CN112028105B - Method for preparing nano praseodymium oxide by fused salt coprecipitation method - Google Patents
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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
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention belongs to the technical field of rare earth oxide preparation, and particularly relates to a method for preparing nano praseodymium oxide by a fused salt coprecipitation method. Weighing high-purity praseodymium chloride crystal powder and anhydrous sodium hydroxide particles, and putting the powder and the anhydrous sodium hydroxide particles into a grinder for grinding; putting the ground mixture into an electric furnace for burning and melting; taking absolute ethyl alcohol, and preparing a compound surfactant; cooling the burned melt, putting the cooled melt into a reaction tank, and then putting 300L of pure water into the reaction tank to obtain a melt solution; adding the prepared surfactant into the melt solution, and fully stirring until the mixture is uniform; then putting the reactant into a plate-frame filter press to remove most of free water; sodium ions and other impurities are removed through plate and frame filter pressing washing; placing the washed reactant into a freeze drying box for drying, and removing free water; calcining the dried product, and preserving heat to obtain the nano praseodymium oxide powder. The method of the invention is easier to control the shape and size of the powder particles, and the synthesized powder has specific morphology.
Description
Technical Field
The invention belongs to the technical field of rare earth oxide preparation, and particularly relates to a method for preparing nano praseodymium oxide by a fused salt coprecipitation method.
Background
Praseodymium oxide is a rare earth element with larger dosage, and is mainly applied to the fields of ceramics, glass, rare earth permanent magnet, rare earth cracking catalyst, rare earth polishing powder, grinding material, accelerator, stabilizer and the like. Praseodymium oxide has good conductivity. Is a raw material for producing permanent magnetic alloy of metal praseodymium and samarium praseodymium cobalt, is also a raw material for preparing praseodymium yellow, and is also used as a colorant in glass industry, etc. After praseodymium oxide is added into ceramic pigment and glaze, rare earth praseodymium yellow, praseodymium green, underglaze red pigment and white ghost glaze, elephant yellow glaze, apple green porcelain and the like can be prepared. Pr can also be added into samarium iron nitrogen novel rare earth bonded permanent magnet material (Sm) 2Fe17N9 to improve the performance, which further expands the application of praseodymium. Therefore, with the development of the application of praseodymium in permanent magnetic materials, the dosage and price of praseodymium are continuously increased, and the praseodymium becomes a 'new pet' in rare earth products.
At present, an oxalic acid precipitation method and an ammonium bicarbonate precipitation method are mostly adopted in industry to prepare praseodymium oxide. The oxalate precipitation method has the advantages of good crystal form of the precipitate, easy filtration and the like, but oxalic acid is expensive and can only reach micron-sized. The ammonium bicarbonate precipitation method is unsuitable for mass production, and the chemical precipitation method is easy to form agglomeration because ammonia is contained in the precipitant, if the precipitant is directly discharged, eutrophication of water body can be caused, the water body can be discharged only through sewage treatment, and the cost can be increased through sewage treatment.
Disclosure of Invention
The invention solves the technical problems that the chemical precipitation method is easy to form agglomeration and uneven, and provides a method for preparing nano praseodymium oxide by a molten salt coprecipitation method, and the prepared nano praseodymium oxide product has good dispersibility, uniform particles and high purity.
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) Weighing high-purity praseodymium chloride crystal powder (TREO: 55%) and anhydrous sodium hydroxide particles;
the praseodymium chloride crystal powder and anhydrous sodium hydroxide particles are weighed according to the stoichiometric ratio;
(2) Putting the weighed praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinding machine to grind for 4-6 hours, wherein 5mm zirconium beads are adopted as grinding media;
(3) Burning the ground mixture in an electric furnace at 400-600 deg.c for 1-3 hr;
(4) Weighing fatty alcohol polyoxyethylene ether and preparing a compound surfactant from cellulose sodium sulfate: firstly, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, and then uniformly mixing the fatty alcohol polyoxyethylene ether and the cellulose sodium sulfate to prepare a surfactant;
fatty alcohol polyoxyethylene ether is used as a main material, cellulose sodium sulfate is used as an auxiliary material, the consumption of the fatty alcohol polyoxyethylene ether is 3-4% of the mass of praseodymium oxide, the consumption of the cellulose sodium sulfate is 1-2% of the mass of praseodymium oxide, and the total consumption of the two is 4-6% of the mass of praseodymium oxide.
