CN106277021A - A kind of large-specific surface area nano Dineodymium trioxide preparation method - Google Patents
A kind of large-specific surface area nano Dineodymium trioxide preparation method Download PDFInfo
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- CN106277021A CN106277021A CN201510321399.8A CN201510321399A CN106277021A CN 106277021 A CN106277021 A CN 106277021A CN 201510321399 A CN201510321399 A CN 201510321399A CN 106277021 A CN106277021 A CN 106277021A
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Abstract
The invention belongs to the preparing technical field of rare earth oxide, particularly relate to the preparation method of a kind of large-specific surface area nano Dineodymium trioxide, described method includes: add surfactant in the inorganic salt solution containing neodymium, again precipitant is instilled in above-mentioned solution, two kinds of solution are enable fully to react by stirring, it is precipitated thing through ageing again, then precipitate is washed with deionized, is vacuum dried, obtains after calcination the Nanometer-sized Neodymium Oxide powder body of bigger serface.The present invention application by surfactant, controls precipitant concentration, rate of addition, and prepared Nanometer-sized Neodymium Oxide TEM detection primary particle size 20～60nm and specific surface area are 60～100m2/g.Present invention process is simple, cost is relatively low, controllability is high, increases significantly product purity and yield, and not pollutes environment, is suitable for industrialized production.
Description
Technical field
The invention belongs to the preparing technical field of rare earth oxide, particularly relate to the preparation method of a kind of bigger serface Dineodymium trioxide.
Background technology
Dineodymium trioxide is a kind of purposes and rare earth oxide widely thereof, it is mainly used in neodymium iron boron (Nd-Fe-B) permanent magnet, TV glass bulb, glass coloration, fluorescent material, laser material and rubber industry additive, because the tone of Dineodymium trioxide is graceful, and have good discoloration, it is also extensively used for the high-tech areas such as pottery, dope dyeing, superconduction and other functional materials, and growth is the most violent.The research applied Dineodymium trioxide at catalytic field in recent years is the most increasingly extensive, and such as catalysis polycarboxylic acids synthesis, fatty alcohol amination, synthetic rubber etc., the especially Nanometer-sized Neodymium Oxide of bigger serface has better properties and purposes, and its catalysis activity is higher.In magnesium alloy or aluminium alloy, add 1.5%～2.5% Nanometer-sized Neodymium Oxide, heavy alloyed high-temperature behavior, air-tightness and corrosion resistance can be put forward, be widely used as aerospace material.It addition, the nano oxidized yttrium-aluminium-garnet mixing Nanometer-sized Neodymium Oxide produces laser beam, industrially it is widely used in welding and the cutting of the following thin material of thickness 10mm.Medically, the nano oxidized YAG laser mixing Nanometer-sized Neodymium Oxide replaces scalpel for excising operation or sterilization wound mouth.
The specific surface area of Nanometer-sized Neodymium Oxide prepared by prior art is both less than 50 m2/ g, technique is the most complicated simultaneously, and production cost is higher, is unfavorable for mass production, and raw materials used have pollution to environment, not environmentally.
Summary of the invention
It is an object of the invention to break through the bottleneck that prior art exists, it is provided that a kind of large-specific surface area nano Dineodymium trioxide and preparation method thereof.
The technical scheme realizing the object of the invention comprises the steps:
(1) in the inorganic salt solution containing neodymium, surfactant is added；
(2) instilling precipitant in the inorganic salt solution containing neodymium, regulation reacting system PH value is to 11；
(3), after dropping, reaction system is stirred, is aged, be precipitated thing；
(4) precipitate is washed with deionized, then is vacuum dried；
(5) the precipitate high temperature sintering after vacuum drying is obtained the Nanometer-sized Neodymium Oxide of bigger serface.
Technique scheme, described in step (1), the inorganic salt solution containing neodymium is at least one in Neodymium chloride, neodymium nitrate, and the concentration of the described inorganic salt solution containing neodymium is 0.2mol/L～0.6mol/L.
Technique scheme, described in step (1), surfactant is dodecylbenzene sodium sulfonate or PEG 20000, and the quality of described surfactant is described containing in neodymium inorganic salt solution the 3%～6% of Dineodymium trioxide quality.
Technique scheme, precipitant described in step (2) is the mixture of sodium carbonate, sodium bicarbonate and Disodium oxalate., and ratio is 2:1:1, and described precipitant concentration is 0.3mol/L～0.6mol/L.
