CN108862362A - A kind of preparation method of micron order cerium oxide powder - Google Patents
A kind of preparation method of micron order cerium oxide powder Download PDFInfo
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- CN108862362A CN108862362A CN201811084598.1A CN201811084598A CN108862362A CN 108862362 A CN108862362 A CN 108862362A CN 201811084598 A CN201811084598 A CN 201811084598A CN 108862362 A CN108862362 A CN 108862362A
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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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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a kind of preparation methods of micron order cerium oxide powder, include the following steps：Cerium-containing compound is added in acid solution and prepares cerium solution；Cerium solution is added in the mixed solution of ethylene glycol and water, surfactant is added after being sufficiently stirred, adjusts pH to 8-10 with ammonium hydroxide after being uniformly mixed；Above-mentioned solution is added in water heating kettle and carries out hydro-thermal reaction 6-10h, filtering, dry, roasting obtain product after generation sediment.The present invention has developed a kind of simple, inexpensive polyxol method for preparing cerium oxide powder using the mixed liquor of ethylene glycol and water as solvent；The present invention prevents the reunion between particle, and carry out the control of modification with pattern by the way that surfactant (CTAB/CTAC) is added；Cerium oxide powder even particle distribution prepared by the present invention, size are controllable, and size can control in 0.1-25 μ m, be appropriate for large-scale production.
Description
Technical field
The present invention relates to the preparation fields of rare earth oxide, more particularly to a kind of preparation side of micron order cerium oxide powder
Method.
Background technique
Cerium oxide is light rare earth oxide a kind of cheap, that purposes is extremely wide, have been used for catalyst, chemically mechanical polishing,
The fields such as electrochemistry, steel and iron industry.As catalyst, cerium oxide is widely used in cleaning catalyst for tail gases of automobiles；With oxidation
Cerium is widely used in various precision glass polishings, polished semiconductor substrate, monocrystalline silicon piece polishing as the polishing fluid of polishing particles
It is polished with integrated circuit middle dielectric layer；In electrochemistry, make electrolyte using cerium oxide base composite oxides, just in medium temperature
There can be sufficiently high cation electrodeposition current density；In steel and iron industry, cerium oxide can be used as trace mineral supplement for steel, cast iron, admire,
In the materials such as aluminium, nickel, tungsten, key, so as to improve the thermal stability of alloy and corrosion resistance etc..
The physicochemical properties of the performance of cerium oxide not only with itself are related, also with their average grain diameter, dispersion feelings
Condition and granular size etc. have close relationship.Therefore, suitable method is selected to prepare controllable with certain pattern, size
Cerium oxide be necessary.Patent of invention CN1699282 proposes the preparation method of monodisperse spherical cerium oxide, gained oxygen
Change cerium partial size is more single (300nm or so), and preparation process is more complicated；Chinese patent CN101898787A discloses a kind of use
Cerium chloride liquid is the method for Material synthesis sub-micron cerium oxide, and for this method using cerium chloride liquid as cerium source, ammonium hydrogen carbonate is precipitating reagent,
A small amount of surfactant is added and does dispersing agent, sub-micron of the D50 between 0.1-0.2 μm has been synthesized using liquid-phase precipitation method and has been aoxidized
The cerium oxide size of cerium, preparation is relatively simple, can not carry out the regulation of size as needed.
Summary of the invention
For above-mentioned problems of the prior art, that the object of the present invention is to provide a kind of sizes is controllable, particle is uniform
Cerium oxide powder preparation method.
To achieve the above object, the present invention is achieved through the following technical solutions：
A kind of preparation method of micron order cerium oxide powder, includes the following steps：
(1) cerium-containing compound is added in acid solution and prepares cerium solution；
(2) cerium solution is added in the mixed solution of ethylene glycol and water, surfactant is added after being sufficiently stirred, stirs
It mixes uniformly mixed；
(3) solution of step (2) ammonium hydroxide is adjusted into pH to 8-10；
(4) solution of step (3) is added in water heating kettle and carries out hydro-thermal reaction 6-10h, generate sediment；
(5) it filters, is dry, roasting obtains product；
Wherein, cerium-containing compound described in step (1) is at least one of cerium oxide, cerous carbonate；
The volume mixture ratio of ethylene glycol described in step (2) and water is 10:(1-3)；
Surfactant described in step (2) is cetyl trimethylammonium bromide (CTAB), cetyl trimethyl chlorine
Change one of ammonium (CTAC).
Further, acid solution described in step (1) is one of hydrochloric acid, nitric acid, sulfuric acid, concentration 0.6-
2.0mol/L。
Further, the concentration of cerium solution described in step (1) is 0.5-1.5mol/L.