(5) Cooling the solution obtained by firing in the step (3), then placing the cooled solution into a reaction tank, and then placing 300L of pure water into the reaction tank, and fully stirring the solution to obtain a melt solution;
(6) Adding the surfactant prepared in the step (4) into the melt solution in the step (5), and fully stirring until the surfactant is uniform; then putting the reactant into a plate-frame filter press to remove most of free water;
(7) Carrying out cross flushing washing by deionized water through plate and frame filter pressing to remove sodium ions and other impurities (the washing is carried out by the weight of praseodymium oxide of 1 kg: 500L); placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water; and (3) placing the dried product into a high-temperature electric furnace for calcining at 750-850 ℃, and preserving heat for 3-6 hours to obtain the nano praseodymium oxide powder.
The beneficial effects are that:
the method uses the low-melting-point salt as a reaction medium, the reactants have certain solubility therein, the diffusion rate of ions is greatly accelerated, then the reactants are mixed in an atomic scale in a liquid phase, the reaction is converted from a solid-solid reaction to a solid-liquid reaction, the shape and the size of powder particles can be controlled more easily, and the method has the advantages of simple process, low synthesis temperature, short heat preservation time, uniform chemical components of the synthesized powder, good crystal morphology, high phase purity and the like.
The sodium hydroxide powder in the mixture after grinding is burned and then melted, and reactants react in sodium hydroxide melt to generate a product; and then adding the surfactant can prevent the agglomeration of the rest of particles or the agglomeration of the particles which are not fully reacted in the molten salt method.
Drawings
FIG. 1 is an SEM image of praseodymium oxide nano powder obtained in example 1.
FIG. 2 is an SEM image of praseodymium oxide nano powder obtained in example 4.
FIG. 3 is an SEM image of praseodymium oxide nano powder obtained in example 5.
FIG. 4 is an SEM image of praseodymium oxide nano powder obtained in comparative example 1.
FIG. 5 is an SEM image of praseodymium oxide nano powder obtained in comparative example 2.
FIG. 6 is an SEM image of praseodymium oxide nano powder obtained in comparative example 3.
FIG. 7 is an SEM image of praseodymium oxide nano powder obtained in comparative example 4.
FIG. 8 is an SEM image of praseodymium oxide nano powder obtained in comparative example 5.
FIG. 9 is an SEM image of praseodymium oxide nano powder obtained in comparative example 6.
FIG. 10 is an SEM image of praseodymium oxide nano powder obtained in comparative example 7.
FIG. 11 is an SEM image of praseodymium oxide nano powder obtained in comparative example 8.
Detailed Description
The invention is further described below in connection with examples, but is not limited thereto.
Example 1
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 5 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 400 ℃ for 3 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.6kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.4kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, and uniformly mixing to prepare a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcination at 850 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 1, the praseodymium oxide nano powder obtained in this example has a particle size of 10 to 30nm, is uniformly distributed, and is detected as BET:63.7m 2 /g；
Example 2
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 6 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 500 ℃ for 2 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.8kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.2kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 750 ℃, and preserving heat for 6 hours to obtain the nano praseodymium oxide powder.
