CN106006703A - Method for preparing nano flaky cerium oxide and lanthanum-cerium hydroxysulfate by hydrothermal process - Google Patents
Method for preparing nano flaky cerium oxide and lanthanum-cerium hydroxysulfate by hydrothermal process Download PDFInfo
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- CN106006703A CN106006703A CN201610352324.0A CN201610352324A CN106006703A CN 106006703 A CN106006703 A CN 106006703A CN 201610352324 A CN201610352324 A CN 201610352324A CN 106006703 A CN106006703 A CN 106006703A
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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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- Condensed Matter Physics & Semiconductors (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a method for preparing nano flaky cerium oxide and lanthanum-cerium hydroxysulfate by a hydrothermal process. The method comprises the following steps: firstly, taking cerous salt and lanthanum chloride as precursors and ammonia water and ammonium sulfate as precipitating agents, and carrying out reaction for 12-20 hours at 120-200 DEG C by a hydrothermal mode to obtain an intermediate product; stirring the obtained intermediate product for 8-12 hours in a 0.4mol/L sodium hydroxide solution in an ion exchange mode; and finally, carrying out separation and washing to obtain a nano flaky oxygen storage material. The method provided by the invention has the advantages that no template is needed, no organic solvent is added, the preparation process is basically pollution-free, and the product has good application prospects in the aspect of novel three-way catalysts.
Description
Technical field
The invention belongs to technical field of inorganic nano-material preparation, prepare nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate particularly to a kind of hydro-thermal method.
Background technology
In recent years, one of vehicle exhaust main source becoming air pollution, control and administer the important topic that automobile exhaust pollution has become the most global.Since 20 century 70s, three-way catalyst (Three Way Conversion Catalyst,
TWC) the most effective means of motor vehicle tail-gas purifying have just been become.In three-way catalyst, hydrogen-storing material is a pith of composition catalyst, determines performance and the life-span of catalyst.The most important effect of hydrogen-storing material is to realize the active oxygen storage of different work phases and release, thus reaches to widen the purpose of operation window.
In various hydrogen-storing materials, the most widely used is all kinds of cerium-based oxygen storage materials.Along with improving constantly of discharge standard, the Oxygen storage capacity of hydrogen-storing material is had higher requirement by people, how to improve material oxygen storage capacity (Oxygen Storage Capacity,
OSC) one of emphasis of concern is become.Two-dimension nano materials has relative to common nanoparticle and preferably stores up oxygen capacity (Angew.
Chem. Int. Ed., 2011,50 (19), 4378-4381), therefore study how to synthesize and there is the two-dimentional cerium-based oxygen storage material of high storage oxygen capacity there is important significance of scientific research.
Summary of the invention
The purpose of the present invention: a kind of low cost, the preparation method of the nano-sheet cerio material of high storage oxygen capacity are provided.
In order to achieve the above object, present invention employs following scheme to realize:
The preparation of nano-sheet cerium oxide.
By 3-4 mmol under room temperature
Solubility cerous salt is dissolved in 10-30 ml water, and stirring is lower adds 1-2 ml ammonia, 1-2 g ammonium sulfate powder, 0.05-1.00 g sodium sulfite powder.After being sufficiently mixed, mixed system is transferred in 50 ml band teflon-lined autoclaves, react 12-20 hour at 120-200 DEG C.Gained precipitates via sucking filtration, after washing with water, is scattered in the sodium hydroxide solution of about 0.4 mol/L, stirs 8-12 hour, to precipitation in light yellow.Precipitation separates through sucking filtration again, and washing and drying is required product.
The preparation of nano-sheet lanthanum cerium Hydroxysulfate.
