CN108217712A - A kind of production method of the big grain size cerous carbonate of high-purity - Google Patents
A kind of production method of the big grain size cerous carbonate of high-purity Download PDFInfo
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- CN108217712A CN108217712A CN201810330699.6A CN201810330699A CN108217712A CN 108217712 A CN108217712 A CN 108217712A CN 201810330699 A CN201810330699 A CN 201810330699A CN 108217712 A CN108217712 A CN 108217712A
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- cerous carbonate
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- grain size
- ammonium bicarbonate
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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
- C01F17/247—Carbonates
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of production method of the big grain size cerous carbonate of high-purity, step is as follows：(1) cerous carbonate is added to the water to form mixed liquor；(2) it is limpid that concentrated nitric acid dissolving is added in into the mixed liquor that step (1) obtains, and the pH of solution is transferred to 4 4.5；(3) solution obtained in step (2) filtered successively, concentrated, spontaneous nucleation and centrifugal dehydration；(4) crystal after centrifugation in step (3) is dissolved in water, diluted and solution is heated to 50 55 DEG C, start stirring and add in ammonium bicarbonate soln, previous hour mixing speed is 28 30 revs/min, and ammonium bicarbonate soln flow velocity is 1.5 2.0L/ minutes；Mixing speed is 31 35 revs/min after one hour, and ammonium bicarbonate soln flow velocity is 2.1 2.5L/ minutes, is precipitated to solution PH 6.5 7 and stands 30 minutes；(5) precipitation in step (4) is washed, is then centrifuged for being dehydrated, pack.
Description
Technical field
The invention belongs to Rare Earth Production fields, and in particular to a kind of production method of the big grain size cerous carbonate of high-purity.
Background technology
The main application of cerous carbonate is：Produce cerium compound, it can also be used to prepare rare earth luminescent material, purifying vehicle exhaust
Catalyst, polishing material and colored engineering plastics color.Impurity content is high in existing cerous carbonate, i.e., purity is low, particularly golden
It is high to belong to impurity content so that the color of product is in faint yellow, and new impurity and shadow are introduced to when preparing other materials with cerous carbonate
Ring the performance for preparing substance；For the different purposes of cerous carbonate, during especially as preparing polishing material, to the grain of cerous carbonate
Diameter requirement is stringent, and the grain size of existing cerous carbonate is small can not be as the raw material for preparing polishing material.
Invention content
It is an object of the invention to for purity existing for above-mentioned existing cerous carbonate is low and grain size is small the problem of, the present invention
A kind of production method of the big grain size cerous carbonate of high-purity is provided, wherein：Big grain size in the application refers to grain size more than 13um's
Particle；High-purity refers to CeO2The cerous carbonate of/REO >=99.00%.
The technical solution adopted by the present invention is as follows：
A kind of production method of the big grain size cerous carbonate of high-purity, step are as follows：
(1), cerous carbonate is added to the water to form mixed liquor；
(2), it is limpid that concentrated nitric acid dissolving is added in into the mixed liquor that step (1) obtains, and with cerous carbonate tune pH value to 1-
1.5, pH to 4-4.5 is adjusted with ammonium bicarbonate soln again after heating, obtains trivalent cerium solution；
(3), the trivalent cerium solution obtained in step (2) is obtained into filtrate by three-stage filtration；
(4), the filtrate in step (3) is concentrated, striking point solution concentration is calculated as 750 g/l by cerium oxide；
(5), the concentrate obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifugal dehydration；
(6), the crystal after the centrifugation in step (5) is dissolved in water and diluted, cerium concentration is made to be calculated as 70- by oxide
80g/L；
(7), the solution obtained after step (6) processing is heated to 50-55 DEG C, starts stirring and add in the bicarbonate after refining
Ammonium salt solution, previous hour mixing speed control is at 28-30 revs/min, and ammonium bicarbonate soln flow control is at 1.5-2.0L/ points
Clock；At 31-35 revs/min, ammonium bicarbonate soln flow control sank at 2.1-2.5L/ minutes for mixing speed control after one hour
It forms sediment to solution PH 6.5-7, precipitation stands 30 minutes after the completion；
(8), the precipitation in step (7) is washed, is then centrifuged for being dehydrated, pack.
Operation principle/the effect of this programme is：When ammonium bicarbonate soln is added in step (7), previous hour stirring
Speed control is at 54 revs/min, and ammonium bicarbonate soln flow control was at 1.5L/ minutes；Mixing speed control is 64 after one hour
Rev/min, ammonium bicarbonate soln flow control was precipitated to solution PH 6.5-7,30 points is stood after the completion of precipitation at 2.5L/ minutes
Clock, the specific surface area of obtained cerous carbonate is small, so reducing the attachment of metal ion, obtains REO >=48% of cerous carbonate,
CeO2/ REO >=99.99%, metal ion ＜ 1ppm, grain size D50>25, meet purity and grain size of the different purposes to cerous carbonate
Requirement.
