CN111592028A - Microwave calcination preparation method of rare earth oxide superfine powder - Google Patents
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Abstract
The invention discloses a microwave calcination preparation method of rare earth oxide ultrafine powder, which comprises the following steps of (1) surface treatment: adjusting the rare earth chloride solution with the concentration of 0.5-2.0mol/L to be alkaline, adding a surface additive into the rare earth chloride solution, and uniformly mixing to obtain a first solution; under the condition of stirring, dropwise adding an ammonium bicarbonate solution into the first solution to obtain a second solution; (2) and (3) peroxide treatment: adding a stabilizer into a hydrogen peroxide solution with the concentration of 35-70%, then adding into a second solution, aging for 4-10 hours, filtering and washing to obtain a rare earth carbonate peroxide precipitate; (3) microwave calcination: and (3) placing the peroxycarbonic acid precipitate into a microwave reactor for microwave heating and calcining to obtain the corresponding rare earth oxide superfine powder. The invention prepares the rare earth oxide superfine powder with uniform granularity and more uniform size by preparing the peroxide precipitation of the rare earth and then heating and calcining the rare earth by microwave.
Description
Technical Field
The invention belongs to the field of rare earth, and particularly relates to a microwave calcination preparation method of rare earth oxide ultrafine powder.
Background
The lanthanum oxide is mainly used for manufacturing special alloy precision optical glass and high-refraction optical fiber boards, and is suitable for being used as a camera, a microscope lens, an advanced optical instrument prism and the like. Also used for manufacturing ceramic capacitors, piezoelectric ceramic doping agents, X-ray luminescent material lanthanum oxybromide powder and the like. Extracted from the bastnasite or obtained by burning lanthanum carbonate or lanthanum nitrate. The methods for preparing the ultrafine rare earth oxide include a precipitation method, a sol-gel method, a hydrothermal method, a microemulsion method, a spray thermal decomposition method and the like, wherein the precipitation method is the most commonly adopted research and production method. The method has the advantages of low cost of raw materials, low requirement on equipment, simple process, simple operation, accurate control of chemical composition, easy preparation of ultrafine powder with multiple uniform components, easy control of particle shape and particle size, etc. However, the precipitation method has the problem that agglomeration occurs due to uneven heating inside and outside the particles during heating and calcining, which affects the quality of the product.
Erbium oxide is mainly used as an yttrium iron garnet additive and a nuclear reactor control material, and is also used for manufacturing special luminescent glass and infrared absorbing glass, and is also used as a glass colorant. Due to the photoelectric property of the erbium oxide, the erbium oxide has higher application value in the fields of photonics, optics and communication science; the large-particle erbium oxide is applied to coating materials, has excellent corrosion resistance and is expected to become an excellent anti-corrosion coating; the high-refractivity and high-transparency coating is used as a reflective coating for devices such as solar cells and the like; the erbium oxide coating is used for a fusion reactor cladding hydrogen-resistant coating, and the erbium oxide hydrogen-resistant coating material is usually applied to a thermonuclear experimental reactor and has the function of preventing tritium permeation, activated martensitic steel or austenitic steel is used as a matrix, Fe-Er is used as a metal transition layer on the matrix, and the erbium oxide coating is coated on the matrix. Another application hotspot of erbium is lasers, especially as medical laser materials. Erbium laser is a solid pulse laser with wavelength of 2940nm, which can be strongly absorbed by water molecules in human tissue, thus obtaining a greater effect with less energy and cutting, grinding and excising soft tissue very precisely. Erbium YAG lasers have also been used for cataract extraction. Because the main component of the cataract crystal is water, the erbium laser has low energy and is easy to be absorbed by water, and the cataract crystal is a promising surgical method for removing the cataract. Erbium laser therapeutic instruments are opening up wider and wider application fields for laser surgery.
At present, the method for preparing lanthanum oxide or erbium oxide usually adopts a high-temperature solid phase method and a precipitation method, the prepared lanthanum oxide or erbium oxide is mostly in a micron-scale, and the lanthanum oxide or erbium oxide of superfine powder (nano-scale) needs to be processed again by a ball milling method and the like. In addition, in the process of calcining the prepared precipitate by adopting a high-temperature solid phase method, agglomeration phenomenon can be generated due to uneven internal and external heating, so that the quality of the prepared product is poor.
Disclosure of Invention
The invention aims to provide a method for preparing rare earth oxide superfine powder with uniform granularity and small particle size by microwave heating and calcining a hyperoxia precipitate.
