CN114477263A - Superfine scandium oxide, preparation method and application thereof - Google Patents

Superfine scandium oxide, preparation method and application thereof Download PDF

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CN114477263A
CN114477263A CN202210205141.1A CN202210205141A CN114477263A CN 114477263 A CN114477263 A CN 114477263A CN 202210205141 A CN202210205141 A CN 202210205141A CN 114477263 A CN114477263 A CN 114477263A
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scandium
oxalate
temperature
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scandium oxide
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CN114477263B (en
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付国燕
刘召波
王玮玮
姚心
杜尚超
彭建华
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China ENFI Engineering Corp
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    • C—CHEMISTRY; METALLURGY
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    • C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/212—Scandium oxides or hydroxides
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Abstract

The invention provides superfine scandium oxide, and a preparation method and application thereof. The preparation method comprises the following steps: carrying out precipitation reaction on a scandium-containing soluble salt solution and a precipitator in the presence of microwaves and an anionic surfactant to obtain scandium oxalate precipitate, wherein the precipitator is oxalic acid or oxalate; roasting the scandium oxalate precipitate to obtain superfine scandium oxide; anionic surfactants include, but are not limited to, sulfate-type surfactants and/or sulfonate-type surfactants. The microwave can quickly raise the temperature of a reaction system in a short time, and oxalic acid and oxalate are used as precipitating agents to perform precipitation reaction with a scandium-containing soluble salt solution, so that the anionic surfactant has good acid and alkali resistance, large steric hindrance and rich surface charge, and can enable scandium oxalate to have good dispersibility and stability after being combined to the precipitation surface of scandium oxalate. Scandium oxide with small grain diameter, high specific surface area and uniform grain size can be obtained by roasting.

Description

Superfine scandium oxide, preparation method and application thereof
Technical Field
The invention relates to the field of material chemistry, and particularly relates to superfine scandium oxide, and a preparation method and application thereof.
Background
Scandium oxide (Sc)2O3) Is one of the more important products in scandium products. Sc (Sc)2O3Is white powder, stable in air at normal temperature, and has melting point of 920 deg.C and density of 3.864g/cm3Belonging to cubic crystal form. Under a certain external condition, Sc2O3Can be made into metal scandium, salts (scandium chloride, scandium fluoride, scandium iodide, scandium oxalate, etc.) and various scandium alloys. Sc (Sc)2O3The aluminum alloy has certain characteristics, so that the aluminum alloy has good application in the aspects of aluminum alloy, electric light sources, laser, catalysts, activators, ceramics, space navigation and the like, and has very wide development prospect. The particle size of the superfine scandium oxide powder is 10-100 nanometers, and the superfine scandium oxide powder can be used for preparing high-efficiency lasers, superconducting materials, electrolyte materials of solid fuel cells and the like. The material structure and the particle size have an important influence on the surface performance of the powder material, the superfine powder material and the powder material with a spherical structure have larger specific surface area and larger chemical activity, and have an important influence on the performance of the subsequently prepared material, and the superfine spherical scandium oxide powder material can obviously improve the performance of the subsequently prepared metal scandium, scandium salt and scandium-containing alloy, thereby widening the application field and the prospect of the scandium-containing material.
CN 110498439 a provides a method for preparing scandium oxide powder with porous structure, which includes: a solution forming step of preparing a solution containing scandium ions; a precipitation step, adding oxalic acid or oxalate serving as a precipitator into the solution to perform precipitation reaction under the condition of microwave radiation; and a roasting step, namely washing and drying the prepared precipitate and roasting. Although the scandium oxide powder with a porous structure is prepared by the method, the particle size is large, the specific surface area is small, and the uniformity of the particle size is low.
