CN103539194B - A kind of preparation method of flake cerium carbonate - Google Patents
A kind of preparation method of flake cerium carbonate Download PDFInfo
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- CN103539194B CN103539194B CN201310440636.3A CN201310440636A CN103539194B CN 103539194 B CN103539194 B CN 103539194B CN 201310440636 A CN201310440636 A CN 201310440636A CN 103539194 B CN103539194 B CN 103539194B
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Abstract
The invention discloses a kind of preparation method of flake cerium carbonate, concentration is equipped with first for the trivalent cerium ion solution A and concentration of 0.58mol/L ~ 0.87mol/L are the ammonium bicarbonate soln B of 1.27mol/L ~ 1.9mol/L so that the mol ratio of trivalent cerium ion and ammonium hydrogen carbonate in solution is 2:7, the ammonium bicarbonate soln B of 1% volume is first added in reaction vessel, trivalent cerium ion solution A and ammonium bicarbonate soln B are added in reaction vessel simultaneously with slow speed respectively afterwards, the precipitation for generating is washed with deionized water C, dried after finally washing suitable cerous carbonate precipitation suction filtration.Energy consumption is small, supplies consumption is relatively low, has the advantages that the requirement of material impurity level is relatively low, later stage treatment is simple, application value is high.
Description
Technical field
The present invention relates to a kind of preparation method of cerous carbonate, a kind of preparation method of flake cerium carbonate is related specifically to.
Background technology
Cerous carbonate is mainly used in the aspects such as advanced liquid crystal polishing powder, purification of air, vehicle exhaust absorption.Cerous carbonate is general
It is added directly into the chloride of cerium, nitrate or sulfate liquor using ammonium hydrogen carbonate, the carbonate of cerium is generated, due to receiving
To the limitation of condition, the amorphous precipitated or crystal of cerium is often can only obtain；The preparation of cerous carbonate it is general low concentration or compared with
Carried out under high-temperature.What the former had just initially formed is amorphous precipitated, it is necessary to digestion time more long is only possible to form crystalline form and sinks
Form sediment, yield is extremely low and production stability is poor, while producing substantial amounts of low concentration ammonium salt waste water to be difficult to process；And the latter can be formed
Crystalline precipitate, but supplies consumption is larger, high energy consumption, and cerous carbonate is easily oxidized at high temperature.
Cerous carbonate easily forms amorphous precipitated or colloid during precipitation, and the precipitation of generation is due to no fixed knot
Structure, surface texture is complicated, is difficult to be separated from water after precipitation, not uncomplicated laundering, and easily absorption, occlusion or parcel impurity, are present miscellaneous
Matter is high, and later stage intractability is big to wait difficult, unfavorable to realize industrialized production.Cerous carbonate can generate a kind of crystal formation and sink at high temperature
Form sediment, but there is high energy consumption, loss of material is serious, and product impurity is high, and there is the phenomenon of high-temperature oxydation, product colour jaundice.
The content of the invention
The present invention is according to above-mentioned technical problem, there is provided a kind of preparation method of flake cerium carbonate, in order to solve mesh
It is preceding exist in terms of cerous carbonate preparation yield poorly, high energy consumption, the cerous carbonate complex structure that obtains it is not single and because structure is drawn
The problems such as impurity for rising is high.The method prepares a kind of pure white crystalline form flake cerium carbonate under compared with low temperature, to raw material and auxiliary material
It is required that level is relatively low, product purity is high, it is easy to industrialized production.
The technical solution adopted by the present invention is：A kind of preparation method of flake cerium carbonate, the wherein reaction principle of cerous carbonate
For：
A kind of preparation method of flake cerium carbonate that the present invention is provided, it is comprised the following steps that：
The first step, is equipped with concentration for the trivalent cerium ion solution A and concentration of 0.58mol/L ~ 0.87mol/L are 1.27mol/
The ammonium bicarbonate soln B of L ~ 1.9mol/L；
Second step, is equipped with the trivalent cerium ion solution A and ammonium bicarbonate soln B of proper volume, and changing in matching makes bicarbonate
Ammonium excessive 10% ~ 16% so that the mol ratio of trivalent cerium ion and ammonium hydrogen carbonate in solution is 2:7；
3rd step, first adds the ammonium bicarbonate soln B of 1% volume in reaction vessel, after respectively with slow speed by three
Valency cerium ion solution A is added in reaction vessel simultaneously with ammonium bicarbonate soln B, after reaction about 5min, trivalent cerium ion is molten
The flow of liquid A and ammonium bicarbonate soln B is opened greatly by its volume ratio, it is ensured that trivalent cerium ion solution A is with ammonium bicarbonate soln B simultaneously
Flow；
4th step, the precipitation for generating is washed with deionized water C, is to stop less than 10 μ s/cm when electrical conductivity in wash water is surveyed
Washing；
5th step, dries 3 hours after washing suitable cerous carbonate precipitation suction filtration, ceria content is more than 50%.
