CN112194168B - Preparation method of rare earth neodymium oxide - Google Patents
Preparation method of rare earth neodymium oxide Download PDFInfo
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- CN112194168B CN112194168B CN202011153594.1A CN202011153594A CN112194168B CN 112194168 B CN112194168 B CN 112194168B CN 202011153594 A CN202011153594 A CN 202011153594A CN 112194168 B CN112194168 B CN 112194168B
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Abstract
The invention belongs to the field of material preparation, and in particular relates to a preparation method of rare earth neodymium oxide. Is convenient for the enlarged production and has high safety coefficient.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a preparation method of rare earth neodymium oxide.
Background
Neodymium oxide is mainly used as a colorant for glass and ceramics, a raw material for ferromagnetic neodymium-iron-boron, a material for heat-shielding coating, an electronic material, a battery material, biopharmaceuticals, electronics industry and the like, and its application shows superior properties. The material can also be used for manufacturing the magnetic bubble material of a computer, so that the magnetic bubble storage has the characteristics of high speed, large capacity, small volume, multiple functions and the like.
At present, most of micron-sized neodymium oxide and irregular shapes are prepared, the usability of the micron-sized neodymium oxide is affected, and the nano particles are prepared by a hydrothermal template method, so that the cost is too high, and a certain danger exists in amplification. And the sodium oxide ions prepared from sodium carbonate and sodium hydroxide are not easy to clean, and the sodium ions are high in common and need post-treatment. With the high-speed development of science and technology, nanoscale high-activity low-impurity materials are more and more favored, and nanoscale neodymium oxide with large surface energy has better application prospect.
Disclosure of Invention
In order to solve the technical problems pointed out in the background art part and achieve the purpose of preparing neodymium oxide with large surface energy, the invention provides a foam method, and the granularity, coercive force and surface energy of the prepared nano neodymium oxide can meet the requirements through the synergistic effect of chemical cyclic precipitation and additives, and the content of sodium ions can be greatly reduced by using sodium carbonate for high-volume production to replace oxalic acid through ordinary water washing. Has wide application prospect. The electromagnetic property of the permanent magnetic material can be improved, and the coercive force of the material is higher.
The invention adopts the following technical scheme to solve the problems:
(1) Firstly, preparing neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding sodium dodecyl benzene sulfonate, OP and ethyl oleate, and uniformly stirring respectively.
The mass ratio of the sodium dodecyl benzene sulfonate to the OP to the ethyl oleate is as follows: 0.5-2.5:1-3:1-3, the total dosage of which is 2-8% of the metered neodymium oxide mass.
(2) Sodium carbonate solution with concentration of 0.4mol/L is prepared.
(3) Placing the sodium carbonate solution in condensed water to enable the temperature to be lower than 10 ℃, rapidly stirring and dripping the solution obtained in the step (1) to enable the PH value to be 5.8-5.9, and obtaining a mixed solution;
the dropping speed is 6-8L/min, and the molar ratio of sodium carbonate to neodymium chloride is 1.6:1.
(4) Pouring the mixed solution obtained in the step (3) into a closed container, adding a thickening agent, placing the mixed solution into condensed water, introducing ammonia gas or ammonia water for internal circulation (namely, pumping gas from the upper layer of the closed container, and pressing gas from the bottom for circulation and foaming), so that the foam of the solution is rich and uniform, and after internal circulation for 2-3 hours, settling for 1 hour, cleaning and suction filtration.
Wherein, every 100g of neodymium chloride needs to use 40ml-80ml of ammonia water with the mass concentration of 25-28 percent (or the ammonia gas with the same proportion is introduced); the thickener is PVA and the dosage is that the measured solution viscosity is more than 300 mPas; the water temperature of the suction filtration is 70-85 ℃.
In the internal circulation process, the circulation air inlet is provided with 400 meshes of screens, the circulation air flow is as slow as possible, the circulation air flow is as good as possible according to the actual container size, and the excessive speed can lead to oversized foam and early foam rupture.
(5) After sinking, taking out the suspended material attached to the glass wall and forming honeycomb, pumping, filtering and washing, and placing the material into a cart furnace for thermal insulation and burning.
The temperature of the thermal insulation firing is 800-850 ℃, and the thermal insulation firing time is 2-3 hours.