CN109133142 provides a preparation method of ultramicro scandium oxide. The method comprises the following steps: extracting the scandium-containing ion solution by using a carboxylic acid extractant-organic solvent mixed solution to obtain a scandium-loaded organic phase, wherein the carboxylic acid extractant in the carboxylic acid extractant-organic solvent mixed solution is added in excess relative to scandium ions in the scandium-containing ion solution; mixing the scandium-loaded organic phase with ammonia water and carrying out saponification reaction to form a water-oil emulsion; heating and drying the water-oil emulsion to perform thermal hydrolysis reaction to obtain scandium precipitate; and calcining the scandium precipitate to obtain the ultramicro scandium oxide. The preparation method effectively prepares the scandium oxide product with the size of ultra-micro level, but the process is more complex.
In view of the above problems, it is necessary to provide a method for preparing scandium oxide, which has both a short process flow and a large specific surface area.
Disclosure of Invention
The invention mainly aims to provide superfine scandium oxide, a preparation method and application thereof, and aims to solve the problems of long process flow and small specific surface area of scandium oxide in the existing method for preparing scandium oxide.
In order to achieve the above object, one aspect of the present invention provides a method for preparing ultrafine scandia, the method comprising: carrying out precipitation reaction on a scandium-containing soluble salt solution and a precipitator in the presence of microwaves and an anionic surfactant to obtain scandium oxalate precipitate, wherein the precipitator is oxalic acid or oxalate; and roasting the scandium oxalate precipitate to obtain superfine scandium oxide, wherein the anionic surfactant is selected from sulfate surfactants and/or sulfonate surfactants.
Further, the sulfate ester surfactant is selected from one or more of the group consisting of sodium lauryl sulfate, sodium dodecylbenzene sulfate and condensed alkyl phenyl ether sulfate; the sulfonate surfactant is one or more selected from the group consisting of sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate and lignosulfonate; preferably, the weight ratio of the sulfate surfactant to the sulfonate surfactant is 1 (2-5).
Furthermore, the content of scandium ions in the scandium-containing soluble salt solution is 0.1-2.0 mol/L, and the content of an anionic surfactant is 0.01-2 g/L; preferably, the content of scandium ions in the scandium-containing soluble salt solution is 0.5-1.5 mol/L.
Further, the precipitation reaction step comprises: mixing a scandium-containing soluble salt solution with an anionic surfactant, and adjusting the pH of a reactant system of a precipitation reaction to 1-5 by using a pH regulator to obtain a mixed solution; adding a precipitant into the mixed solution for reaction to obtain scandium oxalate precipitate; preferably, the precipitant is added to the mixed solution at a first stirring rate, and the first stirring rate is 150 to 500r/min, preferably 200 to 450 r/min.
Furthermore, in the precipitation reaction, the frequency of the microwave is 300-700W, preferably 450-600W; the reaction temperature is 60-100 ℃, and preferably 80-90 ℃.
Further, the temperature of the roasting step is 600-900 ℃, and preferably 700-850 ℃; the time of the roasting step is 120-400 min, preferably 220-300 min.
Further, before the firing step, the preparation method further comprises: continuously stirring a product system of the precipitation reaction at a second stirring speed, and then aging and drying to obtain scandium oxalate precipitate; wherein the second stirring speed is 30-300 r/min, and the stirring time is 15-90 min; the temperature of the aging step is 60-100 ℃, and the time of the aging step is 30-350 min; the temperature of the drying step is 70-120 ℃, and the time of the drying step is 120-350 min.
Further, the second stirring speed is 80-150 r/min; stirring for 30-60 min; the temperature of the aging step is 80-90 ℃; the time of the aging step is 60-300 min; the temperature of the drying step is 80-100 ℃, and the time of the drying step is 180-300 min.
The application also provides superfine scandium oxide, which is prepared by the preparation method, or the superfine scandium oxide has the particle size of 30-80 nm and the specific surface area of 200-500 m2/g。
The application further provides application of the superfine scandium oxide in a laser, a superconducting material or an electrolyte material of a solid fuel cell.
