CN106006703B - Hydro-thermal method prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate - Google Patents
Hydro-thermal method prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate Download PDFInfo
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- CN106006703B CN106006703B CN201610352324.0A CN201610352324A CN106006703B CN 106006703 B CN106006703 B CN 106006703B CN 201610352324 A CN201610352324 A CN 201610352324A CN 106006703 B CN106006703 B CN 106006703B
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- cerium
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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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- 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
- C01F17/282—Sulfates
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
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- Manufacturing & Machinery (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
The present invention relates to a kind of hydro-thermal methods to prepare nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate, and first using cerous salt and lanthanum chloride as presoma, ammonium hydroxide and ammonium sulfate are precipitating reagent, are reacted 12 20 hours at 120 200 DEG C by hydro-thermal mode.Obtained intermediate product, then in a manner of ion exchange, in the sodium hydroxide solution of 0.4 mol/L, stir 8 12 hours, finally carry out separating, washing, obtain nano-sheet hydrogen-storing material.The present invention does not need to any template, does not add organic solvent, and preparation process is substantially pollution-free.Product has good application prospect in terms of novel three-way catalyst.
Description
Technical field
The invention belongs to technical field of inorganic nano-material preparation, more particularly to a kind of hydro-thermal method prepares nano-grade oxygen
Change the method for cerium and lanthanum cerium Hydroxysulfate.
Background technology
In recent years, vehicle exhaust has become one of main source of air pollution, control and improvement automobile exhaust pollution
Current global important topic is become.Since the 1970s, three-way catalyst（Three Way Conversion
Catalyst, TWC）Just into the most effective means of motor vehicle tail-gas purifying.In three-way catalyst, hydrogen-storing material is composition
One pith of catalyst determines performance and the service life of catalyst.The most important effect of hydrogen-storing material is to realize hair
The active oxygen storage and release in motivation different operating stage, so as to achieve the purpose that widen operation window.
In various hydrogen-storing materials, the most widely used is all kinds of cerium-based oxygen storage materials.It is continuous with discharge standard
It improves, people propose the Oxygen storage capacity of hydrogen-storing material higher requirement, how to improve the oxygen storage capacity of material
(Oxygen Storage Capacity, OSC）Become one of emphasis of concern.Two-dimension nano materials are relative to common
Nano particle has preferably storage oxygen capacity (Angew. Chem. Int. Ed., 2011,50 (19), 4378-4381)
, therefore how research synthesizes the two-dimentional cerium-based oxygen storage material with high storage oxygen capacity with important significance of scientific research.
Invention content
The purpose of the present invention：A kind of low cost, the preparation method of the nano-sheet cerium sill of height storage oxygen capacity are provided.
In order to achieve the above object, present invention employs following schemes to realize：
The preparation of nano-sheet cerium oxide.
3-4 mmol solubility cerous salts are dissolved in 10-30 ml water at room temperature, are added with stirring 1-2 ml ammonia
Water, 1-2 g ammonium sulfate powders, 0.05-1.00 g sodium sulfite powder.Mixed system is transferred to 50 after being sufficiently mixed
In autoclaves of the ml with polytetrafluoroethyllining lining, reacted 12-20 hours at 120-200 DEG C.Gained is precipitated via suction filtration,
It after being washed with water, is scattered in the sodium hydroxide solution of about 0.4 mol/L, stirs 8-12 hours, until precipitation is in light yellow.It is heavy
It forms sediment and is detached again through filtering, washing and drying is required product.
The preparation of nano-sheet lanthanum cerium Hydroxysulfate.
