CN108862359B - Preparation method of terbium oxide with D50 of 2-3 mu m - Google Patents
Preparation method of terbium oxide with D50 of 2-3 mu m Download PDFInfo
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- CN108862359B CN108862359B CN201810776222.0A CN201810776222A CN108862359B CN 108862359 B CN108862359 B CN 108862359B CN 201810776222 A CN201810776222 A CN 201810776222A CN 108862359 B CN108862359 B CN 108862359B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a preparation method of D50:2-3 μm terbium oxide, which comprises the following steps of firstly preparing oxalic acid solution, adding polyethylene glycol 20000 with a set mass ratio, stirring until the mixture is uniformly dispersed, then slowly dropwise adding 0.2-0.4mol/L terbium chloride solution while stirring, aging at 0-5 ℃ for 4-5 hours, then carrying out suction filtration and water washing, wherein the water washing temperature is higher than 95 ℃, carrying out water washing and then carrying out filter drying to obtain precipitate, and firing the precipitate at 850-900 ℃ for 3-5 hours to obtain the D50:2-3 μm terbium oxide. The terbium oxide with the specific particle size range prepared by the invention can improve some defects of some lithium iron phosphate materials, thereby effectively improving the specific capacity, the cycle stability, the discharge rate and the like of the battery, and the terbium oxide with the particle size has better chemical performance and electronic performance in the doping improvement of the lithium battery anode material.
Description
Technical Field
The invention belongs to the technical field of rare earth compound ultrafine powder preparation, and particularly relates to a preparation method of terbium oxide with the particle size of D50 being 2-3 mu m.
Background
Terbium oxide is used as a functional material for manufacturing metal terbium, magneto-optical glass, fluorescent powder, magneto-optical storage materials, chemical additives and the like, and can also be used for preparing functional ceramics. However, due to scarcity and high value of terbium oxide, the application field of terbium oxide is limited, and with the development of some industries, a plurality of excellent characteristics of terbium oxide appear. For example, in the lithium battery industry, the performance of a lithium battery is determined by a positive electrode material, a novel lithium iron phosphate material is more and more concerned at present, and the addition of terbium oxide improves some defects of some lithium iron phosphate materials. The terbium oxide with the specific granularity range prepared by the invention has a certain effect, can effectively improve the specific capacity, the cycling stability, the discharge rate and the like of the battery, and reflects better chemical performance and electronic performance in the doping improvement of the lithium battery anode material.
Disclosure of Invention
The invention aims to overcome the technical defects of uneven size distribution and difficult particle control of terbium oxide particles in the existing terbium oxide preparation technology, and provides a preparation method of terbium oxide with the particle size of D50:2-3 mu m.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of D50 terbium oxide with the particle size of 2-3 μm comprises the following steps:
(1) dropwise adding a terbium chloride aqueous solution into the oxalic acid solution in which the polyethylene glycol is uniformly dispersed while stirring, continuously stirring for 10-30min after the dropwise adding is finished, and then standing and aging for 4-5 h to obtain a material mixed solution. Wherein the aging temperature is 0-5 ℃, the concentration of the Chinese herbal acid solution in the material mixed solution is 0.2-0.4mol/L, and the concentration of the terbium chloride aqueous solution is 0.2-0.4 mol/L.
(2) Carrying out suction filtration on the material mixed liquor prepared in the step (1), then washing the material mixed liquor to be neutral, and filtering the material mixed liquor to be dry to prepare a precipitate; wherein the washing temperature is more than or equal to 95 ℃.
(3) And (3) burning the precipitate prepared in the step (2) until the precipitate is decomposed to prepare terbium oxide.
More preferably, the molar ratio of oxalic acid to terbium chloride is 1.5-3: 1. The pH value can be controlled within the range of 6.2-6.8 by the optimization scheme, and the particle size distribution of the terbium oxide can be conveniently controlled within the range of D50:2-3 μm within the pH range.
In the reaction process, oxalic acid reacts with terbium chloride to generate terbium oxalate particles, the directly generated and non-agglomerated terbium oxalate particles are called primary particles, particles formed by agglomeration of the primary particles are called secondary particles, and polyethylene glycol can prevent the primary particles from agglomerating to generate larger secondary particles, so that agglomeration can be effectively prevented, as a further optimization scheme, the mass amount of the polyethylene glycol in the step (1) is 3.5% -5.7% of that of the terbium chloride, wherein the polyethylene glycol is any one or more of polyethylene glycol 20000, polyethylene glycol 2000, polyethylene glycol 1000, polyethylene glycol 3000 and polyethylene glycol 500, and preferably the polyethylene glycol 20000.