By applying the technical scheme of the invention, the temperature of a reaction system can be quickly raised in a short time by introducing microwaves in the preparation process of scandium oxide, and the risk of nonuniform particle size caused by nonuniform internal and external heating of scandium oxide particles due to conventional heating is inhibited. In the presence of a specific anionic surfactant, oxalic acid and oxalate are taken as precipitating agents to carry out precipitation reaction with a scandium-containing soluble salt solution, and the anionic surfactant can be bonded to the surface of the precipitation product scandium oxalate precipitation. The anionic surfactant has good acid and alkali resistance, large steric hindrance and abundant surface charges, so that scandium oxalate precipitates in a precipitation reaction product system have good dispersibility and stability. This enables scandium oxalate to be calcined to obtain scandium oxide with small particle size, high specific surface area and uniform particle size. Meanwhile, the process also has the advantages of short flow, simple preparation method, lower cost and the like.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a scanning electron microscope result image of the ultrafine spherical scandium oxide powder material prepared in the example.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background art, the existing methods for preparing scandium oxide have the problems of long process flow and small specific surface area of scandium oxide. In order to solve the technical problem, the application provides a preparation method of superfine scandium oxide, and the preparation method comprises the following steps: carrying out precipitation reaction on a scandium-containing soluble salt solution and a precipitating agent in the presence of microwaves and an anionic surfactant to obtain scandium oxalate precipitate, wherein the precipitating agent is oxalic acid or oxalate; roasting the scandium oxalate precipitate to obtain superfine scandium oxide; anionic surfactants include, but are not limited to, sulfate-type surfactants and/or sulfonate-type surfactants.
Taking oxalate as an example, the reaction principle of the preparation method is as follows:
Sc3++C2O4 2-→SC2(C2O4)3
SC2(C2O4)3→SC2O3+CO2↑+CO↑。
the introduction of microwaves in the preparation process of scandium oxide can quickly raise the temperature of a reaction system in a short time, and inhibit the risk of nonuniform particle size caused by nonuniform internal and external heating of scandium oxide particles due to conventional heating. In the presence of a specific anionic surfactant, oxalic acid and oxalate are used as precipitating agents to carry out precipitation reaction with scandium-containing soluble salt solution, and the anionic surfactant can be bonded to the surface of the precipitation product scandium oxalate precipitate. The anionic surfactant has good acid and alkali resistance, large steric hindrance and abundant surface charges, so that scandium oxalate precipitates in a precipitation reaction product system have good dispersibility and stability. This enables scandium oxalate to be calcined to obtain scandium oxide with small particle size, high specific surface area and uniform particle size. Meanwhile, the process also has the advantages of short flow, simple preparation method, lower cost and the like.
The anionic surfactant has better acid and alkali resistance and steric hindrance, and the purpose of regulating the scandium oxide morphology can be achieved by adding the anionic surfactant in the scandium oxide preparation process. In a preferred embodiment, the sulfate ester surfactant is selected from one or more of the group consisting of sodium lauryl sulfate, sodium dodecylbenzene sulfate, and condensed alkyl phenyl ether sulfate; the sulfonate surfactant is one or more selected from the group consisting of sodium dodecylsulfonate, sodium dodecylbenzenesulfonate and lignosulfonate. Compared with other types of surfactants, the anionic surfactants have better steric hindrance, so that the adoption of the anionic surfactants is beneficial to further improving the specific surface area and uniformity of scandium oxide and reducing the particle size of scandium oxide. In order to further improve the synergistic effect of the anionic surfactant and further improve the distribution uniformity and integrity of the particle size, the weight ratio of the sulfate surfactant to the sulfonate surfactant is preferably 1 (2-5). The weight ratio of the sulfate surfactant to the sulfonate surfactant can be 1:2, 1:3, 1:4 and 1: 5.
