CN101584981A - Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure - Google Patents
Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure Download PDFInfo
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- CN101584981A CN101584981A CNA2009100627036A CN200910062703A CN101584981A CN 101584981 A CN101584981 A CN 101584981A CN A2009100627036 A CNA2009100627036 A CN A2009100627036A CN 200910062703 A CN200910062703 A CN 200910062703A CN 101584981 A CN101584981 A CN 101584981A
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Abstract
The invention discloses a low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure. The non-aqueous system low-temperature preparation method is used and cerium chloride, ammonium ceric nitrate, cerium nitrate or cerium sulfate is used as the precursor and benzyl alcohol is used as solvent and surfactant and the raw materials react for a certain time in oil-bath heating condition to obtain the ceria nano-crystalline microsphere powder of graduation structure. The prepared ceria has three-dimensional graduation spheroidal structure. The ceria nano-crystalline microsphere powder of graduation structure can quickly and effectively absorb the inorganic and organic pollutant in waste water at room temperature with very high absorption capacity. The low-temperature preparation method has features of simple technology, low cost, friendly environment, high yield, accordance with the practical production requirement.
Description
Technical field
The present invention relates to the low temperature preparation method of ceria sorbing material, be specially graded structure ceria nano-crystalline microsphere powder sorbing material the non-aqueous system low temperature preparation method.
Background technology
The rare earth resources of China is very abundant, and commercial reserves is the first in the world.Among this, ceria is as a kind of rare earth compound, account for rare earth proved reserves about 50%.It has important purposes at aspects such as the catalytic pyrolysis of purifying vehicle exhaust processing, solid fuel cell, metal oxidation resistance, erosion shield and additive, fluid and chemically mechanical polishing grinding agents.
Because the skin effect that nano material had makes nano material have high surface-active, high surface energy and high specific area, so nano material is showing great potential aspect the preparation high-performance sorbing material.In environmental improvement was used, the metal oxide materials of nanostructured had very big specific area and favorable mechanical performance, was suitable for adsorbing the harmful substance of eliminating in the environment, for example can be used for the heavy metal ion etc. in the adsorbed water.A kind of good adsorbent, condition such as it is big to satisfy specific area, and inside has the micro channel of network structure, and adsorption capacity is big, and the three-dimensional nanometer material of graded structure can satisfy these requirements.According to bibliographical information, three-dimensional flower-shaped ceria can effectively be removed the chromium (VI) in the waste water, and is however, but less relatively about the report of three-dimensional structure cerium dioxide nano material.
Document [Chemistry of Materials, 2007,19 (7), 1648-1655] reported the preparation method of three-dimensional flower-shaped ceria, wherein weak point is to adopt surfactant to make the surface complicated, increase cost, and material require can obtain just after 450 ℃ of high-temperature calcinations, energy consumption is very big.Document [Chemistry-A European Journal; 2008; 14; 3380-3390] reported ammonium ceric nitrate Rapid Thermal decomposition reaction in oleic acid and oleyl amine mixed solvent; prepared colored shape ceria nano-crystalline; but should syntheticly need just can finish under inert gas shielding, synthesis temperature be also than higher.Therefore, the cryogenic conditions method of synthesizing with a step down three-dimensional cerium dioxide nano material for preparing graded structure remains a challenge to people.
This raw material of Chinese patent CN101168447A cerium-based, alcohol obtain presoma as organic solvent after solvent thermal reaction a period of time, high temperature obtains the three-dimensional structure ceria that six square rods are formed after the calcining down.Patent CN101117233A has introduced the preparation method who produces high specific surface area meso-porous cerium dioxide micro-balloon: with (NH
4)
2Ce (NO
3)
4Be dissolved in the absolute ethyl alcohol, add N again after the adding acid, dinethylformamide obtains presoma Ce (COOH) after the hydro-thermal
3, obtain the meso-porous cerium dioxide micro-balloon powder after presoma is at high temperature calcined.But above-mentioned two kinds of method complex process, operating procedure is many, equipment investment is big, energy consumption is very big, is unfavorable for suitability for industrialized production and application, so developing low-cost to prepare the method for cerium dioxide nano powder of three-dimensional structure significant.