The beneficial effects are that:
(1) After the sodium dodecyl benzene sulfonate and the ethyl oleate are added in the early stage and saponified, the foam is stabilized and enriched, after ammonia is introduced in the later stage, the ethyl oleate can form oleamide, the oleamide acts with neodymium carbonate, the surface charge is stabilized, the fluidity is better, and the oleamide is burnt out in the later stage, so that the larger coercivity is obtained. The particles mixed between the bubble walls are relatively stable before dehydration, and are not easy to agglomerate. The OP can not only be used as a dispersing agent, but also can increase the tension of water, and can prevent the foam from being broken before the particles of the space framework formed by the bubbles are not stabilized.
(2) The solution viscosity of the PVA is more than 300 mPa.s, more regular small bubbles can be generated, and the bubbles can be stabilized and are not easy to break.
(3) The ammonia gas and water are combined to promote the reaction of neodymium carbonate, and the space hollow structure formed by foaming, stacking, dewatering and air drying is utilized, so that neodymium carbonate is not immersed in the solution, and the ammonia gas acts on the surface of the neodymium carbonate, so that sodium ions are easy to clean, the surface is uneven, and the internal energy is larger.
(4) In the internal circulation process, a small-mesh screen is needed for the circulation air inlet to manufacture a large number of small bubbles, the smaller the circulation air flow is, the better the circulation air flow is, a large number of neodymium carbonate precipitates can be used to be attached to the gaps of the small bubbles, and the neodymium carbonate precipitates are exposed in ammonia.
Drawings
FIG. 1 is a schematic view of a closed container used in the present invention;
FIG. 2 is a TEM photograph of nano neodymium oxide obtained in example 1 of the present invention;
FIG. 3 is a TEM photograph of nano neodymium oxide obtained in example 2 of the present invention;
FIG. 4 is a TEM photograph of nano neodymium oxide obtained in example 3 of the present invention;
FIG. 5 is a TEM photograph of nano neodymium oxide obtained in comparative example 1 of the present invention;
FIG. 6 is a TEM photograph of nano neodymium oxide obtained in comparative example 2 of the present invention;
FIG. 7 is a TEM photograph of nano neodymium oxide obtained in comparative example 3 of the present invention;
fig. 8 is a TEM photograph of nano neodymium oxide obtained in comparative example 4 of the present invention.
Detailed Description
The invention is further described below in connection with examples, but is not limited thereto.
Example 1
(1) Firstly, preparing a rare earth neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding 2% of sodium dodecyl benzene sulfonate, 3% of OP and 3% of ethyl oleate by mass of metered neodymium oxide, and uniformly stirring respectively;
(2) Sodium carbonate solution with concentration of 0.4mol/L is prepared.
(3) And (3) placing the sodium carbonate solution in condensed water to enable the temperature to be lower than 10 ℃, rapidly stirring and dripping the solution in the step (1) at the dripping speed of 7L/min, and reacting to obtain the mixed solution with the pH value of 5.81.
(4) Adding a thickener PVA into the mixed solution to enable the viscosity to be 390 mPas, rapidly pouring the solution into a closed container, placing the closed container into condensed water, rapidly introducing ammonia water for internal circulation to enable the foam of the solution to be rich and uniform, and after internal circulation for 2 hours, precipitating for 1 hour, cleaning and suction filtering.
The ammonia water is 80ml for every 100g neodymium chloride, and the water temperature of suction filtration is 75 ℃.
In the internal circulation process, the mesh screen used by the circulation air inlet is 400 meshes, and the degree of the rotating shaft of the peristaltic pump used in the internal circulation is 100 revolutions per minute.
(5) After sinking, taking out the suspended material attached to the glass wall and forming honeycomb, pumping, filtering and washing, and placing the material into a cart furnace for thermal insulation firing at 800 ℃ for 3 hours.
Specific results BET results were 42.3m 2 And/g, the grain diameter is 15-30 nanometers, and the sodium ion content is 96ppm.
Example 2
(1) Firstly, preparing a rare earth neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding sodium dodecyl benzene sulfonate with the mass of 1% of metered neodymium oxide, OP with the mass of 2.5% and ethyl oleate with the mass of 1.5% into the solution, and uniformly stirring the mixture respectively;
otherwise, the same as in example 1 was conducted.
Specific results BET results were found to be 39.2m 2 And/g, particle size of 15-30nm and sodium ion content of 135ppm.
Example 3
(1) Firstly, preparing rare earth neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding sodium dodecyl benzene sulfonate with the metered mass of 0.5% of neodymium oxide, OP with the metered mass of 1% and ethyl oleate with the metered mass of 1% of neodymium oxide, and uniformly stirring respectively;
otherwise, the same as in example 1 was conducted.
Specific results BET results were found to be 40.1m 2 And/g, the grain diameter is 15-30 nanometers, and the sodium ion content is 186ppm.