Under room temperature, 3.2-6.4 mmol six water lanthanum chloride and 0.8-1.6 mmol solubility cerous salt are dissolved in about 30 ml water, and stirring is lower adds 1-2 ml ammonia, 1-2 g ammonium sulfate powder, 0.05-1 g sodium sulfite powder.After being sufficiently mixed, mixed system is transferred in 50 ml band teflon-lined autoclaves, react 12-20 hour at 120-200 DEG C.Gained precipitates via sucking filtration, after washing with water, is scattered in the sodium hydroxide solution of about 0.3-0.5 mol/L, stirs 8-12 hour, to precipitation in light yellow.Precipitation separates through sucking filtration again, and washing and drying is required product.
Preferably, scheme 1, in 2, solubility cerous salt used is seven water cerous chlorate or cerous sulfates.
Present invention have the advantage that
Described nano-sheet hydrogen-storing material need not any template, and without organic solvent, preparation technology is the most pollution-free.Gained platy cerium oxide storage oxygen capacity is at 200 μm ol O2/ more than g, lamellar lanthanum cerium Hydroxysulfate storage oxygen capacity about 600 μm ol O2/ g, its storage oxygen capacity is with the obvious advantage in similar hydrogen-storing material.
Accompanying drawing explanation
Fig. 1 is the TEM figure of gained nano-sheet cerium oxide of the present invention.
Fig. 2 is the TEM figure of gained nano-sheet lanthanum cerium Hydroxysulfate of the present invention.
Detailed description of the invention
In order to better illustrate the present invention, it is simple to understand technical scheme, the typical case of the present invention but the case study on implementation of indefiniteness are following, and (experimental technique in following embodiment if no special instructions, is conventional method.Test material in following embodiment, if no special instructions, is and is commercially available from conventional chemical reagent shop):
Case study on implementation one:
The preparation of nano-sheet cerium oxide.
By 4 mmol under room temperature
Seven water cerous chlorates are dissolved in about 30 ml water, and stirring is lower adds 2ml 28% volumetric concentration ammonia, 2g ammonium sulfate powder, 0.05g sodium sulfite powder.After being sufficiently mixed, mixed system is transferred in 50 ml band teflon-lined autoclaves, react 20 hours at 200 DEG C.Gained precipitates via sucking filtration, after washing with water, is scattered in the sodium hydroxide solution of about 0.4 mol/L, stirs 12 hours, to precipitation in light yellow.Precipitation separates through sucking filtration again, and 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 under room temperature
Six water lanthanum chloride and 1.6 mmol seven water cerous chlorates are dissolved in about 30 ml water, and stirring is lower adds 2ml 28% volumetric concentration ammonia, 2g ammonium sulfate powder, 0.05g sodium sulfite powder.After being sufficiently mixed, mixed system is transferred in 50 ml band teflon-lined autoclaves, react 20 hours at 200 DEG C.Gained precipitates via sucking filtration, after washing with water, is scattered in the sodium hydroxide solution of about 0.4 mol/L, stirs 12 hours, to precipitation in light yellow.Precipitation separates through sucking filtration again, and washing and drying is required product.Now product is as shown in Figure 2.
Case study on implementation three:
The preparation of nano-sheet cerium oxide.
By 4 mmol under room temperature
Cerous sulfate is dissolved in about 30 ml water, and stirring is lower adds 2ml 28% volumetric concentration ammonia, 2g ammonium sulfate powder, 0.05g sodium sulfite powder.After being sufficiently mixed, mixed system is transferred in 50 ml band teflon-lined autoclaves, react 12 hours at 120 DEG C.Gained precipitates via sucking filtration, after washing with water, is scattered in the sodium hydroxide solution of about 0.4 mol/L, stirs 12 hours, to precipitation in light yellow.Precipitation separates through sucking filtration again, and washing and drying is required product.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (7)
1. a hydro-thermal method prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate, it is characterised in that this hydro-thermal method is prepared the method for nanoscale sheet cerium oxide and lanthanum cerium Hydroxysulfate and comprised the following steps:
1) solubility cerous salt and lanthanum chloride being dissolved in 10-30 ml water under room temperature, stirring is lower adds 1-2 ml ammonia, 1-2 g ammonium sulfate powder, 0.05-1.00 g sodium sulfite powder；Transfer to mixed system after being sufficiently mixed, in 50 ml band teflon-lined autoclaves, add water to liquid level and reach at wall height about 4/5, react 12-20 hour at 120-200 DEG C；
2) step 1) gained is precipitated via sucking filtration, after washing with water, be scattered in the sodium hydroxide solution of 0.3-0.5 mol/L, stir 8-12 hour, to precipitation in light yellow；Precipitation separates through sucking filtration again, and washing and drying is required product.