By contrast, the variety of raw material that uses in the preparation process of the present invention is few, cost of material is cheap, operating process is simple, it is low that equipment requires, and particularly do not need high-temperature process, economical rationality and do not introduce other metal impurities ion, entire reaction is all carried out in non-aqueous system, is convenient to the purification of later stage product.Preparation technology is simple, control easily, and good reproducibility is convenient to large-scale production.
Summary of the invention
The object of the invention is intended to overcome deficiency of the prior art, and a kind of preparation method of ceria nano-crystalline microsphere powder of graded structure is provided.The ceria that synthesizes with the inventive method is used as sorbing material, and good adsorption property is arranged.
The preparation method of the ceria nano-crystalline microsphere powder sorbing material of graded structure of the present invention, the non-aqueous system preparation method is characterized in that may further comprise the steps:
(1) cerium compound at room temperature is dissolved in the phenmethylol, forming concentration is the colorless cleared solution of 0.05 mol～0.1 mol;
(2) colorless cleared solution that (1) is obtained places flask, and the oil bath heat treated is 36～60 hours in 100～130 ℃ atmosphere, must precipitate;
(3) precipitation that (2) are obtained is through ethanol washing back separation, and drying obtains the ceria nano-crystalline microsphere powder sorbing material of khaki graded structure.
The compound of above-mentioned cerium is inorganic cerium compound: cerium chloride, ammonium ceric nitrate, cerous nitrate or cerous sulfate.
Effect of the present invention and advantage:
1. adopt the ceria nano-crystalline microsphere powder of the graded structure that the inventive method obtains, provide new sorbing material for carrying out environmental pollution improvement.
2. whole technical process is simple and easy to control, and power consumption is few, the productive rate height, and cost is low, and realistic production needs.
3. compare with the synthetic method of the cerium dioxide nano material of the three-dimensional structure of former document and patent report, this synthesis condition gentleness, power consumption is few, and is simple, product purity height, steady quality.And product can effectively adsorb the noxious material in the waste water at short notice fast, for it realizes that industrial applications provides the foundation.
Further the present invention will be described below in conjunction with drawings and Examples.
Description of drawings
Fig. 1 is the XRD diffraction pattern of embodiment 1 gained powder, the diffraction maximum correspondence be to be numbered (JCPDS, ceria 75-120).
Fig. 2 and Fig. 3 are respectively the SEM and the TEM figure of embodiment 1 gained powder, contrast these two figure as can be seen, and prepared ceria has three-dimensional graded structure, and sample has kept sphere and hemispherical pattern preferably.
Fig. 4 is that the ceria sample of embodiment 1 gained adsorbs the effect comparison diagram that variable concentrations contains chromium (VI) in chromium (VI) waste water under the property condition at room temperature, and adsorption capacity is represented the amount of the adsorbents adsorb chromium (VI) of every gram.
Fig. 5 is that the at room temperature different rhodamine Bs constantly of the sample of gained among the embodiment 1 are adsorbed the pairing uv absorption spectra that fades.
The absorption property test of the ceria nano-crystalline microsphere powder of graded structure characterizes by at room temperature adsorbing chromium (VI) and rhodamine B.The concentration that contains chromium (VI) waste water is 4 mg/litre and 8 mg/litre successively, and volume is 100 milliliters, and the concentration of adsorbent is every liter of 1 gram, and after 4 hours absorption, adsorption efficiency is all more than 80%.The concentration of rhodamine B solution is 5 mg/litre, and volume is 100 milliliters, and the concentration of adsorbent is every liter of 1 gram, and after adsorbing 1 hour, rhodamine B has been adsorbed 95%.
The specific embodiment
Embodiment 1
Cerous nitrate is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, cerous nitrate concentration is 0.05 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 36 hours in 100 ℃ oil bath, formation khaki precipitation is with the ceria nano-crystalline microsphere powder that precipitation is separated after the ethanol washing, oven dry just can obtain high-purity graded structure under 50 ℃ of conditions that obtains.
Embodiment 2
Cerous nitrate is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, the concentration of cerous nitrate is 0.05 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 48 hours in 100 ℃ oil bath, formation khaki precipitation is with the precipitation separation after the ethanol washing that obtains, the ceria nano-crystalline microsphere powder that just can obtain high-purity graded structure after 50 ℃ of following dryings.