Example 4
In the step (4), 40ml of ammonia was used per 100g of neodymium chloride, and the same procedure as in example 1 was followed.
Specific results BET results were found to be 40.2m 2 And/g, particle size of 15-30nm and sodium ion content of 202ppm.
Example 5
In the step (4), 60ml of aqueous ammonia was used per 100g of neodymium chloride, and the same procedure as in example 1 was repeated.
Specific results BET results were found to be 41.8m 2 And/g, the grain diameter is 15-30 nanometers, and the sodium ion content is 167ppm.
Example 6
In the step (4), ammonia gas was introduced in the same ratio as in example 1.
Specific results BET results were found to be 38.9m 2 And/g, the grain diameter is 15-30 nanometers, and the sodium ion content is 215ppm.
Example 7
The firing time in step (5) was 2 hours, otherwise the same as in example 1.
Specific results BET results were found to be 43.2m 2 And/g, particle size of 20-30 nm and sodium ion content of 143ppm.
Example 8
(1) Firstly, preparing a rare earth neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding 2% of sodium dodecyl benzene sulfonate, 3% of OP and 3% of ethyl oleate by mass of metered neodymium oxide, and uniformly stirring respectively;
(2) Sodium carbonate solution with concentration of 0.4mol/L is prepared.
(3) And (3) placing the sodium carbonate solution in condensed water to enable the temperature to be lower than 10 ℃, rapidly stirring and dripping the solution in the step (1) at the dripping speed of 8L/min, and reacting to obtain the mixed solution with the pH value of 5.81.
(4) Adding a thickener PVA into the mixed solution to enable the viscosity to be 390 mPas, rapidly pouring the solution into a closed container, placing the closed container into condensed water, rapidly introducing ammonia water for internal circulation to enable the foam of the solution to be rich and uniform, and after internal circulation for 2 hours, precipitating for 1 hour, cleaning and suction filtering.
The ammonia water is 80ml for every 100g neodymium chloride, and the water temperature is 80 ℃ after suction filtration.
(5) After sinking, taking out the suspended material attached to the glass wall and forming honeycomb, pumping, filtering and washing, and placing the material into a trolley furnace for heat preservation and burning at 850 ℃ for 2 hours.
Specific results BET results were found to be 43.2m 2 And/g, particle size of 20-30 nm and sodium ion content of 143ppm.
Comparative example 1
Preparing a neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding 2% sodium dodecyl benzene sulfonate, 3% OP and 3% ethyl oleate of metered mass of neodymium oxide, and uniformly stirring respectively. Sodium carbonate solution with concentration of 0.4mol/L is prepared. The sodium carbonate solution is placed in condensed water to enable the temperature to be lower than 10 ℃, the mixed solution is obtained after rapid stirring and reaction with the PH value of 5.81 at the dropping speed of 7L/min, then the mixed solution is poured into a closed container to be placed in the condensed water, 80ml of ammonia water is added, and air bubbles are circulated for 2h. In the process, bubbles are broken faster, are uneven and are not formed, and cannot form a hollowed-out shape after being finally settled, so that the bubbles exist in a mixed liquid form. After 1H of sedimentation, the water temperature is filtered by suction and 75 ℃, and then the heat preservation and burning are carried out at 800 ℃ for 2 hours.
BET 2.2m was finally measured 2 Per gram, particle size 60-80nm, na ion content 2350ppm.
Comparative example 2
Preparing a neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding 2% sodium dodecyl benzene sulfonate, 3% OP and 3% ethyl oleate of metered mass of neodymium oxide, and uniformly stirring respectively. Sodium carbonate solution with concentration of 0.4mol/L is prepared. And (3) placing the sodium carbonate solution in condensed water to enable the temperature to be lower than 10 ℃, rapidly stirring and reacting at the dropping speed of 7L/min to obtain a mixed solution with the pH value of 5.81, adding a thickening agent PVA into the mixed solution to enable the viscosity to be 390 mPa.s, rapidly pouring the solution into a closed container, placing the closed container in the condensed water, directly pumping out gas from the upper layer of the closed container, pressing the gas from a bottom filter screen for circulating foaming, ensuring that the foam of the solution is rich and uniform, settling for 1 hour after internal circulation for 2 hours, and cleaning and suction filtering at 75 ℃. Foam molding was rapid and the foam was more stable relative to example 1.
Taking out, pumping, filtering and washing the suspended material adhered to the glass wall, and burning at 800 deg.c for 3 hr.