Further, the ultimate density of each ingredient is in step (2) system：Surfactant：0.05-0.2mol/L, cerium
Salt：0.1-0.5mol/L.
Further, the mass concentration containing ammonia of ammonium hydroxide described in step (3) is 20-28%.
Further, the temperature of hydro-thermal reaction described in step (4) is 100-140 DEG C.
Further, temperature dry described in step (5) is 120-160 DEG C, and the time of the drying is 4-8h, described
The temperature of roasting is 320-450 DEG C, and the time of the roasting is 4-8h.
Further, a kind of preparation method of micron order cerium oxide powder, includes the following steps：
Cerium oxide is added to the chlorination cerium solution for preparing that concentration is 0.5mol/L in the hydrochloric acid of 0.6mol/L；By cerium salt
Solution be added in the mixed solution of ethylene glycol and water (volumetric mixture ratio of ethylene glycol and water be 10:1) it is added after, being sufficiently stirred
Surfactant (CTAB), is uniformly mixed, and the concentration of surfactant is 0.05mol/L, cerium salt concentration in final system
For 0.1mol/L；It is the pH to 9 that 28% ammonium hydroxide adjusts solution with mass concentration；Above-mentioned solution is added in water heating kettle, at 120 DEG C
Hydro-thermal reaction 8h generates sediment in system, then filters, dry 8h at 140 DEG C；4h is finally roasted at 450 DEG C obtains oxygen
Change cerium powder.
Due to using the technology described above, beneficial effects of the present invention include：
The present invention has developed a kind of simple, low cost and has prepared cerium oxide powder using the mixed liquor of ethylene glycol and water as solvent
Polyxol method；The surfactant (CTAB/CTAC) that the present invention uses, can be used as stabilizer first, makes reaction system
It is uniformly dispersed, prevents the reunion between particle, on the other hand the crystal face of cerium oxide can be modified and carry out appearance and size
Control, different concentration can control the speed of growth of different crystal faces, therefore can be fine by the amount of surfactant
Ground controls the size of cerium oxide powder, and size can control in 0.1-25 μ m；Cerium oxide powder prepared by the present invention
Even particle distribution, size are controllable, are appropriate for large-scale production.
Specific embodiment
It is described further below with reference to embodiment, but the present invention is not limited to these embodiments.
Embodiment 1
Cerium oxide is added to the solution of cerium chloride by oxidation for preparing that concentration is 0.5mol/L in the hydrochloric acid of 0.6mol/L；By cerium chloride
Solution be added in the mixed solution of ethylene glycol and water (volumetric mixture ratio of ethylene glycol and water be 10:1) it is added after, being sufficiently stirred
Surfactant CTAB is uniformly mixed, and the concentration of surfactant is 0.05mol/L, chlorination cerium concentration in final system
For 0.1mol/L；It is the pH to 9 that 28% ammonium hydroxide adjusts solution with mass concentration；Above-mentioned solution is added in water heating kettle, at 120 DEG C
Hydro-thermal reaction 8h generates sediment in system, then filters, dry 8h at 140 DEG C；4h is finally roasted at 450 DEG C obtains oxygen
Change cerium powder.
Embodiment 2
Cerium oxide is added to the cerous nitrate solution for preparing that concentration is 0.8mol/L in the nitric acid solution of 1.0mol/L；By nitre
Sour cerium solution be added in the mixed solution of ethylene glycol and water (volumetric mixture ratio of ethylene glycol and water be 10:2) after, being sufficiently stirred
Surfactant CTAC is added, is uniformly mixed, the concentration of surfactant is 0.1mol/L in final system, and cerous nitrate is dense
Degree is 0.5mol/L；It is the pH to 8 that 20% ammonium hydroxide adjusts solution with mass concentration；Above-mentioned solution is added in water heating kettle, 100 DEG C
Lower hydro-thermal reaction 6h generates sediment in system, then filters, dry 6h at 160 DEG C；Finally 6h is roasted at 400 DEG C to obtain
Ceria oxide powder.
Embodiment 3
Cerous carbonate is added to the cerous sulfate solution for preparing that concentration is 1.0mol/L in the sulfuric acid solution of 1.5mol/L；By sulphur
Sour cerium solution be added in the mixed solution of ethylene glycol and water (volumetric mixture ratio of ethylene glycol and water be 10:3) after, being sufficiently stirred
Surfactant CTAB is added, is uniformly mixed, the concentration of surfactant is 0.15mol/L, cerous sulfate in final system
Concentration is 0.25mol/L；It is the pH to 10 that 25% ammonium hydroxide adjusts solution with mass concentration；Above-mentioned solution is added in water heating kettle,
Hydro-thermal reaction 10h at 140 DEG C generates sediment in system, then filters, dry 4h at 130 DEG C；Finally roasted at 350 DEG C
8h obtains ceria oxide powder.