2. hydro-thermal method described in claim 1 prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate, it is characterised in that step 1) in solubility cerous salt be preferably cerous chlorate or cerous sulfate.
3. hydro-thermal method described in claim 1 prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate, it is characterised in that step 1) in, when preparing platy cerium oxide, solubility cerous salt consumption is 3-4 mmol；When preparing lanthanum cerium Hydroxysulfate, lanthanum chloride consumption is 3.2-6.4 mmol and solubility cerous salt consumption is 0.8-1.6 mmol, and lanthanum chloride and cerium salt mol ratio are 4:1.
4. hydro-thermal method described in claim 1 prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate, it is characterised in that step 1) in ammonia volume be 1-2ml, ammonium sulfate consumption is at 1-2g, and sodium sulfite consumption is at 0.05-1.00g.
5. hydro-thermal method described in claim 1 prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate, it is characterised in that step 1) in hydrothermal temperature at 120-200 DEG C, the time is 12-20 hour.
6. hydro-thermal method described in claim 1 prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate, it is characterised in that step 2) in, process step 1 with sodium hydroxide solution) intermediate product 8-12 hour.
7. cerium oxide prepared by the method that the hydro-thermal method as described in claim 1 to 6 any one prepares nanoscale sheet cerium oxide and lanthanum cerium Hydroxysulfate and lanthanum cerium Hydroxysulfate.
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| CN201610352324.0A CN106006703B (en) | 2016-05-25 | 2016-05-25 | Hydro-thermal method prepares nanoscale sheet cerium oxide and the method for lanthanum cerium Hydroxysulfate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495200A (en) * | 2016-10-27 | 2017-03-15 | 东北大学 | A kind of anhydrous slufuric acid salt form rare earth layered hydroxide and preparation method thereof |
| CN106542560A (en) * | 2016-10-27 | 2017-03-29 | 东北大学 | A kind of preparation method of rare earth oxysulfate |
| CN107473256A (en) * | 2017-08-23 | 2017-12-15 | 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 |
| CN110359043A (en) * | 2019-07-27 | 2019-10-22 | 西北师范大学 | Dielectric soaks the preparation method of the titanium-based lanthana nano flower film of low-voltage response |
| CN115228396A (en) * | 2022-07-26 | 2022-10-25 | 宣城市晶和环保新材料科技有限公司 | Preparation method of nano cerium sol |
Citations (4)
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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 |
| KR20070025016A (en) * | 2005-08-31 | 2007-03-08 | 주식회사 엘지화학 | Method for preparing cerium oxide |
| CN101734706A (en) * | 2009-12-25 | 2010-06-16 | 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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2016
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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 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495200A (en) * | 2016-10-27 | 2017-03-15 | 东北大学 | A kind of anhydrous slufuric acid salt form rare earth layered hydroxide and preparation method thereof |
| CN106542560A (en) * | 2016-10-27 | 2017-03-29 | 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 |
| CN107473256A (en) * | 2017-08-23 | 2017-12-15 | 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 |
| CN110359043A (en) * | 2019-07-27 | 2019-10-22 | 西北师范大学 | Dielectric soaks the preparation method of the titanium-based lanthana nano flower film of low-voltage response |
| 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 |
| CN115228396A (en) * | 2022-07-26 | 2022-10-25 | 宣城市晶和环保新材料科技有限公司 | Preparation method of nano cerium sol |
| 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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