Preferably, in step (1), the weight ratio of cerous carbonate and water is 1 ︰ 1.5.
Preferably, in step (2), the method for heating is：It is heated to boil, be kept for 30 minutes or more.
Preferably, in step (3), the method for filtering is：First with 200 mesh filter-cloth filterings, then the micropore mistake with aperture 1-5um
Filter double-filtration.
Preferably, in step (7), ammonium hydrogen carbonate solution concentration after double-filtration is 80g/L.
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
In the present invention, when adding in ammonium bicarbonate soln, start stirring and add in the ammonium bicarbonate soln after refining, it is previous small
When mixing speed control at 28-30 revs/min, ammonium bicarbonate soln flow control was at 1.5-2.0L/ minutes；It is stirred after one hour
For speed control at 31-35 revs/min, ammonium bicarbonate soln flow control was precipitated to 3 solution PH 6.5- at 2.1-2.5L/ minutes
7, precipitation stands 30 minutes after the completion, obtains REO >=48% of cerous carbonate, CeO2/ REO >=99.99%, metal ion ＜
1ppm, grain size D50>25, meet different purposes to the purity of cerous carbonate and the requirement of grain size.
Specific embodiment
All features or disclosed all methods disclosed in this specification or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Embodiment one
A kind of production method of the big grain size cerous carbonate of high-purity, step are as follows：
(1), 1 part of cerous carbonate is added in 1.2 parts of deionized water and stirred and form mixed liquor；
(2), add in concentrated nitric acid into the mixed liquor that step (1) obtains, stir while adding until mixed liquor it is limpid, be used in combination
Cerous carbonate tune pH value is heated to boiling, then adjust pH to 4 with ammonium bicarbonate soln, boiling is kept for 30 minutes or more, obtained to 1
Trivalent cerium solution；
(3), by the trivalent cerium solution obtained in step (2) first with 200 mesh filter-cloth filterings, then the micropore mistake with aperture 1um
Filter double-filtration obtains filtrate；
(4), the filtrate in step (3) is concentrated, striking point solution concentration is calculated as 750 g/l by cerium oxide；
(5), the concentrate obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifugal dehydration；
(6), the crystal after the centrifugation in step (5) is dissolved in water and diluted, cerium concentration is made to be calculated as 70g/ by oxide
L；
(7), the solution obtained after step (6) processing is heated to 50 DEG C, starts stirring and add in the ammonium hydrogen carbonate after refining
Solution, the ammonium bicarbonate soln after refining refer to that ammonium hydrogen carbonate solution concentration after double-filtration is 80g/L；Previous hour stirs
Speed control is mixed at 28 revs/min, ammonium bicarbonate soln flow control was at 1.5L/ minutes；Mixing speed control exists after one hour
31 revs/min, for ammonium bicarbonate soln flow control at 2.1L/ minutes, it was 6.5 to be precipitated to solution PH, and 30 are stood after the completion of precipitation
Minute；
(8), it by the precipitation washing in step (7) twice, is then centrifuged for being dehydrated, pack.
Embodiment two
A kind of production method of the big grain size cerous carbonate of high-purity, step are as follows：
(1), 1 part of cerous carbonate is added in 1.5 parts of deionized water and stirred and form mixed liquor；
(2), add in concentrated nitric acid into the mixed liquor that step (1) obtains, stir while adding until mixed liquor it is limpid, be used in combination
Cerous carbonate tune pH value is heated to boiling to 1.2, then adjusts pH to 4.3 with ammonium bicarbonate soln, and boiling is kept for 30 minutes or more,
Obtain trivalent cerium solution；
(3), by the trivalent cerium solution obtained in step (2) first with 200 mesh filter-cloth filterings, then the micropore mistake with aperture 3um
Filter double-filtration obtains filtrate；
(4), the filtrate in step (3) is concentrated, striking point solution concentration is calculated as 750 g/l by cerium oxide；
(5), the concentrate obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifugal dehydration；
(6), the crystal after the centrifugation in step (5) is dissolved in water and diluted, cerium concentration is made to be calculated as 75g/ by oxide
L；
(7), the solution obtained after step (6) processing is heated to 53 DEG C, starts stirring and add in the ammonium hydrogen carbonate after refining
Solution, the ammonium bicarbonate soln after refining refer to that ammonium hydrogen carbonate solution concentration after double-filtration is 80g/L；Previous hour stirs
Speed control is mixed at 29 revs/min, ammonium bicarbonate soln flow control was at 1.8L/ minutes；Mixing speed control exists after one hour
33 revs/min, for ammonium bicarbonate soln flow control at 2.3L/ minutes, it was 6.8 to be precipitated to solution PH, and 30 are stood after the completion of precipitation
Minute；
(8), it by the precipitation washing in step (7) twice, is then centrifuged for being dehydrated, pack.
