CN105251421A - Low-temperature preparation method for micron cerium oxide micro-ball - Google Patents
Low-temperature preparation method for micron cerium oxide micro-ball Download PDFInfo
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- CN105251421A CN105251421A CN201510800886.2A CN201510800886A CN105251421A CN 105251421 A CN105251421 A CN 105251421A CN 201510800886 A CN201510800886 A CN 201510800886A CN 105251421 A CN105251421 A CN 105251421A
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Abstract
The invention belongs to the field of rare earth material preparation and relates to a low-temperature preparation method for a micron cerium oxide micro-ball. The low-temperature preparation method comprises the following steps: (1) accurately weighting cerium nitrate hexahydrate and urea, respectively adding little de-ionized water, preparing into a cerium nitrate aqueous solution and a urea aqueous solution, mixing the two aqueous solutions, and then adding glycine betaine, adding some de-ionized water, stirring till completely dissolving, thereby forming a mixed solution, and controlling the concentration of the cerium ion in the mixed solution to be 4.35g/l, the concentration of the urea to be 2.4g/l and the concentration of the glycine betaine to be 1-12.g/l, wherein the mass ratio of cerium nitrate hexahydrate to urea is 1:4; (2) transferring the mixed solution into an airtight reaction vessel, increasing the temperature to 90 DEG C, stirring and reacting for 8-12h, thereby generating white precipitate; (3) centrifugally separating the white precipitate, washing for 4 times with absolute ethyl alcohol, and drying at 80 DEG C for 12h; and (4) heating the products acquired from the step (3), thereby acquiring the micron cerium oxide micro-ball with excellent dispersibility and uniform grain size.
Description
Technical field
The invention belongs to rare earth material preparation field, relate to a kind of low temperature preparation method of micron order cerium oxide microballoon.
Background technology
Cerium oxide is a kind of light rare earth oxide, have the advantages that activity is high, price is low, all be widely used in a lot of field, can be used as the three-way catalyst, SOFC, photocatalysis degradation organic contaminant material, UV absorbing material, lambda sensor etc. that process vehicle exhaust.The size of cerium oxide and pattern have certain influence to its performance, consider that microballoon has outstanding advantage in mobility, close heap, rub resistance etc. compared with the material of other shapes, so cerium oxide microballoon has the special nature that other cerium oxide powders do not possess, especially control the size of microballoon at 0.5 to 1 micron, it can have the double grading of nanostructured and micrometer structure concurrently.
Summary of the invention
The object of the present invention is to provide the low temperature preparation method of the cerium oxide microballoon of a kind of diameter between 0.5 ~ 1 μm, this preparation method's technique is simple, and reaction condition is gentle, adopts cerium oxide microballoon good dispersion, uniform particle sizes prepared by the method.
For realizing above-mentioned object, the technical solution used in the present invention is:
A low temperature preparation method for micron order cerium oxide microballoon, comprises the steps:
(1) six water cerous nitrate and urea are accurately taken, add a small amount of deionized water respectively, make the cerous nitrate aqueous solution and aqueous solution of urea, the ratio of the amount of substance of six water cerous nitrates and urea is 1:4, mix above-mentioned two kinds of aqueous solution, then add betaine wherein, then add a part of deionized water, stir and make it dissolve completely, form mixed solution, the concentration controlling cerium ion in mixed solution is 4.35g/L, and the concentration of urea is 2.4g/L, and beet paper mill wastewater is 1 ~ 1.2g/L;
(2) move in closed reaction vessel by mixed solution, be warmed up to 90 DEG C, stir, reaction 8 ~ 12h, produces white precipitate;
(3) centrifugation goes out white precipitate, with absolute ethanol washing 4 times, and dry 12h at 80 DEG C;
(4) heat-treated by the product that step (3) obtains, obtain the micron order cerium oxide microballoon of good dispersion, uniform particle sizes, the diameter of microballoon is 0.5 ~ 1 μm.
