CN101633515A - Preparation method of large-proportion praseodymium oxide - Google Patents
Preparation method of large-proportion praseodymium oxide Download PDFInfo
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- CN101633515A CN101633515A CN200810150417A CN200810150417A CN101633515A CN 101633515 A CN101633515 A CN 101633515A CN 200810150417 A CN200810150417 A CN 200810150417A CN 200810150417 A CN200810150417 A CN 200810150417A CN 101633515 A CN101633515 A CN 101633515A
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- praseodymium
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Abstract
The invention discloses a preparation method of large-proportion praseodymium oxide. In the process, the large-proportion praseodymium oxide is prepared by controlling the precipitation reaction condition, taking praseodymium chloride solution as a raw material, taking ammonium bicarbonate as the precipitating agent, and controlling the main factors affecting the proportion of praseodymium oxide such as precipitation temperature, feed liquid concentration, precipitation time and the like by controlling the process engineering condition of precipitation. The carbonate prepared by ammonium bicarbonate solution can be directly washed without aging, simultaneously the prepared carbonate has high density, large proportion, large particles, fast clarification and good filter performance, and the loose oxide of the carbonate after calcined decomposition has large proportion. The process flow is short, the purity of praseodymium oxide is greater than or equal to 99.9%, and the yield coefficient of rare earth can be up to as high as 99.5%, thereby being convenient for operation, reducing loss when preparing metal praseodymium by electrolyzation, and reducing production cost.
Description
Technical field
The invention belongs to chemical field, particularly a kind of vegetation method of large-proportion praseodymium oxide.
Background technology
Praseodymium is the rare earth element of large usage quantity, and it is mainly used in glass, pottery and the magneticsubstance.Praseodymium trioxide electroconductibility is good.Being the raw material of producing metal praseodymium and samarium praseodymium brill permanent magnet alloy, also is the raw material of system praseodymium yellow, also is used as glass industry tinting material etc.The preparation Praseodymium trioxide normally obtains after high-temperature calcination with praseodymium carbonate in the industrial production, and the intermediate praseodymium carbonate of preparation Praseodymium trioxide normally prepares under the processing condition that add 40 ℃～70 ℃ of crystal seeds, the Praseodymium trioxide loose specific weight that the praseodymium carbonate of this method preparation obtains after calcining is 0.5～0.7g/cm
3, the Praseodymium trioxide light specific gravity that old technology is produced, loss is big when electrolytic preparation metal praseodymium, yield is low, has increased production cost.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method that can prepare than the large-proportion praseodymium oxide great, that particle big, the loss of metal praseodymium is little.
For achieving the above object, a kind of large-proportion praseodymium oxide of the present invention makes by following steps:
One, to be raw material except that the quantitative praseodymium chloride solution behind the aluminium, in this praseodymium chloride solution, the concentration of praseodymium chloride is 0.7～1.2mol/l, and allotment pH value of solution to 2.5～3.0 are stand-by;
Two, quantitative bicarbonate of ammonia is dissolved in the deionized water, makes the aqueous solution that concentration is 1.5-2.5mol/l;
Three, the ammonium bicarbonate soln for preparing in the praseodymium chloride solution for preparing in the step 1 and the step 2 is mixed, carry out precipitin reaction, precipitation temperature is greater than 90 ℃, and sedimentation time is 120 minutes～150 minutes, and the gained throw out is stand-by;
Four, with behind the prepared throw out usefulness deionized water wash in the step 3 3～5 times, refilter, obtain the praseodymium carbonate solid;
Five, the praseodymium carbonate that makes in the step 4 is placed the tunnel calcining kiln,, can obtain the oarse-grained Praseodymium trioxide product of big proportion 1000 ℃～1100 ℃ following calcinations 3～5 hours.
This technology is by control precipitin reaction condition, with praseodymium chloride solution is raw material, with bicarbonate of ammonia is precipitation agent, and by controlling sedimentary technology condition, to influencing the principal element of Praseodymium trioxide proportion: precipitation temperature, feed concentration, sedimentation time etc. are controlled the preparation large-proportion praseodymium oxide.Carbonate with ammonium bicarbonate soln preparation does not need ageing directly to wash, Zhi Bei carbonate densification simultaneously, than great, particle big, clarification soon, strainability is good, carbonate calcining and decomposing rear oxidation thing loose specific weight is big.This technical process is brief, and the purity of Praseodymium trioxide 〉=99.9%, rare earth yield are convenient to operation up to 99.5%, have reduced loss during than electrolytic preparation metal praseodymium, have reduced production cost.
With praseodymium chloride solution is raw material, is easy to large-scale production.
Embodiment
Embodiment 1
In settling bath, add praseodymium chloride solution 2.5m
3, being made into concentration with deionized water is 0.7mol/l solution, transfers pH to 2.5～3.0 with bicarbonate of ammonia.Claim bicarbonate of ammonia 1500Kg to add in the dissolving tank, add deionized water and be made into the ammonium bicarbonate soln that concentration is 1.5mol/l, the ammonium bicarbonate soln that dissolving is good is squeezed in the high-order storage tank of ammonium bicarbonate soln with the trifluoro pump, then under condition of stirring, ammonium bicarbonate soln is joined in the praseodymium chloride solution and precipitates under the situation of gravity flow, precipitation temperature is controlled at greater than 95 ℃, sedimentation time 120 minutes, and precipitation finishes.Directly draw up clear liquid after waiting to clarify and in settling bath, use deionized water wash number of times 4 times, then throw out is filtered with the vacuum suction filter dish, obtain the praseodymium carbonate intermediates, at last praseodymium carbonate is placed calcining kiln 1000 ℃ of calcinings in tunnel to obtain the oarse-grained Praseodymium trioxide product of big proportion in 3 hours.