The particle size of the praseodymium oxide nanometer powder obtained in the embodiment is 10-30nm, the distribution is uniform, and the BET is detected: 65.5m 2 /g；
Example 3
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 6 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 600 ℃ for 1 hour;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.6kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.2kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcination at 850 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
The particle size of the praseodymium oxide nanometer powder obtained in the embodiment is 10-30nm, the distribution is uniform, and the BET is detected: 56.3m 2 /g；
Example 4
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 400 ℃ for 3 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.8kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.2kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcination at 850 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 2, the praseodymium oxide nanometer powder obtained in this example has a particle size of 10 to 30nm, is uniformly distributed, and is detected as BET:55.7m 2 /g；
Example 5
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 400 ℃ for 3 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.7kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.3kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 3, the praseodymium oxide nanometer powder obtained in this example has a particle size of 10 to 30nm, is uniformly distributed, and is detected as BET:53.7m 2 /g；
Comparative example 1
A preparation method of nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Respectively taking 1kg of absolute ethyl alcohol, 0.7kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.3kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(4) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinding machine; then pouring the surfactant into a grinder, and grinding for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(5) Burning the ground mixture in an electric furnace at 400 ℃ for 3 hours;
(6) Placing the powder obtained in the step (5) into a reaction tank, then placing 300L of pure water, fully stirring until the powder is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 4, the praseodymium oxide nano powder obtained in this example has a particle size of 50 to 200nm, is unevenly distributed, and is detected as BET:16.5m 2 /g；
Comparative example 2
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Respectively taking 1kg of absolute ethyl alcohol, 0.7kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.3kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(5) Placing the powder obtained in the step (3) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(6) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(7) Putting the reactant obtained in the step (6) into plate-and-frame filter pressing to remove most of free water;
(8) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(9) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(10) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 5, the praseodymium oxide nanometer powder obtained in this example has a particle size of 100 to 300nm, is uniformly distributed, and is detected as BET:11.5m 2 /g；
Comparative example 3
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 400 ℃ for 3 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 20000:0.7kg of polyethylene glycol and sodium cellulose sulfate: 0.3kg, respectively adding polyethylene glycol 20000 and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
The praseodymium oxide nano powder obtained in the embodiment is shown in FIG. 6, and is prepared fromAs can be seen from FIG. 6, the particle size of praseodymium oxide nano powder is 50-100 nm, the distribution is not uniform, and the BET is detected: 23.7m 2 /g；
Comparative example 4
A preparation method of nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 400 ℃ for 3 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.7kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.3kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into an oven for drying at 150 ℃ to remove free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 7, the praseodymium oxide nanometer powder obtained in this example has a particle size of 30 to 100nm, is unevenly distributed, and is detected as BET:30.2m 2 /g；
Comparative example 5
A preparation method of nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 1 hour, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 400 ℃ for 3 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.7kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.3kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, uniformly mixing the two, and preparing a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 8, the praseodymium oxide nano powder obtained in this example has a particle size of 100 to 200nm, is uniformly distributed, and is detected as BET:13.7m 2 /g；
Comparative example 6
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 400 ℃ for 3 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol and 1.0kg of fatty alcohol polyoxyethylene ether, adding the fatty alcohol polyoxyethylene ether into the absolute ethyl alcohol, fully stirring, and preparing a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 9, the praseodymium oxide nano powder obtained in this example has a particle size of 100 to 300nm, is uniformly distributed, and is detected as BET:13.5m 2 /g；
Comparative example 7
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 300 ℃ for 2 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.7kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.3kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, and uniformly mixing to prepare a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 10, the praseodymium oxide nano powder obtained in this example has a particle size of 100 to 200nm, is uniformly distributed, and is detected as BET:14.3m 2 /g；
Comparative example 8
A method for preparing nano praseodymium oxide by a molten salt coprecipitation method comprises the following steps:
(1) 36.4kg of high-purity praseodymium chloride crystal powder (TREO: 55%) was weighed;
(2) 9.9kg of anhydrous sodium hydroxide particles are weighed;
(3) Putting praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder to be ground for 4 hours, wherein 5mm zirconium beads are adopted as grinding media;
(4) Burning the ground mixture in an electric furnace at 800 ℃ for 3 hours;
(5) Respectively taking 1kg of absolute ethyl alcohol, 0.6kg of fatty alcohol polyoxyethylene ether and cellulose sodium sulfate: 0.4kg, respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, fully stirring, and uniformly mixing to prepare a surfactant;
(6) Placing the melt obtained in the step (4) into a reaction tank, and then placing 300L of pure water into the reaction tank for fully stirring;
(7) Adding the prepared surfactant into a reaction tank, fully stirring until the surfactant is uniform, and aging for 3 hours;
(8) Putting the reactant obtained in the step (7) into plate-and-frame filter pressing to remove most of free water;
(9) Filtering and washing reactants by deionized water through a plate frame to remove sodium ions and other impurities;
(10) Placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water;
(11) And (3) placing the dried product into a high-temperature electric furnace for calcining at 800 ℃, and preserving heat for 5 hours to obtain the nano praseodymium oxide powder.