The dripping speed of terbium chloride can directly influence the concentration of terbium ions in a system and the reaction speed, so that the size of primary particles is influenced, the primary particles can be agglomerated to generate larger secondary particles due to overhigh dripping speed, and in order to better control the particle size, the dripping speed of the terbium chloride aqueous solution in the step (1) is 4-6L/h as a further optimization scheme.
On the premise of ensuring sufficient reaction, in order to make the particle size of the generated terbium oxide particles more uniform, as a further optimization scheme, the time for continuing stirring after the dropwise addition of the terbium chloride aqueous solution in the step (1) is finished is 15 min.
And (3) when the terbium oxide is obtained through pyrolysis, in order to further optimize the size and specific surface area of terbium oxide particles and avoid agglomeration among the particles, as a further optimization scheme, the ignition temperature in the step (3) is 850-900 ℃, the ignition time is 3-5 hours, and the ignition temperature is 900 ℃ and the ignition time is 3 hours are further preferred.
Through the technical scheme, the beneficial technical effects obtained by the invention are as follows: 1) low-concentration precipitation, low-temperature aging and hot water washing, and the synergistic effect of the three is not sufficient. The low-temperature aging can prevent the grains from growing in the aging process. And the impurities can be effectively removed by hot water washing, and the effective control of the particle size can be further ensured by the other party. 2) Terbium oxide with the proportion of D50:2-3 μm is successfully prepared, and the yield is over 96.5%. 3) The preparation process is simple and the energy consumption is low. 4) Avoids using ammonia precipitator and surfactant, and meets the requirement of environmental protection. 5) The terbium oxide prepared by the invention can effectively improve the specific capacity, the cycling stability, the discharge rate and the like of the battery, and the terbium oxide with the granularity improves the better chemical performance and electronic performance in the doping improvement of the lithium battery anode material.
Detailed Description
The invention is described in more detail below with reference to examples:
example 1:
the specific embodiment adopts the following technical scheme to prepare the terbium oxide powder: firstly, refined oxalic acid (also called oxalic acid dihydrate, molecular formula is C) with two crystal waters is weighed2H2O4.2(H20) Molecular weight of 126.06, the same below) 12.8kg, putting into a reaction tank to prepare oxalic acid solution with concentration of 0.2mol/L, wherein the reaction tank is a ceramic reaction sandwich tank; adding 0.4kg of polyethylene glycol 20000, stirring for 0.5 hour, dropwise adding 214L of terbium chloride aqueous solution with the concentration of 0.2mol/L, dropwise adding at the speed of 5L/min, stirring for 15min after dropwise adding, standing, adding ice water into an interlayer of a ceramic reaction interlayer tank, circularly aging for 5 hours to obtain a material mixed solution, wherein the material temperature in the reaction kettle is controlled to be 0-5 ℃ through ice water circulation in the aging process. Discharging the material mixed solution into a suction filtration barrel, pumping liquid in the material mixed solution, adding pure water for washing, wherein the temperature of the pure water is higher than 95 ℃, the pure water added in the washing process and the quality of the oxide prepared finallyWashing with water to neutrality in the ratio of 300:1, filtering to obtain precipitate, transferring the precipitate to roller kiln, and burning at 900 deg.C for 3 hr to obtain terbium oxide with yield of 98%, and the granularity of terbium oxide obtained by Marwin 2000 particle sizer detection is D50:2.225 μm. And the non-rare earth impurities such as chloride ions, iron ions, calcium ions and the like meet the standard range, namely the chloride ions are less than 50ppm, the iron ions are less than 5ppm, and the calcium ions are less than 10 ppm.
Example 2
The specific embodiment adopts the following technical scheme to prepare the terbium oxide powder: weighing 24kg of refined oxalic acid with two crystal waters, and putting the refined oxalic acid into a reaction tank to prepare an oxalic acid solution with the concentration of 0.4mol/L, wherein the reaction tank is a ceramic reaction interlayer tank; adding 1.05kg of polyethylene glycol 20000, stirring for 0.5 hour, dropwise adding 200L of terbium chloride solution with the concentration of 0.4mol/L, dropwise adding at the speed of 5L/min, stirring for 15min after dropwise adding, standing, adding ice water into an interlayer of a ceramic reaction interlayer tank, circularly aging for 4 hours to obtain a material mixed solution, and controlling the material temperature in the reaction kettle to be 0-5 ℃ through ice water circulation in the aging process. And discharging the material mixed solution into a suction filtration barrel, pumping liquid in the material mixed solution, adding pure water for washing, wherein the temperature of the pure water is higher than 95 ℃, the mass ratio of the pure water added in the washing process to the finally prepared oxide is 300:1, washing with water to be neutral, filtering to be dry to obtain a precipitate, transferring the precipitate to a roller kiln, and burning at 850 ℃ for 4.5 hours to obtain terbium oxide, wherein the yield is 97.67%, and the granularity of the terbium oxide prepared by a Marwin 2000 particle sizer is D50:2.836 mu m. And the non-rare earth impurities such as chloride ions, iron ions, calcium ions and the like meet the standard range, namely the chloride ions are less than 50ppm, the iron ions are less than 5ppm, and the calcium ions are less than 10 ppm.