Embodiment 4
Cerous carbonate is added to the cerous nitrate solution for preparing that concentration is 1.5mol/L in the nitric acid solution of 2.0mol/L；By nitre
Sour cerium solution be added in the mixed solution of ethylene glycol and water (volumetric mixture ratio of ethylene glycol and water be 10:2) after, being sufficiently stirred
Surfactant CTAC is added, is uniformly mixed, the concentration of surfactant is 0.2mol/L in final system, and cerous nitrate is dense
Degree is 0.4mol/L；It is the pH to 9 that 26% ammonium hydroxide adjusts solution with mass concentration；Above-mentioned solution is added in water heating kettle, 110 DEG C
Lower hydro-thermal reaction 8h generates sediment in system, then filters, dry 7h at 150 DEG C；Finally 7h is roasted at 320 DEG C to obtain
Ceria oxide powder.
Embodiment 5
The preparation method of cerium oxide is same as Example 1, the difference is that system after Surfactant CTAB is added
The concentration of middle surfactant is 0.1mol/L.
Embodiment 6
The preparation method of cerium oxide is same as Example 1, the difference is that system after Surfactant CTAB is added
The concentration of middle surfactant is 0.15mol/L.
Embodiment 7
The preparation method of cerium oxide is same as Example 1, the difference is that system after Surfactant CTAB is added
The concentration of middle surfactant is 0.2mol/L.
Comparative example 1
The preparation method of cerium oxide is same as Example 1, the difference is that surfactant is not added in preparation process.
Comparative example 2
The preparation method of cerium oxide is same as Example 1, the difference is that cerium solution is added to two solution of second
In.
Following table (table 1) is the granularity data table of the cerium oxide powder of the method preparation of above-described embodiment and comparative example.
The granularity data table of the cerium oxide powder of the method for 1 embodiment of table and comparative example preparation
| Experimental program | D10/μm | D50/μm | D90/μm |
| Embodiment 1 | 23.01 | 24.08 | 25.47 |
| Embodiment 2 | 16.37 | 17.64 | 18.85 |
| Embodiment 3 | 11.09 | 12.49 | 13.73 |
| Embodiment 4 | 3.77 | 4.50 | 5.67 |
| Embodiment 5 | 11.18 | 11.99 | 12.86 |
| Embodiment 6 | 1.01 | 1.27 | 1.49 |
| Embodiment 7 | 0.09 | 0.10 | 0.12 |
| Comparative example 1 | 50.93 | 86.32 | 98.40 |
| Comparative example 2 | 0.03 | 0.05 | 0.06 |
The above is merely a preferred embodiment of the present invention, and is not intended to limit the present invention；But for the common of this field
Technical staff without departing from the scope of the present invention, made using disclosed above technology contents it is a little more
Dynamic, modification and the equivalent variations developed, are equivalent embodiment of the invention；Meanwhile all substantial technologicals pair according to the present invention
The variation, modification and evolution etc. of any equivalent variations made by above embodiments, still fall within the guarantor of technical solution of the present invention
Within the scope of shield.
Claims (8)
1. a kind of preparation method of micron order cerium oxide powder, which is characterized in that include the following steps：
(1) cerium-containing compound is added in acid solution and prepares cerium solution；
(2) cerium solution is added in the mixed solution of ethylene glycol and water, surfactant is added after being sufficiently stirred, stirring is mixed
It closes uniform；
(3) solution of step (2) ammonium hydroxide is adjusted into pH to 8-10；
(4) solution of step (3) is added in water heating kettle and carries out hydro-thermal reaction 6-10h, generate sediment；
(5) it filters, is dry, roasting obtains product；
Wherein, cerium-containing compound described in step (1) is at least one of cerium oxide, cerous carbonate；
The volumetric mixture ratio of ethylene glycol described in step (2) and water is 10:(1-3)；
Surfactant described in step (2) is cetyl trimethylammonium bromide (CTAB), hexadecyltrimethylammonium chloride
One of (CTAC).
2. the preparation method of micron order cerium oxide powder according to claim 1, which is characterized in that described in step (1)
Acid solution is one of hydrochloric acid, nitric acid, sulfuric acid, concentration 0.6-2.0mol/L.
3. the preparation method of micron order cerium oxide powder according to claim 1, which is characterized in that described in step (1)
The concentration of cerium solution is 0.5-1.5mol/L.