Technique scheme, being instilled by precipitant described in step (2) and instilling speed in the inorganic salt solution containing neodymium is 1L/min～2L/min.
Technique scheme, regulates reacting system PH value to 11 described in step (2).
Technique scheme, described in step (3), reaction system mixing time is 0.5～2 hour, and described reaction system Aging Temperature is 30 DEG C～50 DEG C, and digestion time is 3～5 hours.
Technique scheme, in step (4), deionized water temperature is 50 DEG C～60 DEG C, and mode of washing uses centrifugation.
Technique scheme, being vacuum dried temperature described in step (4) is 70 DEG C, and vacuum is 93.3～98.6KPa.
Technique scheme, it is 800 DEG C～1000 DEG C that precipitate described in step (4) carries out calcination temperature, is incubated 3～5 hours.
Using after technique scheme, the present invention has a following positive effect:
(1) present invention is by adding surfactant in the inorganic salt solution containing neodymium, granule surface activity can be increased, change the charge and various chemistry key state of particle surface, increase granule dispersibility each other, preferably control crystal particle diameter size and crystal specific surface area, thus be conducive to prepared Nanometer-sized Neodymium Oxide powder body to have narrower particle diameter distribution and bigger specific surface area；
(2) present invention is 2:1:1 by regulation containing inorganic salt solution concentration 0.2mol/L of neodymium～0.6mol/L and precipitant sodium carbonate, sodium bicarbonate and Disodium oxalate. weight ratio, concentration is 0.3mol/L～0.6mol/L, control rate of addition 1L/min～2L/min, regulation reacting system PH value is to 11, primary particle size 20～60nm, specific surface area 60～100 m can be obtained2The Nanometer-sized Neodymium Oxide powder body of/g.Present invention process is simple, cost is relatively low, controllability is high, increases significantly product purity and yield, and not pollutes environment, is suitable for industrialized production.
Detailed description of the invention
(embodiment 1)
The present invention is the preparation method of a kind of large-specific surface area nano Dineodymium trioxide, and detailed process is as follows:
(1) take the neodymium chloride solution 5.9L of 1.5mol/L, add the deionized water 38.4L that temperature is 50 DEG C, be configured to 0.2mol/L neodymium chloride solution A；
(2) in solution A, add 60g dodecylbenzene sodium sulfonate to be sufficiently stirred for；
(3) take sodium carbonate 800g, sodium bicarbonate 400g and Disodium oxalate. 400g respectively, add the deionized water 51L that temperature is 50 DEG C, be configured to 0.3mol/L solution B；
(4) in the case of solution A continuous stirring, B solution being added drop-wise in solution A, control rate of addition is 1.7L/min, time for adding 30 minutes, and after B solution completion of dropwise addition, the pH value of reaction system is 11, and temperature of reaction system 43 DEG C produces white precipitate simultaneously；
(5) stirring 0.5 hour is continued, then ageing 3 hours；
(6) being washed by precipitate, mode of washing uses centrifugation, with the deionized water wash that temperature is 50 DEG C, is vacuum dried by the precipitate after washing, and vacuum drying temperature is 70 DEG C, and vacuum is 93.3KPa；
(7) precipitate after vacuum drying being carried out high temperature sintering, calcination temperature is 1000 DEG C, is incubated 5 hours；
(8) product Dineodymium trioxide, after testing, specific surface area 73m are finally obtained2/ g, its primary particle size is 20～60nm.
(embodiment 2)
The present invention is the preparation method of a kind of large-specific surface area nano Dineodymium trioxide, and detailed process is as follows:
(1) take the neodymium nitrate solution 4.92L of 1.8mol/L, add the deionized water 17.2L that temperature is 60 DEG C, be configured to 0.4mol/L neodymium nitrate solution A；
(2) in solution A, add 75g dodecylbenzene sodium sulfonate to be sufficiently stirred for；
(3) take sodium carbonate 800g, sodium bicarbonate 400g and Disodium oxalate. 400g respectively, add the deionized water 30.6L that temperature is 60 DEG C, be configured to 0.5mol/L solution B；
(4) in the case of solution A continuous stirring, B solution being added drop-wise in solution A, control rate of addition is 1.02L/min, time for adding 30 minutes, and after B solution completion of dropwise addition, the pH value of reaction system is 11, and temperature of reaction system 47 DEG C produces white precipitate simultaneously；
(5) stirring 2 hours is continued, then ageing 4 hours；
(6) being washed by precipitate, mode of washing uses centrifugation, with the deionized water wash of 60 DEG C, is vacuum dried by the precipitate after washing, and vacuum drying temperature is 70 DEG C, and vacuum is 98.6KPa；
(7) precipitate after vacuum drying being carried out high temperature sintering, calcination temperature is 850 DEG C, is incubated 4 hours；
(8) product Dineodymium trioxide, after testing, specific surface area 84m are finally obtained2/ g, its primary particle size is 20～60nm.
