CN105174298B - Preparation method of ultrafine cerium oxide powder by adding Ce4+ solution into CeCl3 solution - Google Patents
Preparation method of ultrafine cerium oxide powder by adding Ce4+ solution into CeCl3 solution Download PDFInfo
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- CN105174298B CN105174298B CN201510518753.6A CN201510518753A CN105174298B CN 105174298 B CN105174298 B CN 105174298B CN 201510518753 A CN201510518753 A CN 201510518753A CN 105174298 B CN105174298 B CN 105174298B
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Abstract
The invention relates to a preparation method of ultrafine cerium oxide powder by adding a Ce4+ solution into a CeCl3 solution, and belongs to the field of rare earth material preparation. The method comprises the following steps: adding a CeCl3 solution into a reactor, heating to a temperature of 80 DEG C, then adding PEG 10000 and glacial acetic acid into the CeCl3 solution, after PEG 10000 is dissolved, adding Ce4+ into the CeCl3 solution, then adding an ammonium bicarbonate solution into the CeCl3 solution until the pH value reaches 7 to obtain semi-transparent brown precipitate that is easy to filter, washing the precipitate, filtering, drying, and finally burning the precipitate at a temperature of 900 DEG C so as to obtain ultrafine cerium powder, which is well dispersed and has a median particle size (D50) of 100 to 300 nm.
Description
Technical field
The present invention relates to a kind of CeCl3Add Ce in feed liquid4+The method that solution prepares fine cerium oxide powder body, belongs to rare earth
Field of material preparation.
Background technology
The physical property of rare earth material is applied to have a major impact, and the granularity of wherein powder body is to determine its application
One of key factor, fine cerium oxide are being catalyzed, are polishing, are showing that coatings art tool is widely used, especially in polishing field, grain
The controllable nanometer of degree distribution and fine cerium oxide gain great popularity.The relevant report for preparing ultra-fine and nano-cerium oxide is more,
There are sol-gal process, hydrothermal synthesis method, combustion method, spray pyrolysis, microemulsion method, the sedimentation method, mechanochemical reaction, numerous super
In the thin and preparation method of nano-cerium oxide, collosol and gel, Hydrothermal Synthesiss, burning, spray pyrolysis and microemulsion method are also located at present
In the experimental study stage, as these method cost of material height, low production efficiency, required reaction time are long, it is not suitable for big rule
Mould is produced；The sedimentation method and mechanochemical reaction are produced on a large scale, but mechanochemical reaction also has the shortcomings that cycle length, high cost,
Chemical precipitation method is the optimum selection for preparing nanometer or fine cerium oxide powder body, but using carbonate, ammonia or sodium hydroxide
When carrying out precipitation to cerium chloride, cerous nitrate and preparing fine cerium oxide, as granule is tiny, it is difficult to carry out filtration washing operation,
Make troubles in production process, and the presoma of uncomplicated laundering is not all higher in calcination rear impurity content, powder dispersity is not yet
It is good, become the bottleneck that current industrialization prepares high-quality nanometer and fine cerium oxide.
The content of the invention
It is an object of the invention to provide a kind of easy filtration washing of presoma, powder dispersity is good, low cost, median
The method of controllable fine cerium oxide.
Technical solution：
(1) present invention adds the CeCl of concentration 0.35mol/L in reactor3Solution is simultaneously heated to 80 DEG C, to CeCl3It is molten
PEG10000 and glacial acetic acid, PEG10000 and glacial acetic acid addition is added to be CeCl in liquid3The 3.5% of quality and 2.1%, treat
After PEG10000 dissolvings, the Ce of concentration 2.9mol/L is added in solution4+Solution, Ce4+Solution addition is Ce4+With Ce3+Mole
Than 1: 4～8, then in reactor add concentration 1.9mol/L ammonium bicarbonate soln, when mother liquor of precipitation of ammonium pH value reaches 7, stop
Only add ammonium bicarbonate soln, ageing reaction 10min obtains easily filtering, translucent tan precipitate, by washing of precipitate,
Filter, drying, calcination temperature is 900 DEG C, obtains that particle dispersion is good, median D50For the fine cerium oxide of 100～300nm
Powder body；
(2) Ce described in the technology of the present invention solution (1)4+Solution is Ce (NO3)3、(NH4)4Ce(NO3)6、 Ce
(NO3)3(NH4)4Ce(NO3)6Mixed solution.
Invention effect
(1) Ce is added in the present invention4+Solution is to prepare fine cerium oxide powder technology key, Ce in solution4+With Ce3+Most
Good mol ratio is 1: 4～8, if Ce in solution4+With Ce3+Mol ratio is less than 1: 8, and the cerium oxide particle for obtaining is larger, and with Ce4 +The reduction of solution addition, cerium oxide particle increase；If Ce in solution4+With Ce3+Mol ratio is more than 1: 4, in the cerium oxide for obtaining
Position change of size is little, but preparation cost increases；
(2) method for preparing fine cerium oxide using the present invention, the precipitation for obtaining easily are filtered, are washed, and are easy to industrialization
Production, low production cost.
Description of the drawings
Fig. 1 is fine cerium oxide particle size distribution figure prepared by the present invention.
