A kind of micro-nano structure CeCO3The preparation process of OH
阅读说明：本技术 一种微纳结构CeCO3OH的制备工艺 (A kind of micro-nano structure CeCO3The preparation process of OH ) 是由 兰苑培 李军旗 陈朝轶 夏雪雯 毛锡嵩 顾小英 于 2019-08-28 设计创作，主要内容包括：本发明公开了一种微纳结构CeCO_3OH的制备工艺,是以铈盐作为前驱体,通过水热法合成制备杏仁型或中空球形结构的CeCO_3OH超细粉体材料。本发明具有CeCO_3OH形貌可调,尺寸均匀,分散性好,制备工艺简单的特点。(The invention discloses a kind of micro-nano structure CeCO 3 The preparation process of OH is that the CeCO of almond type or hollow sphere structure is synthetically prepared by hydro-thermal method using cerium salt as presoma 3 OH superfine powdery material.The present invention has CeCO 3 OH pattern is adjustable, of uniform size, good dispersion, the simple feature of preparation process.)
1. a kind of micro-nano structure CeCO3The preparation process of OH, it is characterised in that: be to be closed using cerium salt as presoma by hydro-thermal method At the CeCO for preparing almond type or hollow sphere structure3OH superfine powdery material.
2. micro-nano structure CeCO according to claim 13The preparation process of OH, which is characterized in that specific step is as follows:
1) cerium salt is dissolved in distilled water, stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and dehydrated alcohol is added, stirring obtains B product to clear solution is formed；
3) A product and B product are mixed, stirring then proceedes to stirring slurry 0.1-1h, obtain C product to white " milky " slurries are formed；
4) C product are put into autoclave sealing, and pressurized, heated is handled, after treatment cooled to room temperature obtains D product；
5) it will be filtered after the washing of D product, and white depositions be obtained, up to CeCO after white depositions are dried3OH superfine powdery material.
3. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: cerium salt described in step 1) is Ce(NO3)3·6H2O or CeCl3·7H2O。
4. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: bicarbonate described in step 2 The molar ratio of ammonium and dehydrated alcohol is 3:0.1-0.5.
5. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: A product and B described in step 3) When product mix, cerium salt and the molar ratio of ammonium hydrogen carbonate in B product are 0.1-1:3 in A product.
6. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: the cream of white described in step 3) Shape slurries use magnetic agitation.
7. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: heating described in step 4) adds When pressure processing, pressure 0.5-3MPa, temperature are 80-180 DEG C, handle time 12-48h.
8. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: washing described in step 5) is It is alternately washed using distilled water and dehydrated alcohol.
9. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: drying described in step 5) is adopted With vacuum drying, drying temperature is 30-40 DEG C, time 10-15h.
10. micro-nano structure CeCO according to claim 1 or 23The preparation process of OH, it is characterised in that: the CeCO3OH The average-size of superfine powdery material is 0.2-1.5 μm.
Technical field
The present invention relates to a kind of CeCO3The preparation process of OH, especially a kind of micro-nano structure CeCO3The preparation process of OH.
Background technique
Ce elements are the rare earth elements that reserves are most in the earth's crust, and the chemical combination of Ce elements has preferable functionalized application way Diameter.Cerous carbonate hydroxide (CeCO3It OH is) a kind of important functional material, it, which is provided not only, is different from structure and pattern Relevant unique optical properties and there is novel electronic property and chemical property, and CeCO3OH microstructure is excellent in Electrochemical reversibility, this be it is many application (such as lithium ion battery) important feature.Specifically CeCO3OH different structures There is different performances to can be used for different applications, and the CeCO of different-shape with pattern3OH can be by simply thermally decomposing guarantor Hold pattern it is constant in the case where prepare CeO2If nano Ce CO may be implemented3The control of OH crystal structure and pattern synthesizes, just It is likely to occur more applications and new functional material.
In recent years, the nano Ce CO of different-shape has been synthesized using different methods3OH, such as self assembly, sonochemistry, water Hot and microwave-assisted hydro-thermal method.In all preparation methods, hydro-thermal method is because its synthesis temperature is low, high powdered reaction and diversification The advantages of pattern controls is considered as a kind of preparation method of efficient and cost-effective.It is most of about nanometer in hydrothermal system CeCO3The report of OH Opacity in lens is using CO (NH2)2Alkali and carbon source, and surfactant or template are added to adjust CeCO3It is prepared by the nucleation of OH particle and crystal growth.This makes process complicated, and the cost of raw material is higher.