4. the preparation method of micron order cerium oxide powder according to claim 1, which is characterized in that in step (2) system
The ultimate density of each ingredient is：Surfactant：0.05-0.2mol/L, cerium salt：0.1-0.5mol/L.
5. the preparation method of micron order cerium oxide powder according to claim 1, which is characterized in that described in step (3)
The mass concentration containing ammonia of ammonium hydroxide is 20-28%.
6. the preparation method of micron order cerium oxide powder according to claim 1, which is characterized in that described in step (4)
The temperature of hydro-thermal reaction is 100-140 DEG C.
7. the preparation method of micron order cerium oxide powder according to claim 1, which is characterized in that described in step (5)
Dry temperature is 120-160 DEG C, and the time of the drying is 4-8h, and the temperature of the roasting is 320-450 DEG C, the roasting
Time be 4-8h.
8. the preparation method of micron order cerium oxide powder according to claim 1, which is characterized in that include the following steps：
Cerium oxide is added to the chlorination cerium solution for preparing that concentration is 0.5mol/L in the hydrochloric acid of 0.6mol/L；Cerium solution is added
To in the mixed solution of ethylene glycol and water, (volumetric mixture ratio of ethylene glycol and water is 10:1) surface-active is added after, being sufficiently stirred
Agent CTAB, is uniformly mixed, and the concentration of surfactant is 0.05mol/L in final system, and cerium salt concentration is 0.1mol/L；
It is the pH to 9 that 28% ammonium hydroxide adjusts solution with mass concentration；Above-mentioned solution is added in water heating kettle, hydro-thermal reaction 8h at 120 DEG C,
Sediment is generated in system, is then filtered, dry 8h at 140 DEG C；4h is finally roasted at 450 DEG C obtains ceria oxide powder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665554A (en) * | 2019-01-16 | 2019-04-23 | 南昌大学 | A method of it adjusting solvent burden ratio and obtains the micro-nano ceria of morphology controllable |
| CN109772290A (en) * | 2019-02-28 | 2019-05-21 | 江苏国盛新材料有限公司 | A kind of preparation method of cerium zirconium sosoloid |
| CN113226989A (en) * | 2018-12-28 | 2021-08-06 | 罗地亚经营管理公司 | Cerium oxide particles and process for producing the same |
| CN113830809A (en) * | 2021-10-27 | 2021-12-24 | 中国科学院青海盐湖研究所 | Preparation method of superfine alumina powder and product thereof |
| CN114604888A (en) * | 2020-12-09 | 2022-06-10 | 中国科学院大连化学物理研究所 | Method for preparing rod-shaped, cubic and polyhedral cerium oxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107597092A (en) * | 2017-07-21 | 2018-01-19 | 上海纳米技术及应用国家工程研究中心有限公司 | 3D patterns CeO2/TiO2Preparation method of catalyst |
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2018
- 2018-09-17 CN CN201811084598.1A patent/CN108862362B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107597092A (en) * | 2017-07-21 | 2018-01-19 | 上海纳米技术及应用国家工程研究中心有限公司 | 3D patterns CeO2/TiO2Preparation method of catalyst |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113226989A (en) * | 2018-12-28 | 2021-08-06 | 罗地亚经营管理公司 | Cerium oxide particles and process for producing the same |
| CN109665554A (en) * | 2019-01-16 | 2019-04-23 | 南昌大学 | A method of it adjusting solvent burden ratio and obtains the micro-nano ceria of morphology controllable |
| CN109772290A (en) * | 2019-02-28 | 2019-05-21 | 江苏国盛新材料有限公司 | A kind of preparation method of cerium zirconium sosoloid |
| CN114604888A (en) * | 2020-12-09 | 2022-06-10 | 中国科学院大连化学物理研究所 | Method for preparing rod-shaped, cubic and polyhedral cerium oxide |
| CN113830809A (en) * | 2021-10-27 | 2021-12-24 | 中国科学院青海盐湖研究所 | Preparation method of superfine alumina powder and product thereof |
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Effective date of registration: 20211102 Address after: 225400 group Zhouchen 90, Guangling Town, Taixing City, Taizhou City, Jiangsu Province Patentee after: JIANGSU CHINALCO NEW MATERIAL Co.,Ltd. Patentee after: GRIREM ADVANCED MATERIALS Co.,Ltd. Address before: 225400 Zhouchen group 90, Guangling Town, Taixing City, Taizhou City, Jiangsu Province (Jiangsu Guosheng New Material Co., Ltd.) Patentee before: JIANGSU CHINALCO NEW MATERIAL Co.,Ltd. |