Preferably, described heat treatment comprises the steps: first to be warmed up to 220 DEG C with the programming rate of 20 DEG C/min, constant temperature 5min, and then is warmed up to 550 DEG C with the programming rate of 20 DEG C/min, calcining at constant temperature 2h, is finally cooled to room temperature, completes heat treatment process.
The beneficial effect that the present invention has:
(1) the cerium oxide microballoon good dispersion, the uniform particle sizes that adopt the inventive method to prepare;
(2) diameter of the cerium oxide microballoon adopting the inventive method to prepare can accurately control between 0.5 ~ 1 μm;
(3) preparation method's technique of the present invention is simple, and reaction condition is gentle.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the cerium oxide microballoon of embodiment 1;
Fig. 2 is the partial enlargement scanning electron microscope (SEM) photograph of Fig. 1;
Fig. 3 is the X-ray diffractogram of the cerium oxide microballoon of embodiment 1;
Fig. 4 is the scanning electron microscope (SEM) photograph of the cerium oxide microballoon of embodiment 2.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.
Embodiment 1
A low temperature preparation method for micron order cerium oxide microballoon, comprises the steps:
(1) six water cerous nitrate and urea are accurately taken, add a small amount of deionized water respectively, make the cerous nitrate aqueous solution and aqueous solution of urea, the ratio of the amount of substance of six water cerous nitrates and urea is 1:4, mix above-mentioned two kinds of aqueous solution, then add betaine wherein, then add a part of deionized water, stir and make it dissolve completely, form mixed solution, the concentration controlling cerium ion in mixed solution is 4.35g/L, and the concentration of urea is 2.4g/L, and beet paper mill wastewater is 1g/L;
(2) move in closed reaction vessel by mixed solution, be warmed up to 90 DEG C, stir, reaction 8h, produces white precipitate;
(3) centrifugation goes out white precipitate, absolute ethanol washing 4 times, finally by white precipitate dry 12h at 80 DEG C;
(4) product that step (3) obtains is heat-treated, heat treatment comprises the steps: first to be warmed up to 220 DEG C with the programming rate of 20 DEG C/min, constant temperature 5min, and then be warmed up to 550 DEG C with the programming rate of 20 DEG C/min, calcining at constant temperature 2h, finally be cooled to room temperature, complete heat treatment process, finally obtain micron order cerium oxide microballoon.
Characterize product prepared by the present embodiment, Fig. 1 is the scanning electron microscope (SEM) photograph of the present embodiment product, visible product good dispersion, uniform particle sizes, spherical in shape, the diameter of microballoon is 0.5 ~ 1 μm, Fig. 2 is the partial enlargement scanning electron microscope (SEM) photograph of Fig. 1, and show the pattern of single microballoon, spherical morphology is better.X-ray diffraction analysis being carried out to the product of the present embodiment, the X ray diffracting spectrum that Fig. 3 obtains, through contrasting with standard diagram, can determine that obtained product is cerium oxide.
Embodiment 2
A low temperature preparation method for micron order cerium oxide microballoon, comprises the steps:
(1) six water cerous nitrate and urea are accurately taken respectively, add a small amount of deionized water respectively, make the cerous nitrate aqueous solution and aqueous solution of urea, the ratio of the amount of substance of six water cerous nitrates and urea is 1:4, mix above-mentioned two kinds of aqueous solution, then add betaine wherein, then add a part of deionized water, stir and make it dissolve completely, form mixed solution, the concentration controlling cerium ion in mixed solution is 4.35g/L, and the concentration of urea is 2.4g/L, and beet paper mill wastewater is 1.2g/L;
(2) move in closed reaction vessel by mixed solution, be warmed up to 90 DEG C, stir, reaction 12h, produces white precipitate;
(3) centrifugation goes out white precipitate, absolute ethanol washing 4 times, finally by white precipitate dry 12h at 80 DEG C;
(4) product that step (3) obtains is heat-treated, heat treatment comprises the steps: first to be warmed up to 220 DEG C with the programming rate of 20 DEG C/min, constant temperature 5min, and then be warmed up to 550 DEG C with the programming rate of 20 DEG C/min, calcining at constant temperature 2h, finally be cooled to room temperature, complete heat treatment process, finally obtain micron order cerium oxide microballoon.