Example 3
The specific embodiment adopts the following technical scheme to prepare the terbium oxide powder: weighing 48kg of refined oxalic acid with two crystal waters, and putting the refined oxalic acid into a reaction tank to prepare an oxalic acid solution with the concentration of 0.3mol/L, wherein the reaction tank is a ceramic reaction kettle with a coil pipe arranged inside; adding 1.6kg of polyethylene glycol 1000, stirring for 0.5 hour, dropwise adding 357L of terbium chloride aqueous solution with the concentration of 0.3mol/L, dropwise adding at the speed of 4L/min, stirring for 25min after dropwise adding, standing, adding ice water into a coil pipe of a ceramic reaction kettle, circularly aging for 5 hours to obtain a material mixed solution, and controlling the material temperature in the reaction kettle to be 0-5 ℃ through ice water circulation in the aging process. And discharging the material mixed solution into a suction filtration barrel, pumping liquid in the material mixed solution, adding pure water for washing, wherein the temperature of the pure water is higher than 95 ℃, the mass ratio of the pure water added in the washing process to the finally prepared oxide is 300:1, washing with water to be neutral, filtering to be dry to obtain a precipitate, transferring the precipitate to a roller kiln, burning at 900 ℃ for 3.5 hours to obtain terbium oxide, wherein the yield is 99.12%, and the granularity of the prepared terbium oxide is D50:2.651 mu m through detection of a Malvern 2000 particle sizer. And the non-rare earth impurities such as chloride ions, iron ions, calcium ions and the like meet the standard range, namely the chloride ions are less than 50ppm, the iron ions are less than 5ppm, and the calcium ions are less than 10 ppm.
Example 4
The specific embodiment adopts the following technical scheme to prepare the terbium oxide powder: weighing 16kg of refined oxalic acid with two crystal waters, and putting the refined oxalic acid into a reaction tank to prepare an oxalic acid solution with the concentration of 0.2mol/L, wherein the reaction tank is a ceramic reaction interlayer tank; adding 1.05kg of a mixture of polyethylene glycol 3000 and polyethylene glycol 500 (wherein the mass ratio of the polyethylene glycol 3000 to the polyethylene glycol 500 is 1:1), stirring for 0.5 hour, dropwise adding 200L of terbium chloride solution with the concentration of 0.4mol/L, dropwise adding at the speed of 6L/min, stirring for 10 minutes after dropwise adding, standing, adding ice water into an interlayer of a ceramic reaction interlayer tank, circularly aging for 4 hours to prepare a material mixed solution, and controlling the material temperature in a reaction kettle to be 0-5 ℃ through ice water circulation in the aging process. And discharging the material mixed solution into a suction filtration barrel, pumping liquid in the material mixed solution, adding pure water for washing, wherein the temperature of the pure water is higher than 95 ℃, the mass ratio of the pure water added in the washing process to the finally prepared oxide is 300:1, washing with water to be neutral, filtering to be dry to obtain a precipitate, transferring the precipitate to a roller kiln, and burning at 890 ℃ for 4 hours to obtain terbium oxide, wherein the yield is 97.35%, and the granularity of the prepared terbium oxide is D50:2.278 mu m according to the detection of a Marwin 2000 particle sizer. And the non-rare earth impurities such as chloride ions, iron ions, calcium ions and the like meet the standard range, namely the chloride ions are less than 50ppm, the iron ions are less than 5ppm, and the calcium ions are less than 10 ppm.