Embodiment three
A kind of production method of the big grain size cerous carbonate of high-purity, step are as follows：
(1), 1 part of cerous carbonate is added in 1 part of deionized water and stirred and form mixed liquor；
(2), add in concentrated nitric acid into the mixed liquor that step (1) obtains, stir while adding until mixed liquor it is limpid, be used in combination
Cerous carbonate tune pH value is heated to boiling to 1.5, then adjusts pH to 4.5 with ammonium bicarbonate soln, and boiling is kept for 30 minutes or more,
Obtain trivalent cerium solution；
(3), by the trivalent cerium solution obtained in step (2) first with 200 mesh filter-cloth filterings, then the micropore mistake with aperture 5um
Filter double-filtration obtains filtrate；
(4), the filtrate in step (3) is concentrated, striking point solution concentration is calculated as 750 g/l by cerium oxide；
(5), the concentrate obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifugal dehydration；
(6), the crystal after the centrifugation in step (5) is dissolved in water and diluted, cerium concentration is made to be calculated as 80g/ by oxide
L；
(7), the solution obtained after step (6) processing is heated to 55 DEG C, starts stirring and add in the ammonium hydrogen carbonate after refining
Solution, the ammonium bicarbonate soln after refining refer to that ammonium hydrogen carbonate solution concentration after double-filtration is 80g/L；Previous hour stirs
Speed control is mixed at 30 revs/min, ammonium bicarbonate soln flow control was at 2.0L/ minutes；Mixing speed control exists after one hour
35 revs/min, for ammonium bicarbonate soln flow control at 2.5L/ minutes, it was 7 to be precipitated to solution PH, and 30 points are stood after the completion of precipitation
Clock；
(8), it by the precipitation washing in step (7) twice, is then centrifuged for being dehydrated, pack.
Example IV
A kind of production method of the big grain size cerous carbonate of high-purity, step are as follows：
(1), 1 part of cerous carbonate is added in 1.2 parts of deionized water and stirred and form mixed liquor；
(2), add in concentrated nitric acid into the mixed liquor that step (1) obtains, stir while adding until mixed liquor it is limpid, be used in combination
Cerous carbonate tune pH value is heated to boiling, then adjust pH to 4 with ammonium bicarbonate soln, boiling is kept for 30 minutes or more, obtained to 1
Trivalent cerium solution；
(3), by the trivalent cerium solution obtained in step (2) first with 200 mesh filter-cloth filterings, then the micropore mistake with aperture 1um
Filter double-filtration obtains filtrate；
(4), the filtrate in step (3) is concentrated, striking point solution concentration is calculated as 750 g/l by cerium oxide；
(5), the concentrate obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifugal dehydration；
(6), the crystal after the centrifugation in step (5) is dissolved in water and diluted, cerium concentration is made to be calculated as 70g/ by oxide
L；
(7), the solution obtained after step (6) processing is heated to 35 DEG C, starts stirring and add in the ammonium hydrogen carbonate after refining
Solution, the ammonium bicarbonate soln after refining refer to that ammonium hydrogen carbonate solution concentration after double-filtration is 80g/L；Previous hour stirs
Speed control is mixed at 20 revs/min, ammonium bicarbonate soln flow control was at 1.0L/ minutes；Mixing speed control exists after one hour
20 revs/min, for ammonium bicarbonate soln flow control at 1.2L/ minutes, it was 6.0 to be precipitated to solution PH, and 30 are stood after the completion of precipitation
Minute；
(8), it by the precipitation washing in step (7) twice, is then centrifuged for being dehydrated, pack.