Report preparation CeCO in domestic and foreign literature at present3The pattern of OH mainly has needle-shaped, rodlike, triangle etc., and apricot Benevolence shape and spherical shape CeCO3The preparation of OH has not been reported, and pattern is to CeCO3OH, and to the CeO that decomposition obtains2Performance it is equal There is important influence.
In addition, China is rare earth big country, a large amount of rare earth resources export to after exploitation, refinement and are dealt into country, added Work becomes high added value rare-earth products.Rare earth resources develop the preparation process of high added value rare-earth products as important resource It is most important to current China with product.And CeCO3OH is as a kind of important potential rare-earth products of tool, high-quality CeCO3The Study on Preparation of OH is also of great significance to the comprehensive technological development of China's rare-earth trade and deposit.
Therefore, the present invention develops a kind of micro-nano structure CeCO3The technique of preparation and the regulation of OH, prepared CeCO3OH Pattern, of uniform size, dispersion performance is good, and preparation process simply has preferable prospects for commercial application.
Summary of the invention
The object of the present invention is to provide a kind of micro-nano structure CeCO3The preparation process of OH.The present invention has CeCO3OH shape Looks are adjustable, of uniform size, good dispersion, the simple feature of preparation process.
A kind of technical solution of the present invention: micro-nano structure CeCO3The preparation process of OH is led to using cerium salt as presoma Cross the CeCO that hydro-thermal method is synthetically prepared almond type or hollow sphere structure3OH superfine powdery material.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the specific steps are as follows:
1) cerium salt is dissolved in distilled water, stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and dehydrated alcohol is added, stirring obtains B product to clear solution is formed；
3) A product and B product are mixed, stirring then proceedes to stirring slurry 0.1-1h, obtain C to white " milky " slurries are formed Product；
4) C product are put into autoclave sealing, and pressurized, heated is handled, after treatment cooled to room temperature obtains D Product；
5) it will be filtered after the washing of D product, and white depositions be obtained, up to CeCO after white depositions are dried3OH superfine powder Material.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the step 1) cerium salt are Ce (NO3)3·6H2O or CeCl3·7H2O。
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the molar ratio of step 2) ammonium hydrogen carbonate and dehydrated alcohol For 3:0.1-0.5.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, when step 3) the A product and B product mix, in A product cerium salt with The molar ratio of ammonium hydrogen carbonate is 0.1-1:3 in B product.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, step 3) the white " milky " slurries use magnetic agitation.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, when step 4) the heating pressurized treatments, pressure 0.5- 3MPa, temperature are 80-180 DEG C, handle time 12-48h.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the step 5) washing is using distilled water and dehydrated alcohol Alternately wash.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, step 5) is described dry using vacuum drying, and drying temperature is 30-40 DEG C, time 10-15h.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the CeCO3The average-size of OH superfine powdery material is 0.2-1.5μm。
Beneficial effects of the present invention
1, CeCO can be realized on the basis of regulating and controlling different technological parameters by same set of technique in the present invention3OH shape The CeCO of almond type or hollow sphere structure is prepared in the adjusting of looks3OH superfine powdery material, extends CeCO3OH superfine powder Material morphology structure type, pattern remains unchanged after roasting, has filled up amygdaloidal, hollow sphere CeCO3The preparation of OH micro-nano structure Technological gap, to China's rare earth material exploitation and high added value rare-earth products exploitation all have significance；
2, CeCO produced by the present invention3OH superfine powdery material is of uniform size, and between 0.2-1.5 μm, dispersion performance is good；
3, the present invention uses hydro-thermal law technology, and method is simple, easy to operate, has the characteristics that mass production and advantage.
Detailed description of the invention
Attached drawing 1 is amygdaloidal CeCO produced by the present invention3The SEM of OH superfine powdery material schemes；
Attached drawing 2 is amygdaloidal CeCO produced by the present invention3The XRD diagram of OH superfine powdery material；
Attached drawing 3 is the CeCO of hollow sphere produced by the present invention3The SEM of OH superfine powdery material schemes；
Attached drawing 4 is the CeCO of hollow sphere produced by the present invention3The XRD diagram of OH superfine powdery material.
It can be seen that produced by the present invention amygdaloidal and hollow sphere CeCO from Fig. 1 and Fig. 33OH superfine powdery material Shape and size more uniformly, dispersibility preferably.And its corresponding crystal phase can be seen that by Fig. 2 and Fig. 4.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention