CN109205655B - Preparation method of nano gadolinium oxide with particle size of 80-100nm - Google Patents
Preparation method of nano gadolinium oxide with particle size of 80-100nm Download PDFInfo
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- CN109205655B CN109205655B CN201811404108.1A CN201811404108A CN109205655B CN 109205655 B CN109205655 B CN 109205655B CN 201811404108 A CN201811404108 A CN 201811404108A CN 109205655 B CN109205655 B CN 109205655B
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Abstract
The invention discloses a preparation method of nano gadolinium oxide with the particle size of 80-100nm, which comprises the following steps: firstly, uniformly dripping sodium bicarbonate solution with the concentration of 0.1-0.6 mol/L and the temperature of 0-5 ℃ into gadolinium chloride solution containing polyethylene glycol 10000 and/or polyethylene glycol 20000 at the speed of 3-6L/min, continuously stirring for 0.5-1h after dripping is finished, standing and aging at the temperature of 0-5 ℃ to prepare mother liquor containing precipitates, wherein the temperature of a reaction system is 0-5 ℃ in the process, and the operating environment temperature is maintained at 26-28 ℃. And then carrying out suction filtration and water washing, wherein the suction filtration and water washing mode is that hot pure water with the temperature of more than 95 ℃ is soaked and washed for a plurality of times, a filter cake after the suction filtration and water washing is placed for more than 24h at the temperature of 0-5 ℃, and then the filter cake is burned for 1-2h at the temperature of 800-850 ℃, so that the nano gadolinium oxide with the particle size of 80-100nm is prepared.
Description
Technical Field
The invention belongs to the technical field of nano powder, and particularly relates to a preparation method of nano gadolinium oxide with a particle size of 80-100 nm.
Background
Gadolinium oxide is widely used in the fields of catalysis, ceramics, glass industry, solid oxide fuel cells, luminescent materials, polishing materials, nuclear materials and the like. Gadolinium oxide may also be a major component in solid fuel cells. For the synthesis of nano gadolinium oxide powder, the sol-gel method and the chemical precipitation method are currently used. Synthesis and characterization of conductive polyaniline micro-nano gadolinium oxide composite material, Zulixia et al, proceedings of the faculty of the academy of sciences of the Guangxi province (Nature science edition), 2007, 66-68, a chemical precipitation method is adopted to prepare micro-nano gadolinium oxide flaky powder, but the prepared powder is easy to agglomerate, and the obtained gadolinium oxide has a large size of about 50-800 nm; the nano gadolinium oxide/NBR composite material is prepared by high-temperature calcination in combination of a coprecipitation method and a spray drying method according to the rubber industry 2010, 581-Pioneer and the like, the research on the shielding performance of the nano gadolinium oxide/NBR composite material, and the preparation process is relatively long in time and relatively complex.
With the development of science and technology, manufacturers have higher requirements on the physical properties of gadolinium oxide. Most of the preparation techniques of the rare earth oxide powder disclosed at present adopt ammonium bicarbonate and urea as a precipitator, and sometimes seed crystals or other substances such as ammonium salt and the like are added. Ammonium bicarbonate or ammonium salt can generate a large amount of ammonia nitrogen wastewater, which brings great difficulty to the wastewater reaching the standard; meanwhile, the method of adding the seed crystal firstly obtains better seed crystal, the preparation difficulty of the seed crystal is higher, and the precipitation process is not easy to control.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a more environment-friendly and energy-saving method for preparing nano gadolinium oxide with the particle size of 80-100 nm.
The technical scheme adopted by the invention is as follows: a method for preparing nano gadolinium oxide with the particle size of 80-100nm, which comprises the following steps:
(1) adding a gadolinium chloride solution prepared by pure water and having a concentration of 0.1-0.6 mol/L into a reaction kettle, adding polyethylene glycol 10000 and/or polyethylene glycol 20000 surfactant which is 10-15% of the mass of gadolinium chloride, stirring until the mixture is uniformly dispersed and fully dissolved, and adjusting the temperature of the system to 0-5 ℃.
Then, under the condition of maintaining the temperature of the system at 0-5 ℃, uniformly dropwise adding a sodium bicarbonate precipitator which is prepared by pure water and has the concentration of 0.1-0.6 mol/L and the temperature of 0-5 ℃ into the system at the speed of 3-6L/min; after the dropwise addition of the precipitant is finished, continuously stirring for 0.5-1h, and then standing and aging at the temperature of 0-5 ℃ to obtain mother liquor containing the precipitate. The dropping rate may be increased as appropriate depending on the production magnification, but the stirring rate should be increased at the same time. The above operation is carried out at an ambient temperature of 26-28 deg.C, above which the particles become larger and smaller in specific surface area, and below which the particles become smaller and larger in specific surface area.
(2) Carrying out suction filtration washing on the mother liquor containing the precipitate prepared in the step (1), wherein the suction filtration washing mode is that hot pure water with the temperature of more than 95 ℃ is used for soaking and washing for multiple times in a suction filtration barrel, the soaking time is 15-20min each time, and then the washing is carried out, and the environmental temperature of the suction filtration washing is kept at 26-28 ℃; then the filter cake after the water pumping and washing is placed for more than 24 hours at the temperature of 0-5 ℃, and then is burned for 1-2 hours at the temperature of 800-850 ℃ to prepare the nano gadolinium oxide with the particle size of 80-100 nm.
In order to facilitate the particle size control, the molar ratio of the gadolinium chloride to the sodium bicarbonate in the step (1) is further optimized to be 1:3-1: 3.2.
In order to better control the system temperature, the system temperature in the reaction kettle in the step (1) is further optimized to be controlled by circulating ice water.
In order to achieve more uniform distribution of the particles, it is preferable that the stirring is continued for 0.5h and the aging time is 2h after the dropwise addition of the precipitant in the step (1) is completed.
In order to enhance the burning effect and ensure the particle distribution, it is further preferable that the burning in the step (2) is performed in a car-type rare earth roasting furnace.
The beneficial technical effects obtained by the invention are as follows: 1) preparing 80-100nm nanometer gadolinium oxide with uniform particle size distribution; 2) hot pure water with the temperature of more than 95 ℃ is adopted for soaking and washing for multiple times, so that the defect of large particle fusion in the washing process is effectively avoided on the premise of effectively removing impurities, and the prepared gadolinium oxide particles have good dispersibility; 3) (ii) a The temperature of the environment of the suction filtration and water washing is kept between 26 and 28 ℃, and the particle size is also effectively ensured. 4) After washing, the filter cake is firstly placed for more than 24 hours at the temperature of 0-5 ℃ and then burned, thereby further ensuring the good dispersibility of the particles and ensuring that the particles are not agglomerated and enlarged.
Drawings
FIG. 1 is a scanning electron microscope image of nano-sized gadolinium oxide particles prepared in example 1;
FIG. 2 is a scanning electron micrograph of nano-gadolinium oxide particles prepared in example 2;
FIG. 3 is a scanning electron micrograph of nano-gadolinium oxide particles prepared in example 3;
FIG. 4 is a scanning electron micrograph of nano-gadolinium oxide particles prepared in example 4;
FIG. 5 is a scanning electron micrograph of nano-gadolinium oxide particles prepared in comparative example 1;
FIG. 6 is a scanning electron micrograph of nano-gadolinium oxide particles prepared in comparative example 2;
FIG. 7 is a scanning electron micrograph of nano-gadolinium oxide particles prepared in comparative example 3;
FIG. 8 is a scanning electron micrograph of nano-gadolinium oxide particles prepared in comparative example 4;
FIG. 9 is a scanning electron micrograph of nano-gadolinium oxide particles prepared in comparative example 5.
Detailed Description
The invention is described in more detail below with reference to the following examples:
example 1:
the specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature is controlled to 26 ℃ by an external temperature control device (which may be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute the high-concentration gadolinium chloride solution to prepare a gadolinium chloride solution with the concentration of 0.3mol/L, then putting 91.95L of the gadolinium chloride solution with the concentration of 0.3mol/L into a spacer reaction kettle, and introducing circulating ice water into the spacer to control the temperature of a solution system in the spacer reaction kettle to be 2 ℃. And then weighing 500 g of polyethylene glycol 20000, dissolving the solution into 2L by pure water, adding the solution into the spacer reaction kettle, stirring for 30min, uniformly spraying and dropwise adding a sodium bicarbonate solution with the concentration of 0.3mol/L and the temperature of 2 ℃ into the spacer reaction kettle at the dropwise adding speed of 4L/min, continuing stirring for 30min after dropwise adding is finished, and standing and aging for 2h at the temperature of 2 ℃ to obtain a mother solution containing precipitates. The above operations were all carried out while maintaining the reaction system temperature in the jacket reactor at 2 ℃.
The preparation method of the precipitator comprises the following steps: 6.95kg of sodium bicarbonate was weighed, and 275.85L of purified water was added thereto to prepare a sodium bicarbonate solution having a concentration of 0.3 mol/L.
After the aging is finished, the mother liquor containing the precipitate is filtered, and then is added with hot pure water with the temperature of more than 95 ℃ for soaking, washing and washing. Soaking and washing with 500L of water each time for 15min, washing with 5 times, and maintaining the temperature of the environment for filtering and washing with 2500L of hot pure water at 26-28 deg.C. And after pumping and filtering excessive water, placing the filter cake for 24 hours at the temperature of 0-5 ℃, then placing the filter cake into a cart furnace for burning, wherein the burning temperature is 800 ℃, and the heat preservation time is 1 hour. The obtained nanometer gadolinium oxide has a particle size of 80-100nm and a specific surface area of 8.81m by SEM detection2/g。
Example 2
The specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature was controlled to 28 ℃ by an external temperature control device (which could be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute the high-concentration gadolinium chloride solution to prepare a gadolinium chloride solution with the concentration of 0.2mol/L, then putting 275.86L of the gadolinium chloride solution with the concentration of 0.2mol/L into a spacer reaction kettle, and introducing circulating ice water into the spacer to control the temperature of a solution system in the spacer reaction kettle to be 0 ℃. Then 1500 g of polyethylene glycol 10000 is weighed and dissolved into 6L of solution by pure water, the solution is added into the spacer reaction kettle, after stirring for 30min, the sodium bicarbonate solution with the concentration of 0.2mol/L and the temperature of 0 ℃ is uniformly sprayed and dripped into the spacer reaction kettle, the dripping speed is 6L/min, stirring is continued for 30min after the dripping is finished, and the mother solution containing the precipitate is prepared after standing and aging for 2 h. The above operations were all carried out while maintaining the reaction system temperature in the jacket reactor at 0 ℃.
The preparation method of the precipitator comprises the following steps: 14.83kg of sodium bicarbonate was weighed, and 441.38L of purified water was added thereto to prepare a sodium bicarbonate solution having a concentration of 0.4 mol/L.
After aging, the mother liquor containing the precipitate is filtered, and then is washed by adding hot pure water with the temperature of more than 95 ℃. 500L of water is washed for 10 times each time, 5000L of hot pure water is totally used, and the environmental temperature of the water washing by suction filtration is kept between 26 and 28 ℃. And after pumping and filtering excessive water, placing the filter cake for 24 hours at the temperature of 0-5 ℃, then placing the filter cake into a cart furnace for burning, wherein the burning temperature is 800 ℃, and the heat preservation time is 1 hour. The obtained nanometer gadolinium oxide has a particle size of 80-100nm and a specific surface area of 7.46m by SEM detection2/g。
Example 3
The specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature was controlled to 27 c by an external temperature control device (which could be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute the high-concentration gadolinium chloride solution to prepare a gadolinium chloride solution with the concentration of 0.1mol/L, then putting 441.38L of the gadolinium chloride solution with the concentration of 0.1mol/L into a spacer reaction kettle, and introducing circulating ice water into the spacer to control the temperature of a solution system to be 3 ℃. And then 960 g of polyethylene glycol 10000 is weighed and dissolved into 3.84L of solution by pure water, the solution is added into the spacer reaction kettle, after stirring for 30min, the sodium bicarbonate solution with the concentration of 0.4mol/L and the temperature of 3 ℃ is uniformly sprayed and dripped into the spacer reaction kettle at the dripping speed of 5L/min, after the dripping is finished, the stirring is continued for 30min, and then the solution is kept stand and aged for 2h, so that the mother solution containing the precipitate is prepared. The above operations were all carried out while maintaining the reaction system temperature in the jacket reactor at 3 ℃. The preparation method of the precipitator comprises the following steps: 14.83kg of sodium bicarbonate was weighed, and 342.07L of purified water was added thereto to prepare a sodium bicarbonate solution having a concentration of 0.4 mol/L.
After aging, the mother liquor containing the precipitate is filtered, and then is washed by adding hot pure water with the temperature of more than 95 ℃. 500L of water is washed for each time, 8 times of water washing is carried out, 4000L of hot pure water is totally washed, and the environment temperature of the water washing of suction filtration is kept at 26-28 ℃. And after pumping and filtering excessive water, placing the filter cake for 24 hours at the temperature of 0-5 ℃, then placing the filter cake into a cart furnace for burning, wherein the burning temperature is 800 ℃, and the heat preservation time is 1 hour. The obtained nanometer gadolinium oxide has a particle size of 80-100nm and a specific surface area of 9.86m by SEM detection2/g。
Example 4
The specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature was controlled to 28 ℃ by an external temperature control device (which could be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute and prepare a gadolinium chloride solution with the concentration of 0.6mol/L, then putting 55.17L of the gadolinium chloride solution with the concentration of 0.6mol/L into a spacer reaction kettle, introducing circulating ice water into the spacer to control the temperature of a solution system in the spacer reaction kettle to be 5 ℃, then weighing 780 g of polyethylene glycol 20000, dissolving the solution into 3.12L of the solution by using the pure water, adding the solution into the spacer reaction kettle, stirring for 30min, then uniformly spraying and dropwise adding a sodium bicarbonate solution with the concentration of 0.1mol/L and the temperature of 5 ℃ into the spacer reaction kettle, wherein the dropwise adding speed is 6L/min, continuously stirring for 30min after the dropwise adding is finished, and standing and aging for 2 hours. The system temperature was kept at 5 ℃ above.
Sodium bicarbonate 8.62KG was weighed, 1026.16L of pure water was added, and the mixture was stirred to obtain a sodium bicarbonate solution with a concentration of 0.1 mol/L. After aging, the mother liquor containing the precipitate is filtered, and then is washed by adding hot pure water with the temperature of more than 95 ℃. Washing with 500L of water for 6 times each time, and maintaining the temperature of the environment for suction filtration and washing at 26-28 deg.C for 3000L of hot pure water. Filtering the excessive water, standing the filter cake at 0-5 deg.C for 24 hr, and burning in a cart furnaceBurning at 800 deg.c for 1 hr. The obtained nanometer gadolinium oxide has a particle size of 80-100nm and a specific surface area of 7.86m by SEM detection2/g。
Comparative example 1
The specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature is controlled to 35 ℃ by an external temperature control device (which may be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute and prepare a gadolinium chloride solution with the concentration of 0.3mol/L, then putting 91.95L of the gadolinium chloride solution with the concentration of 0.3mol/L into a spacer reaction kettle, introducing circulating ice water into the spacer to control the temperature of a solution system in the spacer reaction kettle to be 2 ℃, weighing 500 g of polyethylene glycol 20000, dissolving the solution into 2L of the solution by using the pure water, adding the solution into the spacer reaction kettle, stirring for 30min, uniformly spraying and dropwise adding a sodium bicarbonate solution with the concentration of 0.3mol/L and the temperature of 2 ℃ into the spacer reaction kettle at the dropwise adding speed of 4L/min, continuously stirring for 30min after dropwise adding, and then standing and aging for 2h to prepare a mother solution containing precipitates. The above operations were all carried out while maintaining the reaction system temperature in the jacket reactor at 2 ℃. The preparation method of the precipitator comprises the following steps: 6.6.95kg of sodium bicarbonate was weighed, 275.85L of pure water was added thereto, and a sodium bicarbonate solution having a concentration of 0.3mol/L was prepared by stirring. After aging, the mother liquor containing the precipitate is filtered, and then is washed by adding hot pure water with the temperature of more than 95 ℃. Washing with 500L water each time, washing with 5 times, and maintaining the temperature of the environment for suction filtration and washing at 26-28 deg.C for 2500L hot pure water. And after pumping and filtering excessive water, placing the filter cake for 24 hours at the temperature of 0-5 ℃, then placing the filter cake into a cart furnace for burning, wherein the burning temperature is 800 ℃, and the heat preservation time is 1 hour. The obtained nanometer gadolinium oxide has a particle size of above 100nm and a specific surface area of 5.43m2/g。
Comparative example 2
The specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature is controlled to 32 degrees by an external temperature control device (which may be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute and prepare a gadolinium chloride solution with the concentration of 0.3mol/L, then putting 91.95L of the gadolinium chloride solution with the concentration of 0.3mol/L into a spacer reaction kettle, wherein the temperature of a solution system in the spacer is normal temperature, then weighing 500 g of polyethylene glycol 20000, dissolving the solution into 2L of the solution by using the pure water, adding the solution into the spacer reaction kettle, stirring for 30min, then uniformly spraying and dropwise adding a sodium bicarbonate solution with the concentration of 0.3mol/L into the spacer reaction kettle at the dropwise adding speed of 4L/min, continuing stirring for 30min after the dropwise adding is finished, and then standing and aging for 2 hours to obtain a mother solution containing precipitates. The reaction system temperature in the above-mentioned operation spacer reactor is room temperature.
The preparation method of the precipitator comprises the following steps: at room temperature, 6.95kg of sodium bicarbonate was weighed, and 275.85L of purified water was added thereto to prepare a sodium bicarbonate solution having a concentration of 0.3 mol/L. After aging, the mother liquor containing the precipitate is filtered, and then is washed by adding hot pure water with the temperature of more than 95 ℃. Washing with 500L water each time, washing with 5 times, and maintaining the temperature of the environment for suction filtration and washing at 26-28 deg.C for 2500L hot pure water. And after pumping and filtering excessive water, placing the filter cake for 24 hours at the temperature of 0-5 ℃, then placing the filter cake into a cart furnace for burning, wherein the burning temperature is 800 ℃, and the heat preservation time is 1 hour. The obtained nanometer gadolinium oxide has irregular particles with particle size of more than 200nm and specific surface area of 2.94m detected by SEM2/g。
Comparative example 3
The specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature is controlled to 26 ℃ by an external temperature control device (which may be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute the high-concentration gadolinium chloride solution to prepare a gadolinium chloride solution with the concentration of 0.6mol/L, then putting 45.98L of the gadolinium chloride solution with the concentration of 0.6mol/L into a spacer reaction kettle, and introducing circulating ice water into the spacer to control the temperature of a solution system in the spacer reaction kettle to be 2 ℃. And then weighing 500 g of polyethylene glycol 20000, dissolving the solution into 2L by pure water, adding the solution into the spacer reaction kettle, stirring for 30min, uniformly spraying and dropwise adding a sodium bicarbonate solution with the concentration of 0.8mol/L and the temperature of 2 ℃ into the spacer reaction kettle at the dropwise adding speed of 4L/min, continuing stirring for 30min after dropwise adding is finished, and standing and aging for 2h to obtain a mother solution containing precipitates. The above operations were all carried out while maintaining the reaction system temperature in the jacket reactor at 2 ℃.
The preparation method of the precipitator comprises the following steps: 6.95kg of sodium bicarbonate is weighed,103.42L of purified water was added to the solution to prepare a sodium hydrogencarbonate solution having a concentration of 0.8 mol/L. After aging, the mother liquor containing the precipitate is filtered, and then is washed by adding hot pure water with the temperature of more than 95 ℃. Washing with 500L water each time, washing with 5 times, and maintaining the temperature of the environment for suction filtration and washing at 26-28 deg.C for 2500L hot pure water. And after pumping and filtering excessive water, placing the filter cake for 24 hours at the temperature of 0-5 ℃, and then putting the filter cake into a cart furnace for burning, wherein the burning temperature is 800 ℃, and the heat preservation time is 1 hour. The obtained nanometer gadolinium oxide has a particle size of 80-100nm and a specific surface area of 6.58m by SEM detection2/g。
Comparative example 4
The specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature is controlled to 20 ℃ by an external temperature control device (which may be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute the high-concentration gadolinium chloride solution to prepare a gadolinium chloride solution with the concentration of 0.3mol/L, then putting 91.95L of the gadolinium chloride solution with the concentration of 0.3mol/L into a spacer reaction kettle, and introducing circulating ice water into the spacer to control the temperature of a solution system in the spacer reaction kettle to be 0 ℃. And then weighing 500 g of polyethylene glycol 20000 to dissolve into 2L of solution, adding the solution into the spacer reaction kettle, stirring for 30min, uniformly spraying and dropwise adding sodium bicarbonate solution with the concentration of 0.3mol/L and the temperature of 2 ℃ into the spacer reaction kettle at the dropwise adding speed of 4L/min, continuing stirring for 30min after dropwise adding is finished, and then standing and aging for 2h to obtain mother liquor containing precipitates. The above operations were all carried out while maintaining the reaction system temperature in the jacket reactor at 0 ℃.
The preparation method of the precipitator comprises the following steps: 6.95kg of sodium bicarbonate was weighed, and 275.85L of purified water was added thereto to prepare a sodium bicarbonate solution having a concentration of 0.3 mol/L.