Six water lanthanum chlorides of 3.2-6.4 mmol and 0.8-1.6 mmol solubility cerous salts are dissolved in about 30 at room temperature
In ml water, it is added with stirring 1-2 ml ammonium hydroxide, 1-2 g ammonium sulfate powders, 0.05-1 g sodium sulfite powder.After being sufficiently mixed
Mixed system is transferred in 50 autoclaves of the ml with polytetrafluoroethyllining lining, reacts 12- at 120-200 DEG C
20 hours.Gained is precipitated via suction filtration, after being washed with water, is scattered in the sodium hydroxide solution of about 0.3-0.5 mol/L, is stirred
It mixes 8-12 hours, until precipitation is in light yellow.Precipitation detaches again through filtering, and washing and drying is required product.
Preferably, scheme 1, soluble cerous salt used is seven water cerous chlorates or cerous sulfate in 2.
The invention has the advantages that：
The nano-sheet hydrogen-storing material does not need to any template, does not add organic solvent, and preparation process is substantially pollution-free.
Gained platy cerium oxide stores up oxygen capacity in 200 μm of ol O2/ more than g, about 600 μm of ol of sheet lanthanum cerium Hydroxysulfate storage oxygen capacity
O2/ g, storage oxygen capacity are with the obvious advantage in similar hydrogen-storing material.
Description of the drawings
Fig. 1 is the TEM figures of present invention gained nano-sheet cerium oxide.
Fig. 2 is the TEM figures of present invention gained nano-sheet lanthanum cerium Hydroxysulfate.
Specific embodiment
In order to better illustrate the present invention, technical scheme of the present invention is easy to understand, of the invention is typical but non-limiting
Case study on implementation it is as follows（Experimental method in following embodiments is conventional method unless otherwise specified.In following embodiments
Test material, be to be commercially available from conventional chemical reagent shop unless otherwise specified）：
Case study on implementation one：
The preparation of nano-sheet cerium oxide.
4 mmol, seven water cerous chlorates are dissolved in about 30 ml water at room temperature, it is dense to be added with stirring 28% volumes of 2ml
Spend ammonium hydroxide, 2g ammonium sulfate powders, 0.05g sodium sulfite powder.Mixed system is transferred to 50 ml bands after being sufficiently mixed
In the autoclave of polytetrafluoroethyllining lining, reacted 20 hours at 200 DEG C.Gained precipitation is via suction filtration, after being washed with water,
It is scattered in the sodium hydroxide solution of about 0.4 mol/L, stirs 12 hours, until precipitation is in light yellow.Precipitation is divided again through filtering
From washing and drying is required product.Product is as shown in Figure 1.
Case study on implementation two：
The preparation of nano-sheet lanthanum cerium Hydroxysulfate.
6.4 mmol, six water lanthanum chlorides and 1.6 mmol, seven water cerous chlorates are dissolved in about 30 ml water at room temperature, stirring
Lower addition 28% volumetric concentration ammonium hydroxide of 2ml, 2g ammonium sulfate powders, 0.05g sodium sulfite powder.After being mixed after being sufficiently mixed
System be transferred in 50 autoclaves of the ml with polytetrafluoroethyllining lining, reacted 20 hours at 200 DEG C.Gained precipitates
It via suction filtration, after being washed with water, is scattered in the sodium hydroxide solution of about 0.4 mol/L, stirs 12 hours, until precipitation is in shallow
Yellow.Precipitation detaches again through filtering, and washing and drying is required product.Product is as shown in Figure 2 at this time.
Case study on implementation three：
The preparation of nano-sheet cerium oxide.