Comparative example 1
The specific embodiment adopts the following technical scheme to prepare the terbium oxide powder: weighing 24kg of refined oxalic acid with two crystal waters, and putting the refined oxalic acid into a reaction tank to prepare an oxalic acid solution with the concentration of 0.4mol/L, wherein the reaction tank is a ceramic reaction interlayer tank; adding 1.05kg of polyethylene glycol 20000, stirring for 0.5 hour, dropwise adding 200L of terbium chloride solution with the concentration of 0.4mol/L, dropwise adding at the speed of 5L/min, stirring for 15min after dropwise adding, standing, aging at normal temperature for 4 hours to obtain material mixed solution, discharging the material mixed solution into a suction filtration barrel, draining liquid in the material mixed solution, adding pure water for washing, wherein the temperature of the pure water is higher than 95 ℃, the mass ratio of the pure water added in the washing process to the finally prepared terbium oxide is 300:1, washing with water to neutrality, draining to obtain precipitate, transferring the precipitate to a roller kiln, burning at 900 ℃ for 3 hours to obtain the terbium oxide, wherein the yield is 92%, and the granularity of the prepared terbium oxide detected by a Malvern 2000 particle size analyzer is D50:5.397 mu m. And the non-rare earth impurities such as chloride ions, iron ions, calcium ions and the like meet the standard range, namely the chloride ions are less than 50ppm, the iron ions are less than 5ppm, and the calcium ions are less than 10 ppm.
Comparative example 2
The specific embodiment adopts the following technical scheme to prepare the terbium oxide powder: weighing 24kg of refined oxalic acid with two crystal waters, and putting the refined oxalic acid into a reaction tank to prepare an oxalic acid solution with the concentration of 0.4mol/L, wherein the reaction tank is a ceramic reaction interlayer tank; adding 1.05kg of polyethylene glycol 20000, stirring for 0.5 hour, dropwise adding 200L of terbium chloride solution with the concentration of 0.4mol/L, dropwise adding at the speed of 5L/min, stirring for 15min after dropwise adding, standing, adding ice water into an interlayer of a ceramic reaction interlayer tank, circularly aging for 4 hours to obtain a material mixed solution, and controlling the material temperature in the reaction kettle to be 0-5 ℃ through ice water circulation in the aging process. And discharging the material mixed solution into a suction filtration barrel, draining liquid in the material mixed solution, adding pure water for washing, washing with pure water at normal temperature, washing with pure water at the normal temperature, wherein the mass ratio of the pure water added in the washing process to the finally prepared oxide is 300:1, washing with water to neutrality, filtering to dryness to obtain a precipitate, transferring the precipitate to a roller kiln, and burning at 900 ℃ for 3 hours to obtain terbium oxide, wherein the yield is 94.35%, and the granularity of the prepared terbium oxide is D50:3.637 mu m according to the detection of a Malvern 2000 particle sizer. And the non-rare earth impurities such as chloride ions, iron ions, calcium ions and the like exceed the standard range, namely the chloride ions are more than 50ppm, the iron ions are more than 5ppm, and the calcium ions are more than 10 ppm.
Claims (5)
1. A preparation method of terbium oxide with the particle size of D50:2-3 μm is characterized in that: the method comprises the following steps:
(1) dropwise adding a terbium chloride aqueous solution into the oxalic acid solution in which the polyethylene glycol is uniformly dispersed while stirring, continuously stirring for 10-30min after the dropwise adding is finished, and then standing and aging for 4-5 h to prepare a material mixed solution, wherein the aging temperature is 0-5 ℃, the concentration of the solution of the Chinese herbal acid in the material mixed solution is 0.2-0.4mol/L, and the concentration of the terbium chloride aqueous solution is 0.2-0.4 mol/L;
(2) carrying out suction filtration on the material mixed liquor prepared in the step (1), then washing with water to be neutral, and filtering to be dry to prepare a precipitate, wherein the washing temperature is more than or equal to 95 ℃;
(3) burning the precipitate prepared in the step (2) until the precipitate is decomposed to prepare terbium oxide;
the molar weight ratio of the oxalic acid to the terbium chloride in the step (1) is 1.5-3: 1; the mass amount of the polyethylene glycol in the step (1) is 3.5-5.7% of that of the terbium chloride, and the pH value of the system is controlled to be 6.2-6.8; the dripping speed of the aqueous solution of terbium chloride in the step (1) is 4-6L/h; the burning temperature in the step (3) is 850-900 ℃, and the burning time is 3-5 hours.
2. The method for preparing D50:2-3 μm terbium oxide according to claim 1, wherein the polyethylene glycol is any one or more of polyethylene glycol 20000, polyethylene glycol 2000, polyethylene glycol 1000, polyethylene glycol 3000 and polyethylene glycol 500.
3. The method for preparing D50:2-3 μm terbium oxide according to claim 1, wherein the polyethylene glycol used in step (1) is polyethylene glycol 20000.
4. The method for preparing terbium oxide (D50: 2-3 μm) according to claim 1, wherein the stirring of the aqueous solution of terbium chloride in step (1) is continued for 15min after the end of the dropwise addition.
5. The method for preparing terbium oxide (D50) 2-3 μm according to claim 1, wherein the calcination temperature in step (3) is 900 ℃ and the calcination time is 3 hours.
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