CN101898785B - Method for reducing content of Al2O3 in neodymium carbonate and praseodymium-neodymium carbonate product - Google Patents
Method for reducing content of Al2O3 in neodymium carbonate and praseodymium-neodymium carbonate product Download PDFInfo
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- CN101898785B CN101898785B CN 200910022679 CN200910022679A CN101898785B CN 101898785 B CN101898785 B CN 101898785B CN 200910022679 CN200910022679 CN 200910022679 CN 200910022679 A CN200910022679 A CN 200910022679A CN 101898785 B CN101898785 B CN 101898785B
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Abstract
The invention discloses a method for reducing the content of Al2O3 in a neodymium oxide and praseodymium-neodymium oxide product. The method can ensure that the content of Al2O3 in a neodymium oxide product prepared by calcinating neodymium carbonate is less than 100ppm by taking the solution of neodymium chloride and praseodymium-neodymium chloride as a raw material and an industry sulfosalicylic acid as a complexing agent. Therefore, the method has the advantages of greatly improving the quality of the product, ensuring the product quality and reducing the content of impurities in the product.
Description
Technical field
The invention belongs to the rare earth material preparation field, particularly Al in a kind of reduction neodymium carbonate, the praseodymium carbonate neodymium product
2O
3The method of content.
Background technology
Making behind the neodymium metal as the main component of sintering and boned neodymium iron boron permanent magnet with purity 〉=99% Neodymium trioxide, is the Application Areas with very big development potentiality; After in the rare earth laserable material, adding purity 〉=99.99% Neodymium trioxide, can obtain good laserable material, the laser that they produce is a kind of novel light source: have monochromaticity, directivity and coherency preferably, can obtain very high brightness again, obtained practical application in fields such as industry, agricultural, medicine and defence and militaries, its use potentiality and development prospect are better; After in the glass of different components, adding purity 〉=99% Neodymium trioxide, can effectively improve glass properties and show specific color, improve the factor of merit of glass; Can make laser generation matter, image intensifer and fiber sensor etc. after in quartz is the heart yearn of single mode transmission glass fibre, adding purity 〉=99% Neodymium trioxide; Purity 〉=99% Neodymium trioxide is added in the stupalith, can improve coking property, density, microstructure and the phase composite etc. of pottery, can satisfy quality and the performance demands of different potteries; Characteristics such as add purity 〉=99% Neodymium trioxide in the radio ceramics dielectric material after, the capacitor ceramic dielectric of making has that medium coefficient is not high, dielectric loss is low, the loss heating is little under working conditions, dielectric properties greatly improve.The Pr-Nb fused alumina emery wheel can improve the use properties of emery wheel, and it is fast that it is lived down, and sticking scrap metal again and does not add Praseodymium trioxide neodymium emery wheel relatively, and the grinding rate can improve 30 ~ 100%, improve 1 times work-ing life.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with Neodymium trichloride, praseodymium chloride neodymium solution, and the technical grade sulphosalicylic acid is network and agent, can make the calcination neodymium carbonate and the Neodymium trioxide product in alumina content less than the method for 100ppm.
For achieving the above object, Al in a kind of reduction neodymium carbonate of the present invention, the praseodymium carbonate neodymium product
2O
3The method of content realizes by following processing step:
One, take by weighing a certain amount of sulphosalicylic acid in proportion, the aqueous solution that is mixed with 15%-20% with water is stand-by;
Two, Neodymium trichloride or praseodymium chloride neodymium solution are pumped into 3M
3Behind the enamel groove, be warming up to the 55-60 degree, start and stir, a kind of sulphosalicylic acid solution for preparing of step is evenly joined the enamel groove, continue to stop to stir behind the stirring 25min, wait to precipitate;
Three, Neodymium trichloride or the praseodymium chloride neodymium solution of crossing with the agricultural ammonium bicarbonate precipitation process is washed 2 times to remove the non-rare earth impurity of carrying secretly in the precipitation with deionized water, and centrifuge dewatering obtains solid carbonic acid neodymium or praseodymium carbonate neodymium; Be 99.5% with obtaining purity after solid carbonic acid neodymium or the high-temperature calcination of praseodymium carbonate neodymium, alumina content is less than Neodymium trioxide or the Praseodymium trioxide neodymium product of 100ppm.
By Al in above-mentioned reduction neodymium carbonate, the praseodymium carbonate neodymium product
2O
3The method of content owing to be raw material with Neodymium trichloride, praseodymium chloride neodymium solution, the technical grade sulphosalicylic acid is network and agent, can make the calcination neodymium carbonate and the Neodymium trioxide product in alumina content less than 100ppm.So just improve the quality of product greatly, guaranteed quality product, reduced the content of impurity in the product.
Embodiment
Embodiment 1
The 14.65Kg sulphosalicylic acid divided drop into for 4 times in the 20L plastic tank, add 18L pure water stirring and dissolving, after treating to dissolve fully, neodymium chloride solution is pumped into 3m
3Behind the enamel groove, be warming up to 56 degree.Start and stir, the sulphosalicylic acid solution for preparing is evenly joined the enamel groove, continue to stir 25min.Stop to stir, the neodymium chloride solution after handling is pumped into 20m
3Settling bath is waited to precipitate.Repeat above operation, until with 8m
3Till the neodymium chloride solution of rare-earth oxidation amount REO=0.88mol/l handled.To 20m
3Evenly slowly add ammonium bicarbonate solution in the settling bath, survey the solution pH value with test paper behind the 4.5h, just stop precipitation as PH=6.5.Behind the ageing 2h, wash 2 times.Neodymium carbonate precipitation after the washing enters centrifuge dewatering, is packaged as neodymium carbonate salt, and it is 99.5% that neodymium carbonate obtains purity after the packing through 1150 ℃ of calcinings after 6 hours, and alumina content is less than the Neodymium trioxide product of 100ppm.