As shown in fig. 11, the praseodymium oxide nanometer powder obtained in this example has a particle size of 50 to 100nm, is uniformly distributed, and is detected as BET:26.5m 2 /g；
The examples are preferred embodiments of the present invention, but the present invention is not limited to the above-described embodiments, and any obvious modifications, substitutions or variations that can be made by one skilled in the art without departing from the spirit of the present invention are within the scope of the present invention.
Claims (6)
1. A nano praseodymia is characterized in that the particle diameter of the nano praseodymia is 10-30nm, and the specific surface area is 50-70m 2 /g; the preparation method of the nano praseodymium oxide comprises the following steps:
(1) Weighing high-purity praseodymium chloride crystal powder and anhydrous sodium hydroxide particles;
(2) Putting the weighed praseodymium chloride crystal powder and anhydrous sodium hydroxide particles into a grinder for grinding;
(3) Putting the ground mixture into an electric furnace for burning and melting;
(4) Respectively adding fatty alcohol polyoxyethylene ether and cellulose sodium sulfate into absolute ethyl alcohol, and then fully mixing and uniformly stirring the two to prepare a compound surfactant;
(5) Cooling the melt burnt in the step (3), then placing the cooled melt into a reaction tank, and then placing 300L of pure water into the reaction tank, and fully stirring the mixture to obtain a melt solution;
(6) Adding the surfactant prepared in the step (4) into the melt solution in the step (5), and fully stirring until the surfactant is uniform; then putting the reactant into a plate-frame filter press to remove free water;
(7) Filtering and washing with deionized water through a plate frame to remove sodium ions and other impurities; placing the washed reactant into a freeze drying box at the temperature of minus 40 ℃ for drying, and removing free water; and (3) placing the dried product into a high-temperature electric furnace for calcination, and preserving heat to obtain the nano praseodymium oxide powder.
2. The nano-praseodymia of claim 1, wherein the praseodymia crystal powder of step (1) and anhydrous sodium hydroxide are weighed in stoichiometric proportions.
3. The nano praseodymium oxide according to claim 1, wherein the grinding time in the step (2) is 4 to 6 hours, and the grinding medium is 5mm zirconium beads.
4. The nano praseodymium oxide according to claim 1, wherein the firing temperature in the step (3) is 400-600 ℃ and the temperature is kept for 1-3 hours.
5. The nano praseodymium oxide according to claim 1, wherein the fatty alcohol polyoxyethylene ether in the step (4) is 3% -4% of the praseodymium chloride in mass, the sodium cellulose sulfate is 1% -2% of the praseodymium chloride in mass, and the total amount of the two is 4-6% of the praseodymium chloride in mass.
6. The nano praseodymium oxide according to claim 1, wherein the calcination temperature in the step (7) is 750-850 ℃ and the holding time is 3-6 hours.
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| CN1724380A (en) * | 2005-07-15 | 2006-01-25 | 清华大学 | Process for synthesizing nano cerium oxide crystal material |
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| CN103011241A (en) * | 2012-12-31 | 2013-04-03 | 江西理工大学 | Rare-earth praseodymium lamellar crystal and preparation method for same |
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| CN111099650A (en) * | 2020-01-21 | 2020-05-05 | 江苏理工学院 | CeO2Molten salt method for synthesizing nano spherical particles |
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| CN1724380A (en) * | 2005-07-15 | 2006-01-25 | 清华大学 | Process for synthesizing nano cerium oxide crystal material |
| CN101412529A (en) * | 2008-11-19 | 2009-04-22 | 中国科学院过程工程研究所 | Method for preparing rare-earth oxide or composite rare-earth oxide nano-powder by molten salt synthesis |
| CN103011241A (en) * | 2012-12-31 | 2013-04-03 | 江西理工大学 | Rare-earth praseodymium lamellar crystal and preparation method for same |
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