The trivalent cerium ion solution A is 55 DEG C with the reaction temperature of ammonium bicarbonate soln B.
The temperature for being used to wash the deionized water C for precipitating in the step 4 is 35 DEG C ~ 45 DEG C.
Drying temperature after being washed in the step 5 is 55 DEG C ~ 65 DEG C.
The trivalent cerium ion solution A uses solution of cerium chloride by oxidation or cerous nitrate solution.
The trivalent cerium ion solution A can also use CeO2, and its concentration is 100g/L ~ 150g/L, corresponding bicarbonate
Ammonium B concentration is 100g/L ~ 150g/L.
Beneficial effects of the present invention are：Energy consumption is small, supplies consumption is relatively low；Simultaneously in the absence of Ce3+ by high-temperature oxydation can
Energy；Separated out because the invention is precipitated as moment, it is not necessary to be aged, it is with short production cycle；With material impurity level requirement it is relatively low, after
The advantages of phase treatment is simple, application value is high.
Brief description of the drawings
Fig. 1 is reaction principle figure of the invention；
Wherein A is trivalent cerium solution, and B is ammonium bicarbonate soln, and C is deionized water.
Fig. 2 is the electron microscope of embodiment 1；
Fig. 3 is the electron microscope of embodiment 2；
Fig. 4 is the electron microscope of embodiment 3.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
A kind of preparation method of flake cerium carbonate, the flake cerium carbonate reaction principle is as follows：
As shown in figure 1, trivalent cerium solution A is concentration 0.58mol/L ~ 0.87mol/L（I.e. folding CeO2 is 100g/L ~ 150g/
L）Ce3+ solution, regulation solution acidity is to 0.1 ± 0.01mol/L, 55 ± 5 DEG C of temperature；B be concentration 1.27mol/L ~
1.9mol/L（100g/L~150g/L）Ammonium bicarbonate soln, 55 ± 5 DEG C of temperature；C is deionized water, 55 ± 5 DEG C of temperature；
When reaction starts, stirring is opened, in first adding a small amount of ammonium bicarbonate soln B to deionized water C, after a while by trivalent
Cerium solution A is also added in deionized water C, and trivalent cerium solution A is with ammonium bicarbonate soln B while complete in being added to deionized water C
Into reaction.
The flake cerium carbonate prepare specific implementation step be：
The first step, it is the trivalent cerium ion solution A of 0.58mol/L ~ 0.87mol/L to be equipped with concentration；Being equipped with concentration is
The ammonium bicarbonate soln B of 1.27mol/L ~ 1.9mol/L；
Second step, the amount of product is prepared according to plan, and the trivalent cerium ion solution A for being equipped with proper volume is molten with ammonium hydrogen carbonate
B, it is ensured that trivalent cerium ion solution A is 2 with the mol ratio of trivalent cerium ion and ammonium hydrogen carbonate in ammonium bicarbonate soln B:7 (carbonic acid
Hydrogen ammonium excessive 10% ~ 16% is advisable)；
3rd step, in first adding the ammonium bicarbonate soln B to deionized water C of 1% volume, after respectively will with slow speed
Trivalent cerium ion solution A is added in deionized water C simultaneously with ammonium bicarbonate soln B, after reaction about 5min, by trivalent cerium ion
Solution A is opened greatly with the flow of ammonium bicarbonate soln B by its volume ratio, it is ensured that trivalent cerium ion solution A is same with ammonium bicarbonate soln B
When flowed.
4th step, the precipitation for generating is washed with 40 DEG C or so deionized water C, and 10 μ s/ are less than when electrical conductivity in wash water is surveyed
Cm is to stop washing；
5th step, dries 3 hours after washing suitable cerous carbonate precipitation suction filtration at 60 DEG C, it is ensured that its folding ceria contains
Amount is advisable more than 50%, and drying temperature is unsuitable too high, and the time is unsuitable oversize, can otherwise cause the oxidative phenomena of cerous carbonate, and influence is produced
Product quality.
Specific embodiment of the invention is as follows：
Example one：
1. it is 0.58mol/L solution of cerium chloride by oxidation 1L to be equipped with concentration, is equipped with the ammonium hydrogen carbonate 1.6L of 1.27mol/L, controls him
Temperature at 55 DEG C or so；
2. 0.5L deionized waters C is added into 3L beakers, and is put into water-bath and is incubated to 55 DEG C；
3. open stirring, rotating speed 250r/min, in first matching somebody with somebody the ammonium hydrogen carbonate got ready plus 16ml to deionized water C, after will
Ammonium hydrogen carbonate and solution of cerium chloride by oxidation are slowly added dropwise into beaker simultaneously, and ammonium hydrogen carbonate and cerium chloride flow are about 16ml/min, instead
Ammonium hydrogen carbonate flow should be opened big to 50ml/min after about 5min, cerium chloride flow opens big to 33ml/min, untill having flowed.