After aging, the mother liquor containing the precipitate is filtered, and then is washed by adding hot pure water with the temperature of more than 95 ℃. Washing with 500L water each time, washing with 5 times, and maintaining the temperature of the environment for suction filtration and washing at 26-28 deg.C for 2500L hot pure water. And after pumping and filtering excessive water, placing the filter cake for 24 hours at the temperature of 0-5 ℃, then placing the filter cake into a cart furnace for burning, wherein the burning temperature is 800 ℃, and the heat preservation time is 1 hour. The obtained nanometer gadolinium oxide has particle size of 60-80nm and specific surface area of 11.53m by SEM detection2/g.
Comparative example 5
The specific implementation mode adopts the following technical scheme to prepare the nano gadolinium oxide powder with the particle size of 80-100 nm: the ambient temperature is controlled to 26 ℃ by an external temperature control device (which may be an air conditioner). Taking a high-concentration gadolinium chloride solution, adding pure water to dilute the high-concentration gadolinium chloride solution to prepare a gadolinium chloride solution with the concentration of 0.3mol/L, then putting 91.95L of the gadolinium chloride solution with the concentration of 0.3mol/L into a spacer reaction kettle, and introducing circulating ice water into the spacer to control the temperature of a solution system in the spacer reaction kettle to be 2 ℃. And then weighing 500 g of polyethylene glycol 20000, dissolving the solution into 2L by pure water, adding the solution into the spacer reaction kettle, stirring for 30min, uniformly spraying and dropwise adding a sodium bicarbonate solution with the concentration of 0.3mol/L and the temperature of 2 ℃ into the spacer reaction kettle at the dropwise adding speed of 4L/min, continuing stirring for 30min after dropwise adding is finished, and standing and aging for 2h to obtain a mother solution containing precipitates. The above operations were all carried out while maintaining the reaction system temperature in the jacket reactor at 2 ℃.
The preparation method of the precipitator comprises the following steps: 6.6.95kg of sodium bicarbonate was weighed, 275.85L of pure water was added thereto, and a sodium bicarbonate solution having a concentration of 0.3mol/L was prepared by stirring.
After the aging is finished, the mother liquor containing the precipitate is filtered, and then the mother liquor is added with pure water at normal temperature for washing. Washing with 500L water each time, washing with 5 times, and maintaining the temperature of the environment for suction filtration and washing at 26-28 deg.C for 2500L hot pure water. And after pumping and filtering excessive water, placing the filter cake for 24 hours at the temperature of 0-5 ℃, then placing the filter cake into a cart furnace for burning, wherein the burning temperature is 800 ℃, and the heat preservation time is 1 hour. The obtained nanometer gadolinium oxide has a particle size of above 100nm and a specific surface area of 4.08m by SEM detection2/g。
Claims (5)
1. A method for preparing nano gadolinium oxide with the particle size of 80-100 nm; the method is characterized in that: the method comprises the following steps:
(1) adding a gadolinium chloride solution prepared by pure water and having a concentration of 0.1-0.6 mol/L into a reaction kettle, adding a polyethylene glycol 10000 and/or polyethylene glycol 20000 surfactant which is 10-15% of the mass of gadolinium chloride, stirring until the gadolinium chloride is uniformly dispersed and fully dissolved, and adjusting the temperature of the system to 0-5 ℃;
then, uniformly dropwise adding a sodium bicarbonate precipitator which is prepared by pure water and has the concentration of 0.1-0.6 mol/L and the temperature of 0-5 ℃ into the system at the speed of 3-6L/min under the condition of maintaining the temperature of the system at 0-5 ℃, continuously stirring for 0.5-1h after dropwise adding, and then standing and aging at the temperature of 0-5 ℃ to prepare a mother solution containing precipitates;
the operating environment temperature is maintained at 26-28 ℃;
(2) carrying out suction filtration washing on the mother liquor containing the precipitate prepared in the step (1), wherein the suction filtration washing mode is that hot pure water with the temperature of more than 95 ℃ is used for soaking and washing for multiple times in a suction filtration barrel, the soaking time is 15-20min each time, and then the washing is carried out, and the environmental temperature of the suction filtration washing is kept at 26-28 ℃; then the filter cake after the water pumping and washing is placed for more than 24 hours at the temperature of 0-5 ℃, and then is burned for 1-2 hours at the temperature of 800-850 ℃ to prepare the nano gadolinium oxide with the particle size of 80-100 nm.