4 mmol cerous sulfates are dissolved in about 30 ml water at room temperature, are added with stirring 28% volumetric concentration ammonia of 2ml
Water, 2g ammonium sulfate powders, 0.05g sodium sulfite powder.Mixed system is transferred to 50 ml with poly- four after being sufficiently mixed
In the autoclave of vinyl fluoride liner, reacted 12 hours at 120 DEG C.Gained precipitation is via suction filtration, after being washed with water, dispersion
It in the sodium hydroxide solution of about 0.4 mol/L, stirs 12 hours, until precipitation is in light yellow.Precipitation detaches again through filtering, water
It is required product to wash dry.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of hydro-thermal method prepares nanoscale sheet cerium oxide or the method for lanthanum cerium Hydroxysulfate, which is characterized in that nanoscale
The preparation method of platy cerium oxide or lanthanum cerium Hydroxysulfate includes the following steps：
1) soluble cerous salt and lanthanum chloride are dissolved in 10-30 ml water at room temperature, are added with stirring 1-2 ml ammonium hydroxide,
1-2 g ammonium sulfate powders, 0.05-1.00 g sodium sulfite powder；Mixed system is transferred to 50 ml after being sufficiently mixed
In autoclave with polytetrafluoroethyllining lining, add water to liquid level and reach at wall height 4/5, react 12- at 120-200 DEG C
20 hours；
2) by step 1）Gained is precipitated via suction filtration, after being washed with water, is scattered in the sodium hydroxide solution of 0.3-0.5 mol/L
In, it stirs 8-12 hours, until precipitation is in light yellow；Precipitation detaches again through filtering, and washing and drying is required product；
3）When preparing nanoscale sheet cerium oxide, lanthanum chloride is added without, step is with preparing nano-grade lanthanum cerium hydroxyl sulphur
Hydrochlorate is identical.
2. hydro-thermal method described in claim 1 prepares nanoscale sheet cerium oxide or the method for lanthanum cerium Hydroxysulfate, feature
It is, soluble cerous salt is cerous chlorate or cerous sulfate in step 1)；
In step 1), when preparing platy cerium oxide, soluble cerous salt dosage is 3-4 mmol；Prepare lanthanum cerium sulfovinic acid
During salt, lanthanum chloride dosage is 3.2-6.4 mmol and soluble cerous salt dosage is 0.8-1.6 mmol, lanthanum chloride and cerium salt
Molar ratio is 4：1.
3. a kind of hydro-thermal method as described in claim 1 to 2 any one prepares nanoscale sheet cerium oxide or lanthanum cerium hydroxyl sulphur
Cerium oxide or lanthanum cerium Hydroxysulfate prepared by the method for hydrochlorate.
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| CN106006703B true CN106006703B (en) | 2018-06-26 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106542560B (en) * | 2016-10-27 | 2017-12-29 | 东北大学 | A kind of preparation method of rare earth oxysulfate |
| CN106495200B (en) * | 2016-10-27 | 2017-12-29 | 东北大学 | A kind of anhydrous slufuric acid salt form rare earth layered hydroxide and preparation method thereof |
| CN107473256B (en) * | 2017-08-23 | 2019-04-05 | 电子科技大学 | A kind of Ce1-xZrxO2Nanometer sheet material and preparation method thereof |
| CN108178179A (en) * | 2018-01-31 | 2018-06-19 | 江苏大学 | A kind of cerium lanthanum solid solution nanometer rods preparation method of high-temperature stable and its application as catalyst carrier |
| CN110359043B (en) * | 2019-07-27 | 2021-03-26 | 西北师范大学 | Preparation method of titanium-based lanthanum oxide nanoflower film with dielectric wetting low-voltage response |
| CN115228396B (en) * | 2022-07-26 | 2024-02-02 | 宣城市晶和环保新材料科技有限公司 | Preparation method of nano cerium sol |
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| CN1335349A (en) * | 2000-07-21 | 2002-02-13 | 中国科学技术大学 | Rare earth subsulfate luminous material and its hot synthesis in solvent |
| KR100787346B1 (en) * | 2005-08-31 | 2007-12-18 | 주식회사 엘지화학 | Method for preparing cerium oxide |
| CN101734706B (en) * | 2009-12-25 | 2012-05-30 | 中国科学院上海微***与信息技术研究所 | Method for preparing diamond platy cerium oxide |
| CN102992376A (en) * | 2011-09-15 | 2013-03-27 | 华东理工大学 | Preparation method of sheet-shaped nano-grade cerium oxide |
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