiotics and resistance genes by activating sodium hypochlorite through cerium oxide modified carbon nanotube film |
| CN115215410B (en) * | 2022-07-18 | 2024-03-08 | 山东大学 | Method for synchronously removing antibiotics and resistance genes by activating sodium hypochlorite through cerium oxide modified carbon nano tube film |
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