Embodiment 2
The 15.35Kg sulphosalicylic acid divided drop into for 4 times in the 20L plastic tank, add 19.2L pure water stirring and dissolving, after treating to dissolve fully, praseodymium chloride neodymium solution is pumped into 3m
3Behind the enamel groove, be warming up to 55 degree.Start and stir, the sulphosalicylic acid solution for preparing is evenly joined the enamel groove, continue to stir 25min.Stop to stir, the praseodymium chloride neodymium solution after handling is pumped into 20m
3Settling bath is waited to precipitate.Repeat above operation, until with 9.4m
3Till the praseodymium chloride neodymium solution-treated of rare-earth oxidation amount REO=0.87mol/l is intact.To 20m
3Evenly slowly add ammonium bicarbonate solution in the settling bath, survey the solution pH value with test paper behind the 4.5h, stop precipitation as PH=6.5.Behind the ageing 2h, wash 2 times.Praseodymium carbonate neodymium precipitation after the washing enters centrifuge dewatering, is packaged as praseodymium carbonate neodymium salt, and it is 99.5% that the praseodymium carbonate neodymium obtains purity after the packing through 1150 ℃ of calcinings after 6 hours, and alumina content is less than the Praseodymium trioxide neodymium product of 100ppm.
Embodiment 3
The 15.45Kg sulphosalicylic acid divided drop into for 4 times in the 20L plastic tank, add 19.3L pure water stirring and dissolving, after treating to dissolve fully, neodymium chloride solution is pumped into 3m
3Behind the enamel groove, be warming up to 57 degree.Start and stir, the sulphosalicylic acid solution for preparing is evenly joined the enamel groove, continue to stir 25min.Stop to stir, the neodymium chloride solution after handling is pumped into 20m
3Settling bath is waited to precipitate.Repeat above operation, until with 10.2m
3Till the neodymium chloride solution of rare-earth oxidation amount REO=0.92mol/l is handled.To 20m
3Evenly slowly add ammonium bicarbonate solution in the settling bath, survey the solution pH value with test paper behind the 4.5h, stop precipitation as PH=6.5.Behind the ageing 2h, wash 2 times.Neodymium carbonate precipitation after the washing enters centrifuge dewatering, is packaged as neodymium carbonate salt, and it is 99.5% that neodymium carbonate obtains purity after the packing through 1150 ℃ of calcinings after 6 hours, and alumina content is less than the Neodymium trioxide product of 100ppm.
Claims (2)
1. one kind is reduced Al in the Neodymium trioxide product
2O
3The method of content is characterized in that: this method realizes by following processing step:
One, take by weighing a certain amount of sulphosalicylic acid in proportion, be mixed with 15% ~ 20% the aqueous solution with water stand-by;
Two, neodymium chloride solution is pumped into 3m
3Behind the enamel groove, be warming up to 55 degree, start and stir, the sulphosalicylic acid solution for preparing in the step 1 is evenly joined the enamel groove, continue to stop to stir behind the stirring 25min, wait to precipitate;
Three, the neodymium chloride solution of crossing with the agricultural ammonium bicarbonate precipitation process is washed 2 times to remove the non-rare earth impurity of carrying secretly in the precipitation with deionized water, and centrifuge dewatering obtains the solid carbonic acid neodymium; It is 99.5% that the solid carbonic acid neodymium is obtained purity after through 1150 ℃ of calcinings, and alumina content is less than the Neodymium trioxide product of 100ppm.
2. one kind is reduced Al in the Praseodymium trioxide neodymium product
2O
3The method of content is characterized in that: this method realizes by following processing step:
One, take by weighing a certain amount of sulphosalicylic acid in proportion, be mixed with 15% ~ 20% the aqueous solution with water stand-by;
Two, praseodymium chloride neodymium solution is pumped into 3m
3Behind the enamel groove, be warming up to 55 degree, start and stir, the sulphosalicylic acid solution for preparing in the step 1 is evenly joined the enamel groove, continue to stop to stir behind the stirring 25min, wait to precipitate;
Three, the praseodymium chloride neodymium solution of crossing with the agricultural ammonium bicarbonate precipitation process is washed 2 times to remove the non-rare earth impurity of carrying secretly in the precipitation with deionized water, and centrifuge dewatering obtains solid carbonic acid praseodymium neodymium; It is 99.5% that solid carbonic acid praseodymium neodymium is obtained purity after through 1150 ℃ of calcinings, and alumina content is less than the Praseodymium trioxide neodymium product of 100ppm.
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CN102531024A (en) * | 2011-10-28 | 2012-07-04 | 内蒙古科技大学 | Method for preparing large-grain spherical praseodymium neodymium oxide |
CN103864131B (en) * | 2014-01-28 | 2015-08-26 | 福建省长汀金龙稀土有限公司 | A kind of preparation method of praseodymium neodymium oxide |
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CN101306829A (en) * | 2008-07-01 | 2008-11-19 | 上海大学 | Dendritic basic neodymium carbonate and neodymium oxide nano materials and method for preparing same |
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CN101306829A (en) * | 2008-07-01 | 2008-11-19 | 上海大学 | Dendritic basic neodymium carbonate and neodymium oxide nano materials and method for preparing same |
Non-Patent Citations (3)
Title |
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孙肃 等.降低氯化钕溶液中铝离子的工艺研究.《无机盐工业》.2007,第39卷(第11期),34-35、43. * |
王毅军 等.快速沉淀晶型碳酸钕的试验研究.《湿法冶金》.2004,第23卷(第1期),40-42. * |
许延辉.从碳酸镨钕中除铝的研究.《湿法冶金》.2005,第24卷(第2期),92-94. * |
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