The purpose of the invention is realized by the following technical scheme:
a microwave calcination preparation method of rare earth oxide superfine powder comprises the following steps,
(1) surface treatment: adjusting the rare earth chloride solution with the concentration of 0.5-2.0mol/L to be alkaline, adding a surface additive into the rare earth chloride solution, and uniformly mixing to obtain a first solution; under the condition of stirring, dropwise adding an ammonium bicarbonate solution into the first solution to obtain a second solution;
(2) and (3) peroxide treatment: adding a stabilizer into a hydrogen peroxide solution with the concentration of 35-70%, then adding into a second solution until the solution becomes neutral, aging for 4-10 hours, filtering and washing to obtain a rare earth carbonate peroxide precipitate;
(3) microwave calcination: and placing the peroxycarbonate rare earth precipitate into a microwave reactor for microwave heating and calcining to obtain the rare earth oxide superfine powder.
Preferably, in the step (1), the surface auxiliary agent is one of polyvinylpyrrolidone, stearic acid, oleic acid, sodium dodecyl sulfate, polyethylene glycol and polyacrylate; the addition amount of the surface auxiliary agent is 5-10% of the molar mass of the rare earth chloride.
Preferably, the rare earth chloride is lanthanum chloride or erbium chloride.
Preferably, the adding amount of the ammonium bicarbonate in the step (1) is 1.0 to 3.0 times of the molar mass of the rare earth chloride solution.
Preferably, in the step (2), the stabilizer is acrylic acid or polyacrylamide.
Preferably, the adding amount of the stabilizer is 3-10% of the volume ratio of the hydrogen peroxide solution.
Preferably, in the step (3), the frequency of the microwave heating calcination is 915 +/-50 MHz or 2450 +/-50 MHz, the power of the microwave is 1-10kw, and the microwave output mode comprises two modes of continuous waves and pulse waves or two combinations thereof.
Preferably, the microwave heating calcination time in the step (3) is 1 to 3 hours.
Preferably, the temperature for microwave heating calcination is 800-.
The invention has the following beneficial effects:
1. the invention prepares rare earth oxide (lanthanum oxide or erbium oxide) superfine powder with uniform granularity and more uniform size by firstly preparing peroxide precipitation of lanthanum (or erbium) and then performing microwave heating calcination.
2. The invention adds the stabilizing agent into the hydrogen peroxide, because the hydrogen peroxide is stabilized under the acidic condition, the peroxy precipitate of lanthanum (or erbium) is carried out under the alkaline condition, and the stabilizing agent is chelated with the hydrogen peroxide to ensure that the hydrogen peroxide can still keep stable under the alkaline condition so as to facilitate the generation of the peroxide.
3. Because lanthanum carbonate peroxide (or erbium carbonate peroxide) has high oxidability, in the traditional high-temperature calcination process, the lanthanum oxide (or erbium oxide) obtained by preparation is agglomerated and has uneven granularity due to violent reaction caused by uneven internal and external heating, and the granularity of the lanthanum oxide (or erbium oxide) obtained by preparation is larger and is mostly micron-sized; the invention adopts a microwave heating method, so that the lanthanum oxide (or erbium oxide) is heated uniformly inside and outside in the heating and calcining process, and the agglomeration phenomenon caused by too fast temperature rise or nonuniform heating is avoided.
4. The surface auxiliary agent is added in the invention, so that not only can the surface energy of the particles be reduced and the particles can be prevented from growing, but also the reaction intensity of the peroxide in the calcining process can be reduced, the product agglomeration is avoided, and the quality of the prepared product is better.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the following will clearly and completely describe the technical solutions in the present application with reference to the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and all other embodiments obtained by a person of ordinary skill in the art without making creative efforts based on the embodiments in the present application shall fall within the protection scope of the present application.
Example 1
A microwave calcination preparation method of lanthanum oxide superfine powder comprises the following steps,
(1) surface treatment: regulating a lanthanum chloride solution with the concentration of 0.5mol/L to be alkaline, adding polyvinylpyrrolidone with the molar mass of 5% of lanthanum chloride, and uniformly mixing to obtain a first solution; dropwise adding an ammonium bicarbonate solution with the molar mass of 1.0 time of that of the lanthanum chloride solution into the first solution under the stirring condition to obtain a second solution;
(2) and (3) peroxide treatment: adding 3 volume percent of acrylic acid into 35 volume percent hydrogen peroxide solution, then adding into the second solution until the solution becomes neutral, aging for 4 hours, filtering and washing to obtain a lanthanum carbonate peroxide precipitate;
(3) microwave calcination: placing the lanthanum carbonate peroxide precipitate into a microwave reactor, and calcining for 1 hour at 800 ℃ by microwave heating to obtain lanthanum oxide superfine powder; the frequency of the microwave is 915 +/-50 MHz, the power is 1kw, and the microwave output mode is a continuous wave mode.