Embodiment 2
In settling bath, add praseodymium chloride solution 2.8m
3, being made into concentration with deionized water is 1mol/l solution, transfers pH to 2.5～3.0 with bicarbonate of ammonia.Claim bicarbonate of ammonia 1500Kg to add in the dissolving tank, add deionized water and be made into the ammonium bicarbonate soln that concentration is 2.5mol/l, the ammonium bicarbonate soln that dissolving is good is squeezed in the high-order storage tank of ammonium bicarbonate soln with the trifluoro pump, then under condition of stirring, ammonium bicarbonate soln is joined in the praseodymium chloride solution and precipitates under the situation of gravity flow, precipitation temperature is controlled at greater than 95 ℃, sedimentation time 150 minutes, directly draw up clear liquid after waiting to clarify after precipitation finishes and in settling bath, use deionized water wash number of times 4 times, then throw out is filtered with the vacuum suction filter dish, obtain the praseodymium carbonate intermediates, at last praseodymium carbonate is placed calcining kiln 1000 ℃ of calcinings in tunnel to obtain the oarse-grained Praseodymium trioxide product of big proportion in 4 hours.
Embodiment 3
In settling bath, add praseodymium chloride solution 3m
3, being made into concentration with deionized water is 1.2mol/l solution, transfers pH to 2.5～3.0 with bicarbonate of ammonia.Claim bicarbonate of ammonia 1500Kg to add in the dissolving tank, add deionized water and be made into the ammonium bicarbonate soln that concentration is 2.5molg/l, the ammonium bicarbonate soln that dissolving is good is squeezed in the high-order storage tank of ammonium bicarbonate soln with the trifluoro pump, then under condition of stirring, ammonium bicarbonate soln is joined in the praseodymium chloride solution and precipitates under the situation of gravity flow, precipitation temperature is controlled at greater than 95 ℃, sedimentation time 150 minutes, directly draw up clear liquid after waiting to clarify after precipitation finishes and in settling bath, use deionized water wash number of times 4 times, then throw out is filtered with the vacuum suction filter dish, obtain the praseodymium carbonate intermediates, at last praseodymium carbonate is placed calcining kiln 1100 ℃ of calcinings in tunnel to obtain the oarse-grained Praseodymium trioxide product of big proportion in 4 hours.
Claims (1)
1. the preparation method of a large-proportion praseodymium oxide, it is characterized in that: described large-proportion praseodymium oxide makes by following steps,
One, to be raw material except that the quantitative praseodymium chloride solution behind the aluminium, in this praseodymium chloride solution, the concentration of praseodymium chloride is 0.7～1.2mol/l, and allotment pH value of solution to 2.5～3.0 are stand-by;
Two, quantitative bicarbonate of ammonia is dissolved in the deionized water, makes the aqueous solution that concentration is 1.5-2.5mol/l;
Three, the ammonium bicarbonate soln for preparing in the praseodymium chloride solution for preparing in the step 1 and the step 2 is mixed, carry out precipitin reaction, precipitation temperature is greater than 90 ℃, and sedimentation time is 120 minutes～150 minutes, and the gained throw out is stand-by;
Four, with behind the prepared throw out usefulness deionized water wash in the step 3 3～5 times, refilter, obtain the praseodymium carbonate solid;
Five, the praseodymium carbonate that makes in the step 4 is placed the tunnel calcining kiln,, can obtain the oarse-grained Praseodymium trioxide product of big proportion 1000 ℃～1100 ℃ following calcinations 3～5 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810150417A CN101633515A (en) | 2008-07-23 | 2008-07-23 | Preparation method of large-proportion praseodymium oxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983926A (en) * | 2010-11-12 | 2011-03-09 | 北京工业大学 | Method for preparing three-dimensional ordered macroporous praseodymium oxide and terbium oxide with mesoporous walls |
| CN103276440A (en) * | 2013-06-15 | 2013-09-04 | 清远市嘉禾稀有金属有限公司 | Processing method for rare earth carbonate with low chlorine ions |
| CN106517295A (en) * | 2016-10-18 | 2017-03-22 | 西北工业大学 | Method for synthesizing high-stability gamma-Pr2S3 powder |
-
2008
- 2008-07-23 CN CN200810150417A patent/CN101633515A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983926A (en) * | 2010-11-12 | 2011-03-09 | 北京工业大学 | Method for preparing three-dimensional ordered macroporous praseodymium oxide and terbium oxide with mesoporous walls |
| CN103276440A (en) * | 2013-06-15 | 2013-09-04 | 清远市嘉禾稀有金属有限公司 | Processing method for rare earth carbonate with low chlorine ions |
| CN103276440B (en) * | 2013-06-15 | 2015-09-02 | 清远市嘉禾稀有金属有限公司 | A kind of low chlorine root rare earth carbonate working method |
| CN106517295A (en) * | 2016-10-18 | 2017-03-22 | 西北工业大学 | Method for synthesizing high-stability gamma-Pr2S3 powder |
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Application publication date: 20100127 |