Characterize product prepared by the present embodiment, Fig. 4 is the scanning electron microscope (SEM) photograph of the present embodiment product, visible product good dispersion, and uniform particle sizes is spherical in shape, and the diameter of microballoon is 0.5 ~ 1 μm.
Above-described embodiment is only one of preferred embodiment of the present invention, not limits the scope of the invention with this, therefore: all equivalence changes done according to structure of the present invention, shape, principle, all should be covered by within protection scope of the present invention.
Claims (2)
1. a low temperature preparation method for micron order cerium oxide microballoon, is characterized in that, described preparation method comprises the steps:
(1) six water cerous nitrate and urea are accurately taken, add a small amount of deionized water respectively, make the cerous nitrate aqueous solution and aqueous solution of urea, the ratio of the amount of substance of six water cerous nitrates and urea is 1:4, mix above-mentioned two kinds of aqueous solution, then add betaine wherein, then add a part of deionized water, stir and make it dissolve completely, form mixed solution, the concentration controlling cerium ion in mixed solution is 4.35g/L, and the concentration of urea is 2.4g/L, and beet paper mill wastewater is 1 ~ 1.2g/L;
(2) move in closed reaction vessel by mixed solution, be warmed up to 90 DEG C, stir, reaction 8 ~ 12h, produces white precipitate;
(3) centrifugation goes out white precipitate, with absolute ethanol washing 4 times, and dry 12h at 80 DEG C;
(4) heat-treated by the product that described step (3) obtains, obtain the micron order cerium oxide microballoon of good dispersion, uniform particle sizes, the diameter of microballoon is 0.5 ~ 1 μm.
2. the low temperature preparation method of a kind of micron order cerium oxide microballoon according to claim 1, it is characterized in that, the heat treatment of described step (4) comprises the steps: first to be warmed up to 220 DEG C with the programming rate of 20 DEG C/min, constant temperature 5min, and then be warmed up to 550 DEG C with the programming rate of 20 DEG C/min, calcining at constant temperature 2h, is finally cooled to room temperature, completes heat treatment process.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108083316A (en) * | 2016-11-22 | 2018-05-29 | 厦门稀土材料研究所 | A kind of preparation method of nano rareearth oxidate powder body |
| WO2020221052A1 (en) * | 2019-04-28 | 2020-11-05 | 中国科学院上海药物研究所 | Alpha-tocopherol microsphere and preparation method therefor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699282A (en) * | 2005-06-09 | 2005-11-23 | 江苏工业学院 | Preparation of monodisperse spherical cerium oxide and its application in high precision polishing |
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2015
- 2015-11-19 CN CN201510800886.2A patent/CN105251421A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699282A (en) * | 2005-06-09 | 2005-11-23 | 江苏工业学院 | Preparation of monodisperse spherical cerium oxide and its application in high precision polishing |
Non-Patent Citations (1)
| Title |
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| 董赛男 等: "表面活性剂对超细钛酸钡粉体制备的影响", 《世界科技研究与发展》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108083316A (en) * | 2016-11-22 | 2018-05-29 | 厦门稀土材料研究所 | A kind of preparation method of nano rareearth oxidate powder body |
| CN108083316B (en) * | 2016-11-22 | 2020-08-21 | 厦门稀土材料研究所 | Preparation method of nano rare earth oxide powder |
| WO2020221052A1 (en) * | 2019-04-28 | 2020-11-05 | 中国科学院上海药物研究所 | Alpha-tocopherol microsphere and preparation method therefor |
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Application publication date: 20160120 |