Example 2
A microwave calcination preparation method of erbium oxide superfine powder comprises the following steps,
(1) surface treatment: adjusting the erbium chloride solution with the concentration of 2.0mol/L to be alkaline, adding stearic acid with the molar mass of 10% of erbium chloride into the erbium chloride solution, and uniformly mixing to obtain a first solution; dropwise adding an ammonium bicarbonate solution which is 3.0 times of the molar mass of the erbium chloride solution into the first solution under the stirring condition to obtain a second solution;
(2) and (3) peroxide treatment: adding 10 volume percent of polyacrylamide into a hydrogen peroxide solution with the concentration of 70 percent, then adding into a second solution until the solution becomes neutral, aging for 10 hours, filtering and washing to obtain erbium carbonate peroxide precipitate;
(3) microwave calcination: placing the erbium carbonate peroxide precipitate into a microwave reactor, and calcining for 3 hours at 1200 ℃ by microwave heating to obtain erbium oxide superfine powder; the frequency of the microwave is 2450 +/-50 MHz, the power is 10kw, and the microwave output mode is pulse wave.
Example 3
A microwave calcination preparation method of lanthanum oxide superfine powder comprises the following steps,
(1) surface treatment: adjusting a lanthanum chloride solution with the concentration of 0.8mol/L to be alkaline, adding oleic acid with the molar mass of 6% of lanthanum chloride, and uniformly mixing to obtain a first solution; dropwise adding an ammonium bicarbonate solution which is 1.5 times of the molar mass of the lanthanum chloride solution into the first solution under the stirring condition to obtain a second solution;
(2) and (3) peroxide treatment: adding 3 volume percent of acrylic acid into 40 volume percent hydrogen peroxide solution, then adding into the second solution until the solution becomes neutral, aging for 6 hours, filtering and washing to obtain a lanthanum carbonate peroxide precipitate;
(3) microwave calcination: placing the lanthanum carbonate peroxide precipitate into a microwave reactor, and calcining for 1.2 hours at 900 ℃ by microwave heating to obtain lanthanum oxide superfine powder; the frequency of the microwave is 915 +/-50 MHz, the power is 3kw, and the microwave output mode is a combination mode of continuous wave and pulse wave.
Example 4
A microwave calcination preparation method of lanthanum oxide superfine powder comprises the following steps,
(1) surface treatment: regulating a lanthanum chloride solution with the concentration of 1.0mol/L to be alkaline, adding sodium dodecyl sulfate with the molar mass of 7% of lanthanum chloride into the lanthanum chloride solution, and uniformly mixing to obtain a first solution; dropwise adding an ammonium bicarbonate solution which is 2.0 times of the molar mass of the lanthanum chloride solution into the first solution under the stirring condition to obtain a second solution;
(2) and (3) peroxide treatment: adding 5 volume percent of polyacrylamide into a hydrogen peroxide solution with the concentration of 50 percent, then adding the solution into a second solution until the solution becomes neutral, aging for 7 hours, filtering and washing to obtain a lanthanum carbonate peroxide precipitate;
(3) microwave calcination: placing the lanthanum carbonate peroxide precipitate into a microwave reactor, and calcining for 2 hours at the temperature of 1000 ℃ by microwave heating to obtain lanthanum oxide superfine powder; the frequency of the microwave is 2450 +/-50 MHz, the power is 5kw, and the microwave output mode is a combination mode of continuous wave and pulse wave.
Example 5
A microwave calcination preparation method of erbium oxide superfine powder comprises the following steps,
(1) surface treatment: adjusting the erbium chloride solution with the concentration of 1.2mol/L to be alkaline, adding polyethylene glycol with the molar mass of 8% of erbium chloride into the erbium chloride solution, and uniformly mixing to obtain a first solution; under the condition of stirring, dropwise adding an ammonium bicarbonate solution with the molar mass being 2.4 times that of the erbium chloride solution into the first solution to obtain a second solution;
(2) and (3) peroxide treatment: adding 7 volume percent of acrylic acid into a 60 volume percent hydrogen peroxide solution, then adding into a second solution until the solution becomes neutral, aging for 8 hours, filtering and washing to obtain erbium carbonate peroxide precipitate;
(3) microwave calcination: placing the erbium carbonate peroxide precipitate into a microwave reactor, and carrying out microwave heating calcination for 2.5 hours at the temperature of 800-; the frequency of the microwave is 2450 +/-50 MHz, the power is 5kw, and the microwave output mode is a combination mode of continuous wave and pulse wave.