Embodiment five
A kind of production method of the big grain size cerous carbonate of high-purity, step are as follows：
(1), 1 part of cerous carbonate is added in 1.2 parts of deionized water and stirred and form mixed liquor；
(2), add in concentrated nitric acid into the mixed liquor that step (1) obtains, stir while adding until mixed liquor it is limpid, be used in combination
Cerous carbonate tune pH value is heated to boiling, then adjust pH to 4 with ammonium bicarbonate soln, boiling is kept for 30 minutes or more, obtained to 1
Trivalent cerium solution；
(3), by the trivalent cerium solution obtained in step (2) first with 200 mesh filter-cloth filterings, then the micropore mistake with aperture 1um
Filter double-filtration obtains filtrate；
(4), the filtrate in step (3) is concentrated, striking point solution concentration is calculated as 750 g/l by cerium oxide；
(5), the concentrate obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifugal dehydration；
(6), the crystal after the centrifugation in step (5) is dissolved in water and diluted, cerium concentration is made to be calculated as 70g/ by oxide
L；
(7), the solution obtained after step (6) processing is heated to 66 DEG C, starts stirring and add in the ammonium hydrogen carbonate after refining
Solution, the ammonium bicarbonate soln after refining refer to that ammonium hydrogen carbonate solution concentration after double-filtration is 80g/L；Previous hour stirs
Speed control is mixed at 40 revs/min, ammonium bicarbonate soln flow control was at 3.0L/ minutes；Mixing speed control exists after one hour
40 revs/min, for ammonium bicarbonate soln flow control at 4.0L/ minutes, it was 8 to be precipitated to solution PH, and 35 points are stood after the completion of precipitation
Clock；
(8), it by the precipitation washing in step (7) twice, is then centrifuged for being dehydrated, pack.
Each parameter value of cerous carbonate prepared by 1. three above embodiment of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of production method of the big grain size cerous carbonate of high-purity, which is characterized in that step is as follows：
(1), cerous carbonate is added to the water to form mixed liquor；
(2), it is limpid that concentrated nitric acid dissolving is added in into the mixed liquor that step (1) obtains, and with cerous carbonate tune pH value to 1-1.5, is added
PH to 4-4.5 is adjusted with ammonium bicarbonate soln again after heat, obtains trivalent cerium solution；
(3), the trivalent cerium solution obtained in step (2) is obtained into filtrate by three-stage filtration；
(4), the filtrate in step (3) is concentrated, striking point solution concentration is calculated as 750 g/l by cerium oxide；
(5), the concentrate obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifugal dehydration；
(6), the crystal after the centrifugation in step (5) is dissolved in water and diluted, cerium concentration is made to be calculated as 70-80g/L by oxide；
(7), the solution obtained after step (6) processing is heated to 50-55 DEG C, it is molten starts the ammonium hydrogen carbonate that stirring is added in after refining
Liquid, previous hour mixing speed control is at 28-30 revs/min, and ammonium bicarbonate soln flow control was at 1.5-2.0L/ minutes；
At 31-35 revs/min, ammonium bicarbonate soln flow control was precipitated at 2.1-2.5L/ minutes for mixing speed control after one hour
Solution PH 6.5-7, precipitation stand 30 minutes after the completion；
(8), the precipitation in step (7) is washed, is then centrifuged for being dehydrated, pack.
A kind of 2. production method of the big grain size cerous carbonate of high-purity according to claim 1, which is characterized in that step (1)
In, the weight ratio of cerous carbonate and water is 1 ︰ 1.5.
A kind of 3. production method of the big grain size cerous carbonate of high-purity according to claim 1, which is characterized in that step (2)
In, the method for heating is：It is heated to boil, be kept for 30 minutes or more.
A kind of 4. production method of the big grain size cerous carbonate of high-purity according to claim 1, which is characterized in that step (3)
In, the method for filtering is：First with 200 mesh filter-cloth filterings, then the millipore filter double-filtration with aperture 1-5um.
A kind of 5. production method of the big grain size cerous carbonate of high-purity according to claim 1, which is characterized in that step (7)
In, ammonium hydrogen carbonate solution concentration after double-filtration is 80g/L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925844A (en) * | 2015-06-11 | 2015-09-23 | 乐山沃耐稀电子材料有限公司 | Method for refining high-purity cerium carbonate |
| CN106315655A (en) * | 2016-07-28 | 2017-01-11 | 乐山沃耐稀电子材料有限公司 | Method for producing high-purity lanthanum carbonate |
| CN106335920A (en) * | 2016-07-28 | 2017-01-18 | 乐山沃耐稀电子材料有限公司 | Production technology of low-chlorine cerium carbonate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925844A (en) * | 2015-06-11 | 2015-09-23 | 乐山沃耐稀电子材料有限公司 | Method for refining high-purity cerium carbonate |
| CN106315655A (en) * | 2016-07-28 | 2017-01-11 | 乐山沃耐稀电子材料有限公司 | Method for producing high-purity lanthanum carbonate |
| CN106335920A (en) * | 2016-07-28 | 2017-01-18 | 乐山沃耐稀电子材料有限公司 | Production technology of low-chlorine cerium carbonate |
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Application publication date: 20180629 |