BET 17.2m was finally measured 2 And/g. Particle size 40-60nm, sodium ion content 1640ppm.
Comparative example 3
Preparing a neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding 5% of sodium dodecyl benzene sulfonate with the mass of metered neodymium oxide, and uniformly stirring 3% OP respectively. Sodium carbonate solution with concentration of 0.4mol/L is prepared. And (3) placing the sodium carbonate solution in condensed water to enable the temperature to be lower than 10 ℃, rapidly stirring and reacting at the dropping speed of 7L/min to obtain a mixed solution with the pH value of 5.81, adding a thickening agent PVA into the mixed solution to enable the viscosity to be 390 mPa.s, rapidly pouring the solution into a closed container, placing the closed container in the condensed water, adding 80ml of ammonia water, directly pumping gas from the upper layer of the closed container, pressing the gas into a filter screen at the bottom for circulation foaming, and carrying out sedimentation for 1 hour after internal circulation for 2 hours, and washing and suction filtering at the temperature of 75 ℃. Placing the mixture into a trolley furnace for thermal insulation firing at 800 ℃ for 3 hours.
BET 3.4m was finally measured 2 And/g, random small particles, sodium ion content 1640ppm.
Comparative example 4
Preparing a neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding 5% sodium dodecyl benzene sulfonate and 3% ethyl oleate by mass of metered neodymium oxide, and uniformly stirring respectively. Sodium carbonate solution with concentration of 0.4mol/L is prepared. And (3) placing the sodium carbonate solution in condensed water to enable the temperature to be lower than 10 ℃, rapidly stirring and reacting at the dropping speed of 7L/min to obtain a mixed solution with the pH value of 5.81, adding a thickening agent PVA into the mixed solution to enable the viscosity to be 390 mPa.s, rapidly pouring the solution into a closed container, placing the closed container in the condensed water, adding 80ml of ammonia water, directly pumping gas from the upper layer of the closed container, pressing the gas into a filter screen at the bottom for circulation foaming, and carrying out sedimentation for 1 hour after internal circulation for 2 hours, and washing and suction filtering at the temperature of 75 ℃. Placing the mixture into a trolley furnace for thermal insulation firing at 800 ℃ for 3 hours.
BET 1.5m was finally measured 2 And/g, random particles, sodium ion content 3380ppm.
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. The preparation method of the rare earth neodymium oxide is characterized by comprising the following steps:
(1) Preparing rare earth neodymium chloride solution with the concentration of 0.4mol/L, sequentially adding sodium dodecyl benzene sulfonate, OP and ethyl oleate, and uniformly stirring respectively;
(2) Preparing sodium carbonate solution with the concentration of 0.4 mol/L;
(3) Placing the sodium carbonate solution in condensed water to enable the temperature to be lower than 10 ℃, rapidly stirring and dripping the solution obtained in the step (1) to enable the PH value to be 5.8-5.9, and obtaining a mixed solution;
(4) Quickly adding a thickening agent into the mixed solution in the step (3), pouring the mixed solution into a closed container, placing the closed container into condensed water, quickly introducing ammonia gas or ammonia water for internal circulation, and washing and filtering after the internal circulation is carried out for 2-3 hours and the sedimentation is carried out for 1 hour;
(5) And (5) putting the taken filter cake into a cart furnace for thermal insulation burning after loading the filter cake into a pot.
2. The method for preparing rare earth neodymium oxide according to claim 1, wherein the mass ratio of sodium dodecyl benzene sulfonate, OP and ethyl oleate in the step (1) is: 0.5-2.5:1-3:1-3, the total dosage of which is 2-8% of the metered neodymium oxide mass.
3. The method for preparing rare earth neodymium oxide according to claim 1, wherein the dropping speed in the step (3) is 6-8L/min; the molar ratio of sodium carbonate to neodymium chloride is 1.6:1.
4. the method for producing rare earth neodymium oxide according to claim 1, wherein 40ml to 80ml of ammonia water is used per 100g of neodymium chloride in the step (4); the thickener is PVA and the dosage is that the measured solution viscosity is more than 300 mPas; the water temperature of the suction filtration is 70-85 ℃.
5. The method for preparing rare earth neodymium oxide according to claim 1, wherein the firing temperature in the step (5) is 800-850 ℃, and the heat preservation time is 2-3 hours.
6. A rare earth neodymium oxide prepared by the method according to any one of claims 1 to 5, wherein the specific surface area of the prepared rare earth neodymium oxide is 30 to 45m 2 And/g, particle size of 15-30nm and sodium ion content of 100-220ppm.
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