Example 6
A microwave calcination preparation method of erbium oxide superfine powder comprises the following steps,
(1) surface treatment: adjusting the erbium chloride solution with the concentration of 1.6mol/L to be alkaline, adding polyacrylate with the molar mass of erbium chloride of 9% into the erbium chloride solution, and uniformly mixing to obtain a first solution; under the condition of stirring, dropwise adding an ammonium bicarbonate solution with the molar mass being 2.8 times that of the erbium chloride solution into the first solution to obtain a second solution;
(2) and (3) peroxide treatment: adding 9 volume percent of polyacrylamide into 55 volume percent hydrogen peroxide solution, then adding into the second solution until the solution becomes neutral, aging for 9 hours, filtering and washing to obtain erbium carbonate peroxide precipitate;
(3) microwave calcination: placing the erbium carbonate peroxide precipitate into a microwave reactor, and carrying out microwave heating calcination for 2.7 hours at the temperature of 1100 ℃ to obtain erbium oxide superfine powder; the frequency of the microwave is 915 +/-50 MHz, the power is 7kw, and the microwave output mode is a combination mode of continuous wave and pulse wave.
While embodiments of the invention have been disclosed above, it is not intended to be limited to the uses set forth in the specification and examples. It can be applied to all kinds of fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art. The invention is therefore not to be limited to the specific details described herein, without departing from the general concept as defined by the appended claims and their equivalents.
Claims (9)
1. A microwave calcination preparation method of rare earth oxide superfine powder is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
(1) surface treatment: adjusting the rare earth chloride solution with the concentration of 0.5-2.0mol/L to be alkaline, adding a surface additive into the rare earth chloride solution, and uniformly mixing to obtain a first solution; under the condition of stirring, dropwise adding an ammonium bicarbonate solution into the first solution to obtain a second solution;
(2) and (3) peroxide treatment: adding a stabilizer into a hydrogen peroxide solution with the concentration of 35-70%, then adding into a second solution, aging for 4-10 hours, filtering and washing to obtain a rare earth carbonate peroxide precipitate;
(3) microwave calcination: and placing the peroxycarbonate rare earth precipitate into a microwave reactor for microwave heating and calcining to obtain the rare earth oxide superfine powder.
2. The microwave calcination preparation method of rare earth oxide ultrafine powder according to claim 1, characterized in that: the surface auxiliary agent in the step (1) is one of polyvinylpyrrolidone, stearic acid, oleic acid, sodium dodecyl sulfate, polyethylene glycol and polyacrylate; the addition amount of the surface auxiliary agent is 5-10% of the molar mass of the rare earth chloride.
3. The microwave calcination preparation method of rare earth oxide ultrafine powder according to claim 1, characterized in that: the rare earth chloride is lanthanum chloride or erbium chloride.
4. The microwave calcination preparation method of rare earth oxide ultrafine powder according to claim 1, characterized in that: the adding amount of ammonium bicarbonate in the step (1) is 1.0 to 3.0 times of the molar mass of the rare earth chloride solution.
5. The microwave calcination preparation method of rare earth oxide ultrafine powder according to claim 1, characterized in that: and (3) the stabilizer in the step (2) is acrylic acid or polyacrylamide.
6. The microwave calcination preparation method of rare earth oxide ultrafine powder according to claim 1, characterized in that: the addition amount of the stabilizer is 3-10% of the volume ratio of the hydrogen peroxide solution.
7. The microwave calcination preparation method of rare earth oxide ultrafine powder according to claim 1, characterized in that: the microwave heating calcination frequency in the step (3) is 915 +/-50 MHz or 2450 +/-50 MHz, the microwave power is 1-10kw, and the microwave output mode comprises two modes of continuous waves and pulse waves or two combination modes of the continuous waves and the pulse waves.
8. The microwave calcination preparation method of rare earth oxide ultrafine powder according to claim 1, characterized in that: the microwave heating calcination time in the step (3) is 1-3 hours.
9. The microwave calcination preparation method of rare earth oxide ultrafine powder according to claim 1, characterized in that: the temperature of the microwave heating calcination is 800-1200 ℃.
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