Specific embodiment
Embodiment 1
1000ml concentration is added in reactor for the CeCl of 0.35mol/L3Solution is simultaneously heated to 80 DEG C, to CeCl3Solution
Middle addition 3g PEG10000 and 1.8g glacial acetic acids, after PEG10000 dissolvings, add 20ml concentration 2.9mol/L in solution
Ce(NO3)4Solution, then concentration is added in reactor for the ammonium bicarbonate soln of 1.9mol/L, when mother liquor of precipitation of ammonium pH value reaches 7
When, stop adding ammonium bicarbonate soln, ageing reaction 10min to obtain easily filtration, translucent tan precipitate, will precipitation
Washing, filter, drying, calcination temperature is 900 DEG C, obtains that particle dispersion is good, median D50For the ultra-fine oxidation of 212nm
Cerium powder body.
Embodiment 2
1000ml concentration is added in reactor for the CeCl of 0.35mol/L3Solution is simultaneously heated to 80 DEG C, to CeCl3Solution
Middle addition 3g PEG10000 and 1.8g glacial acetic acids, after PEG10000 dissolvings, add 25ml concentration 2.9mol/L in solution
(NH4)4Ce(NO3)6Solution, then concentration is added in reactor for the ammonium bicarbonate soln of 1.9mol/L, when mother liquor of precipitation of ammonium pH value
When reaching 7, stop adding ammonium bicarbonate soln, ageing reaction 10min to obtain easily filtration, translucent tan precipitate, will
Washing of precipitate, filtration, drying, calcination temperature are 900 DEG C, obtain that particle dispersion is good, median D50For the ultra-fine of 165nm
Cerium oxide powder.
Embodiment 3
20L concentration is added in retort for the CeCl of 0.35mol/L3Solution is simultaneously heated to 80 DEG C, to CeCl3In solution
60g PEG10000 and 36g glacial acetic acids are added, after PEG10000 dissolvings, 200ml concentration 2.9mol/L is added in solution
(NH4)4Ce(NO3)6Ce (the NO of solution and 100ml concentration 2.9mol/L3)4Solution, then addition concentration is in reactor
The ammonium bicarbonate soln of 1.9mol/L, when mother liquor of precipitation of ammonium pH value reaches 7, stops adding ammonium bicarbonate soln, ageing reaction
10min, obtains easily filtration, translucent tan precipitate, is 900 DEG C by washing of precipitate, filtration, drying, calcination temperature, obtains
To particle dispersion is good, median D50For the fine cerium oxide powder body of 242nm.
Claims (2)
1.CeCl3Add Ce in feed liquid4+The method that solution prepares fine cerium oxide powder body, it is characterised in that add in reactor
Enter the CeCl of 0.35 mol/L of concentration3Solution is simultaneously heated to 80 DEG C, to CeCl3PEG10000 and glacial acetic acid are added in solution,
PEG10000 and glacial acetic acid addition are CeCl3The 3.5% of quality and 2.1%, after PEG10000 dissolvings, add in solution and rub
The Ce of your 2.9 mol/L of concentration4+Solution, Ce4+Solution addition and CeCl3Mol ratio is 1:4 ~ 8, Ce4+Solution is added and is finished
Afterwards, then in reactor the ammonium bicarbonate soln of 1.9 mol/L of molar concentration is added, when mother liquor of precipitation of ammonium pH value reaches 7, is stopped
Ammonium bicarbonate soln, ageing 10 min of reaction is added to obtain easily filtration, translucent tan precipitate, by washing of precipitate, mistake
Filter, drying, calcination temperature is 900 DEG C, obtains that particle dispersion is good, median D50For the fine cerium oxide powder of 100 ~ 300 nm
Body..
2. CeCl according to claim 13Add Ce in feed liquid4+The method that solution prepares fine cerium oxide powder body, which is special
Levy and be, Ce4+Solution is Ce (NO3)4、(NH4)2Ce(NO3)6Or Ce (NO3)4(NH4)2Ce(NO3)6Mixed solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510518753.6A CN105174298B (en) | 2015-08-17 | 2015-08-17 | Preparation method of ultrafine cerium oxide powder by adding Ce4+ solution into CeCl3 solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510518753.6A CN105174298B (en) | 2015-08-17 | 2015-08-17 | Preparation method of ultrafine cerium oxide powder by adding Ce4+ solution into CeCl3 solution |
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| CN105174298A CN105174298A (en) | 2015-12-23 |
| CN105174298B true CN105174298B (en) | 2017-05-03 |
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Families Citing this family (1)
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| CN111333098B (en) * | 2018-11-30 | 2022-04-19 | 中国科学院大连化学物理研究所 | Preparation method of cerium dioxide nano cube |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550318A (en) * | 2008-04-03 | 2009-10-07 | 北京有色金属研究总院 | Ce<3+>-contained rare-earth polishing powder and preparation method thereof |
| CN102502758A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Method for preparing large-particle cerium oxide |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550318A (en) * | 2008-04-03 | 2009-10-07 | 北京有色金属研究总院 | Ce<3+>-contained rare-earth polishing powder and preparation method thereof |
| CN102502758A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Method for preparing large-particle cerium oxide |
Non-Patent Citations (2)
| Title |
|---|
| 氧化铈粒度控制研究;桑晓云等;《包钢科技》;20050430;全文 * |
| 氧化铈超细粉体的制备研究;李梅等;《中国稀土学报》;20030830;全文 * |
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