(embodiment 3)
The present invention is the preparation method of a kind of large-specific surface area nano Dineodymium trioxide, and detailed process is as follows:
(1) take the mixed solution 6.33L of the Neodymium chloride of 1.4mol/L, neodymium nitrate, add the deionized water 11.4L that temperature is 55 DEG C, be configured to 0.5mol/L solution A；
(2) in solution A, add 90g PEG 20000 to be sufficiently stirred for；
(3) take sodium carbonate 800g, sodium bicarbonate 400g and Disodium oxalate. 400g respectively, add the deionized water 38.3L that temperature is 55 DEG C, be configured to 0.4mol/L solution B；
(4) in the case of solution A continuous stirring, B solution being added drop-wise in solution A, control rate of addition is 1.28L/min, time for adding 30 minutes, and after B solution completion of dropwise addition, the pH value of reaction system is 11, and temperature of reaction system 45 DEG C produces white precipitate simultaneously；
(5) stirring 1.5 hours is continued, then ageing 5 hours；
(6) being washed by precipitate, mode of washing uses centrifugation, with the deionized water wash of 55 DEG C, is vacuum dried by the precipitate after washing, and vacuum drying temperature is 70 DEG C, and vacuum is 95KPa；
(7) precipitate after vacuum drying being carried out high temperature sintering, calcination temperature is 800 DEG C, is incubated 3 hours；
(8) product Dineodymium trioxide, after testing, specific surface area 95m are finally obtained2/ g, its primary particle size is 20～60nm.
Claims (10)
1. the preparation method of a large-specific surface area nano Dineodymium trioxide, it is characterised in that comprise the following steps:
(1) in the inorganic salt solution containing neodymium, surfactant is added；
(2) instilling precipitant in the inorganic salt solution containing neodymium, regulation reacting system PH value is to alkalescence；
(3), after dropping, reaction system is stirred, is aged, be precipitated thing；
(4) precipitate is washed with deionized, then is vacuum dried；
(5) the precipitate high temperature sintering after vacuum drying is obtained the Nanometer-sized Neodymium Oxide of bigger serface.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterised in that described in step (1), the inorganic salt solution containing neodymium is at least one in Neodymium chloride, neodymium nitrate, and concentration is 0.2mol/L～0.6mol/L.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterized in that, described in step (1), surfactant is dodecylbenzene sodium sulfonate or PEG 20000, and the consumption of described surfactant is described containing in neodymium inorganic salt solution the 3%～6% of neodymium quality.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterised in that precipitant described in step (2) is the mixture of sodium carbonate, sodium bicarbonate and Disodium oxalate., ratio is 2:1:1, and concentration is 0.3mol/L～0.6mol/L.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterised in that being instilled by precipitant described in step (2) and instilling speed in the inorganic salt solution containing neodymium is 1L/min～2L/min.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterised in that regulate reacting system PH value described in step (2) to 11.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterised in that described in step (3), reaction system mixing time is 0.5～2 hour, Aging Temperature is 30 DEG C～50 DEG C, and digestion time is 3～5 hours.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterised in that in step (4), deionized water temperature is 50 DEG C～60 DEG C, mode of washing uses centrifugation.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterised in that being vacuum dried temperature described in step (4) is 70 DEG C, and vacuum is 93.3～98.6KPa.
The preparation method of large-specific surface area nano Dineodymium trioxide the most according to claim 1, it is characterised in that it is 800 DEG C～1000 DEG C that precipitate described in step (4) carries out calcination temperature, is incubated 3～5 hours.