2. The method for preparing nano gadolinium oxide with particle size of 80-100nm as claimed in claim 1, wherein: the molar ratio of the gadolinium chloride to the sodium bicarbonate in the step (1) is 1:3-1: 3.2.
3. The method for preparing nano gadolinium oxide with particle size of 80-100nm as claimed in claim 2, wherein: and (2) controlling the system temperature in the reaction kettle in the step (1) by circulating ice water.
4. The method for preparing nano gadolinium oxide with particle size of 80-100nm as claimed in claim 1, wherein: after the dropwise addition of the precipitant in the step (1) is finished, continuously stirring for 0.5h, and aging for 2 h.
5. The method for preparing nano gadolinium oxide with particle size of 80-100nm as claimed in claim 1, wherein: and (3) the firing in the step (2) is carried out in a trolley type rare earth roasting furnace.
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| CN111018527A (en) * | 2019-12-26 | 2020-04-17 | 江西鑫泰功能材料科技有限公司 | Preparation method of nano gadolinium oxide for dielectric ceramic capacitor |
| CN111017976A (en) * | 2019-12-27 | 2020-04-17 | 江西鑫泰功能材料科技有限公司 | Preparation method of nano yttrium oxide for dielectric ceramic capacitor |
| CN111533157A (en) * | 2020-04-24 | 2020-08-14 | 广西科学院 | Microwave calcination preparation method of gadolinium oxide nano powder |
| 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 |
| CN112174188B (en) * | 2020-09-30 | 2023-03-24 | 甘肃稀土新材料股份有限公司 | Method for preparing gadolinium oxide with high apparent density by ammonium bicarbonate precipitation method |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394811A (en) * | 2002-06-17 | 2003-02-05 | 施越群 | Preparation method of nano yttrium oxide |
| KR20040069404A (en) * | 2003-01-29 | 2004-08-06 | 한국화학연구원 | Preparation method of ceria particles with nano-size |
| CN1749169A (en) * | 2004-09-15 | 2006-03-22 | 北京有色金属研究总院 | Low bulk specific weight and large specific surface rare-earth oxide REO and its preparing method |
| CN102358785A (en) * | 2011-07-18 | 2012-02-22 | 包头嘉创科技有限公司 | Method for preparing rare-earth organic material reinforcing agent |
| CN105502467A (en) * | 2014-09-22 | 2016-04-20 | 常州市卓群纳米新材料有限公司 | Nanometer dysprosium oxide preparation method |
| CN106277021A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of large-specific surface area nano Dineodymium trioxide preparation method |
| CN106830047A (en) * | 2015-12-04 | 2017-06-13 | 常州市卓群纳米新材料有限公司 | A kind of nano oxidized holmium preparation method |
| CN108585014A (en) * | 2018-04-25 | 2018-09-28 | 北京化工大学 | A series of micro-/ nano rare earth materials and preparation method thereof |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140151913A1 (en) * | 2012-11-30 | 2014-06-05 | Corning Incorporated | Cost effective y2o3 synthesis and related functional nanocomposites |
-
2018
- 2018-11-23 CN CN201811404108.1A patent/CN109205655B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394811A (en) * | 2002-06-17 | 2003-02-05 | 施越群 | Preparation method of nano yttrium oxide |
| KR20040069404A (en) * | 2003-01-29 | 2004-08-06 | 한국화학연구원 | Preparation method of ceria particles with nano-size |
| CN1749169A (en) * | 2004-09-15 | 2006-03-22 | 北京有色金属研究总院 | Low bulk specific weight and large specific surface rare-earth oxide REO and its preparing method |
| CN102358785A (en) * | 2011-07-18 | 2012-02-22 | 包头嘉创科技有限公司 | Method for preparing rare-earth organic material reinforcing agent |
| CN105502467A (en) * | 2014-09-22 | 2016-04-20 | 常州市卓群纳米新材料有限公司 | Nanometer dysprosium oxide preparation method |
| CN106277021A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of large-specific surface area nano Dineodymium trioxide preparation method |
| CN106830047A (en) * | 2015-12-04 | 2017-06-13 | 常州市卓群纳米新材料有限公司 | A kind of nano oxidized holmium preparation method |
| CN108585014A (en) * | 2018-04-25 | 2018-09-28 | 北京化工大学 | A series of micro-/ nano rare earth materials and preparation method thereof |
| 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 |
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