Embodiment 3
Cerous nitrate is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, the concentration of cerous nitrate is 0.1 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 60 hours in 120 ℃ oil bath, formation khaki precipitation is with the precipitation separation after the ethanol washing that obtains, the ceria nano-crystalline microsphere powder that just can obtain high-purity graded structure after drying under 50 ℃ of C.
Embodiment 4
Cerous nitrate is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, the concentration of cerous nitrate is 0.1 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 36 hours in 130 ℃ oil bath, formation khaki precipitation is with the precipitation separation after the ethanol washing that obtains, the ceria nano-crystalline microsphere powder that just can obtain high-purity graded structure after 50 ℃ of following dryings.
Embodiment 5
Cerous nitrate is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, the concentration of cerous nitrate is 0.1 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 60 hours in 130 ℃ oil bath, formation khaki precipitation is with the precipitation separation after the ethanol washing that obtains, the ceria nano-crystalline microsphere powder that just can obtain high-purity graded structure after 50 ℃ of following dryings.
Embodiment 6
Cerous nitrate is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, the concentration of cerous nitrate is 0.07 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 40 hours in 110 ℃ oil bath, formation khaki precipitation is with the precipitation separation after the ethanol washing that obtains, the ceria nano-crystalline microsphere powder that just can obtain high-purity graded structure after 50 ℃ of following dryings.
Embodiment 7
Cerium chloride is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, cerium chloride concentration is 0.05 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 46 hours in 100 ℃ oil bath, formation khaki precipitation is with the ceria nano-crystalline microsphere powder that precipitation is separated after the ethanol washing, oven dry just can obtain high-purity graded structure under 50 ℃ of conditions that obtains.
Ammonium ceric nitrate is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, the concentration of ammonium ceric nitrate is 0.1 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 50 hours in 120 ℃ oil bath, formation khaki precipitation is with the precipitation separation after the ethanol washing that obtains, the ceria nano-crystalline microsphere powder that just can obtain high-purity graded structure after 50 ℃ of following dryings.
Embodiment 9
Cerous sulfate is added in 10 milliliters of phenmethylols, at room temperature form colorless cleared solution after the magnetic agitation, the concentration of cerous sulfate is 0.08 mol, then colorless cleared solution is placed flask, the heating stirring reaction is 50 hours in 130 ℃ oil bath, formation khaki precipitation is with the precipitation separation after the ethanol washing that obtains, the ceria nano-crystalline microsphere powder that just can obtain high-purity graded structure after drying under 50 ℃ of C.
The absorption property test of the ceria nano-crystalline microsphere powder of the prepared graded structure of embodiment 1-9 characterizes by at room temperature adsorbing chromium (VI) and rhodamine B.The concentration that contains chromium (VI) waste water is 4 mg/litre and 8 mg/litre successively, and volume is 100 milliliters, and the concentration of adsorbent is every liter of 1 gram, and after 4 hours absorption, adsorption efficiency is all more than 80%.The concentration of rhodamine B solution is 5 mg/litre, and volume is 100 milliliters, and the concentration of adsorbent is every liter of 1 gram, and after adsorbing 1 hour, rhodamine B has been adsorbed 95%.
Claims (2)
1. the preparation method of the ceria nano-crystalline microsphere powder sorbing material of graded structure, the non-aqueous system preparation method is characterized in that may further comprise the steps:
(1) cerium compound at room temperature is dissolved in the phenmethylol, forming concentration is the colorless cleared solution of 0.05 mol～0.1 mol;
(2) colorless cleared solution that (1) is obtained places flask, and the oil bath heat treated is 36～60 hours in 100～130 ℃ atmosphere, must precipitate;
(3) precipitation that (2) are obtained is through ethanol washing back separation, and drying obtains the ceria nano-crystalline microsphere powder sorbing material of khaki graded structure.
2. the preparation method of the ceria nano-crystalline microsphere powder sorbing material of graded structure according to claim 1 is characterized in that described cerium compound is cerium chloride, ammonium ceric nitrate, cerous nitrate or cerous sulfate.
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| 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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| CN106145955A (en) * | 2016-08-08 | 2016-11-23 | 屠秀芬 | The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics |
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