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Cited By (10)
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| CN108217710A (en) * | 2018-01-24 | 2018-06-29 | 常州市卓群纳米新材料有限公司 | A kind of preparation method for being conducive to stablize neodymia particle size distribution |
| CN108285166A (en) * | 2017-01-09 | 2018-07-17 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of ultrafine yttria |
| CN108689422A (en) * | 2018-06-05 | 2018-10-23 | 常州市卓群纳米新材料有限公司 | A kind of large-specific surface area nano gadolinium oxide raw powder's production technology |
| CN109019655A (en) * | 2017-06-09 | 2018-12-18 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of large-specific surface area nano luteium oxide |
| CN109205655A (en) * | 2018-11-23 | 2019-01-15 | 常州市卓群纳米新材料有限公司 | A kind of preparation method for the nano oxidized gadolinium that partial size is 80-100nm |
| CN110510653A (en) * | 2019-09-27 | 2019-11-29 | 内蒙古包钢和发稀土有限公司 | The preparation method of neodymia |
| CN111634935A (en) * | 2020-04-24 | 2020-09-08 | 广西科学院 | Microwave preparation method of nano rare earth oxide |
| CN112010338A (en) * | 2020-07-27 | 2020-12-01 | 常州市卓群纳米新材料有限公司 | Method for preparing low-sodium nanometer ytterbium oxide with good monodispersity by sodium salt precipitation |
| CN112194168A (en) * | 2020-10-26 | 2021-01-08 | 常州市卓群纳米新材料有限公司 | Preparation method of rare earth neodymium oxide |
| CN113149060A (en) * | 2021-04-14 | 2021-07-23 | 中稀(常州)稀土新材料有限公司 | High-purity neodymium oxide high-efficiency iron removal method for industrial processing |
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Cited By (15)
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| CN108285166A (en) * | 2017-01-09 | 2018-07-17 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of ultrafine yttria |
| CN109019655A (en) * | 2017-06-09 | 2018-12-18 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of large-specific surface area nano luteium oxide |
| CN108217710B (en) * | 2018-01-24 | 2020-04-17 | 常州市卓群纳米新材料有限公司 | Preparation method beneficial to stabilizing particle size distribution of neodymium oxide particles |
| CN108217710A (en) * | 2018-01-24 | 2018-06-29 | 常州市卓群纳米新材料有限公司 | A kind of preparation method for being conducive to stablize neodymia particle size distribution |
| CN108689422A (en) * | 2018-06-05 | 2018-10-23 | 常州市卓群纳米新材料有限公司 | A kind of large-specific surface area nano gadolinium oxide raw powder's production technology |
| CN109205655A (en) * | 2018-11-23 | 2019-01-15 | 常州市卓群纳米新材料有限公司 | A kind of preparation method for the nano oxidized gadolinium that partial size is 80-100nm |
| CN109205655B (en) * | 2018-11-23 | 2020-05-12 | 常州市卓群纳米新材料有限公司 | Preparation method of nano gadolinium oxide with particle size of 80-100nm |
| CN110510653A (en) * | 2019-09-27 | 2019-11-29 | 内蒙古包钢和发稀土有限公司 | The preparation method of neodymia |
| CN110510653B (en) * | 2019-09-27 | 2021-11-09 | 内蒙古包钢和发稀土有限公司 | Preparation method of neodymium oxide |
| CN111634935A (en) * | 2020-04-24 | 2020-09-08 | 广西科学院 | Microwave preparation method of nano rare earth oxide |
| CN112010338A (en) * | 2020-07-27 | 2020-12-01 | 常州市卓群纳米新材料有限公司 | Method for preparing low-sodium nanometer ytterbium oxide with good monodispersity by sodium salt precipitation |
| CN112010338B (en) * | 2020-07-27 | 2023-10-31 | 常州市卓群纳米新材料有限公司 | Method for preparing monodisperse low-sodium nanometer ytterbium oxide by sodium salt precipitation |
| CN112194168A (en) * | 2020-10-26 | 2021-01-08 | 常州市卓群纳米新材料有限公司 | Preparation method of rare earth neodymium oxide |
| CN112194168B (en) * | 2020-10-26 | 2023-06-20 | 常州市卓群纳米新材料有限公司 | Preparation method of rare earth neodymium oxide |
| CN113149060A (en) * | 2021-04-14 | 2021-07-23 | 中稀(常州)稀土新材料有限公司 | High-purity neodymium oxide high-efficiency iron removal method for industrial processing |
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Application publication date: 20170104 |