4. precipitated with 40 DEG C of deionized water C repeated washings cerous carbonates, its wash water electrical conductivity is less than 10 μ s/cm；
5. will wash completely after cerous carbonate in baking oven 60 DEG C drying 3h both finished product pure white flake cerium carbonate.
Electron microscope is as shown in Figure 2.
Example two
Cerium chloride in example one is changed to cerous nitrate, the experimental procedure of example one is repeated and is similarly obtained pure white sheet carbonic acid
Cerium.
Electron microscope is as shown in Figure 3.
Example three
1. it is the solution of cerium chloride by oxidation 100L of 0.87mol/l to be equipped with concentration, is equipped with concentration for the ammonium hydrogen carbonate of 1.9mol/L is molten
Liquid 160L；
2. about 50L deionized water C are first added in 500L weighing apparatus tepidarium reaction vessels, is incubated 55 DEG C；
3. open stirring, first add ammonium hydrogen carbonate cumulative volume 1% to deionization C in, after ammonium hydrogen carbonate and cerium chloride is molten
Liquid is slowly added dropwise in deionized water C simultaneously, after crystalline precipitate to be formed, ammonium hydrogen carbonate flow is opened into 5L/min, by chlorine
Change cerium solution concentration and be opened into 3L/min, the reaction time is controlled in 30min or so.
4. precipitated with 40 DEG C of deionized water C repeated washings cerous carbonates, its wash water electrical conductivity is less than 10 μ s/cm；
5. will wash completely after cerous carbonate in baking oven 60 DEG C drying 3h both finished product pure white flake cerium carbonate.
Electron microscope is as shown in Figure 4.
Claims (4)
1. a kind of preparation method of flake cerium carbonate, it is characterised in that the preparation method of the flake cerium carbonate is comprised the following steps that：
The first step, be equipped with concentration for 0.58mol/L~0.87mol/L trivalent cerium ion solution A and concentration be 1.27mol/L~
The ammonium bicarbonate soln B of 1.9mol/L；The trivalent cerium ion solution A is 55 DEG C with the reaction temperature of ammonium bicarbonate soln B；
Second step, is equipped with the trivalent cerium ion solution A and ammonium bicarbonate soln B of proper volume, and ammonium hydrogen carbonate mistake is made in the proportioning
Amount 10%~16% so that the mol ratio of trivalent cerium ion and ammonium hydrogen carbonate in solution is 2:7；
3rd step, first adds the ammonium bicarbonate soln B of 1% volume in reaction vessel, after respectively with slow speed by trivalent
Cerium ion solution A is added in reaction vessel simultaneously with ammonium bicarbonate soln B, after reaction about 5min, by trivalent cerium ion solution A
Flow with ammonium bicarbonate soln B is opened greatly by its volume ratio, it is ensured that trivalent cerium ion solution A flows simultaneously with ammonium bicarbonate soln B
It is complete；
4th step, the precipitation for generating is washed with deionized water C, is to stop washing less than 10 μ s/cm when electrical conductivity in wash water is surveyed；
5th step, will dry 3 hours after washing suitable cerous carbonate precipitation suction filtration, make the content of ceria sign cerous carbonate big
In 50%.
2. the preparation method of a kind of flake cerium carbonate according to claim 1, it is characterised in that：It is described to be precipitated for washing
Deionized water C temperature be 35 DEG C~45 DEG C.
3. the preparation method of a kind of flake cerium carbonate according to claim 1, it is characterised in that：Drying after the washing
Temperature is 55 DEG C~65 DEG C.
4. the preparation method of a kind of flake cerium carbonate according to claim 1, it is characterised in that：The trivalent cerium ion is molten
Liquid A uses cerium chloride or cerous nitrate solution.
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| CN104310456B (en) * | 2014-10-14 | 2017-03-01 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | A kind of production method of the low chlorine root carbonated rare earth of fine granularity |
| CN112126977B (en) * | 2020-08-11 | 2021-11-19 | 南昌大学 | Method for preparing high-purity flaky single crystal and flaky crystal dense aggregated cerium carbonate |
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| JP4917098B2 (en) * | 2005-09-20 | 2012-04-18 | エルジー・ケム・リミテッド | Cerium carbonate powder and production method, cerium oxide powder produced therefrom and production method, and CMP slurry containing the same |
| CN101372353A (en) * | 2008-06-12 | 2009-02-25 | 江苏工业学院 | Method for preparing nano CeO2 power by ultrasonic atomization process |
| CN101633517A (en) * | 2008-07-23 | 2010-01-27 | 甘肃稀土新材料股份有限公司 | Production process of oil-free cerium carbonate |
| CN101481131A (en) * | 2009-02-20 | 2009-07-15 | 包头市金蒙稀土有限责任公司 | Preparation of high purity cerous carbonate with high total amount of rare earth |
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| CN102060319B (en) * | 2011-01-27 | 2013-03-13 | 南昌大学 | Preparation method of cerous carbonate midbody |
| 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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