A soluble compound containing scandium is used as a raw material to prepare a solution. Or a sparingly soluble compound of scandium is reacted with an acid to form a solution of scandium ions. A solution containing scandium ions may be prepared using scandium chloride as a raw material. Scandium oxide, scandium hydroxide, or scandium carbonate may be used as a raw material to react with hydrochloric acid to form a solution as a scandium ion-containing solution. In a preferred embodiment, the scandium ion content in the scandium-containing soluble salt solution is 0.1-2.0 mol/L, and the anionic surfactant content is 0.01-2 g/L. Limiting the ratio of the amounts of the two to the above range is advantageous for further reducing the particle size of the scandium oxide particles and improving the uniformity thereof. More preferably, the content of scandium ions in the scandium-containing soluble salt solution is 0.5-1.5 mol/L. Alternatively, the anionic surfactant is used in an amount of 0.01g/L, 0.05g/L, 0.1g/L, 0.2g/L, 0.3g/L, 0.4g/L, 0.5g/L, 0.6g/L, 0.7g/L, 0.8g/L, 0.9g/L, 1g/L, 1.1g/L, 1.2g/L, 1.3g/L, 1.4g/L, 1.5g/L, 1.6g/L, 1.7g/L, 1.8g/L, 1.9g/L, 2.0 g/L.
Under acidic conditions, scandium oxalate can precipitate in the form of a precipitate. In order to increase the efficiency of scandium oxalate precipitation and simultaneously increase the yield of scandium oxide, in a preferred embodiment, the precipitation reaction step comprises: mixing a scandium-containing soluble salt solution with an anionic surfactant, and adjusting the pH of a reactant system of a precipitation reaction to 1-5 by using a pH regulator to obtain a mixed solution; and adding a precipitator into the mixed solution for reaction to obtain scandium oxalate precipitate. The pH may be selected from 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 and 5. In order to further improve the reaction rate of the precipitation reaction and the uniformity of the particle size of the target product, preferably, the precipitant is added into the mixed solution at a first stirring rate, and the first stirring rate is 150 to 500 r/min. Wherein the first stirring speed can be selected from 150r/min, 200r/min, 250r/min, 300r/min, 350r/min, 400r/min, 450r/min and 500 r/min. More preferably, the first stirring speed is 200 to 450 r/min.
In a preferred embodiment, the frequency of the microwave is 300-700W, and the reaction temperature is 60-100 ℃. Limiting the frequency of the microwaves and the reaction temperature within the above ranges compared to other ranges is advantageous for better control of the temperature during the precipitation reaction, and thus for reducing the risk of aggregation of the particles of scandium oxide. The frequency of the microwave can be selected from 300W, 350W, 400W, 450W, 500W, 550W, 600W, 650W and 700W, and the reaction temperature can be selected from 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 100 ℃. In order to further reduce the particle size of the scandium oxide particles and increase the specific surface area, the frequency of the microwave is more preferably 450 to 600W, and the reaction temperature is more preferably 80 to 90 ℃.
After scandium precipitation is obtained, scandium oxide powder can be obtained only by calcining scandium precipitation. In a preferred embodiment, the temperature of the roasting step is 600-900 ℃, and the roasting time is 120-400 min. The temperature and time of the calcination step include, but are not limited to, the above range, and it is limited to the above range, and the decomposition of scandium hydroxide is more complete, and the anionic surfactant and the like precipitated therewith can also be decomposed into CO2And water vapor, and the scandium oxide powder formed is more dense. The roasting step can be carried out at 600 deg.C, 650 deg.C, 700 deg.C, 750 deg.C, 800 deg.C, 850 deg.C, 900 deg.C, and the roasting time can be 120min, 150min, 200min, 250min, 300min, 350min, 400 min. In order to further improve the comprehensive performance of scandium oxide, the temperature of the roasting step is more preferably 700-850 ℃, and the roasting time is 220-300 min.
In a preferred embodiment, the preparation method further comprises, before the firing step: continuously stirring a product system of the precipitation reaction at a second stirring speed, and then aging and drying to obtain scandium oxalate precipitate; wherein the second stirring speed is 30-300 r/min, and the stirring time is 15-90 min; the temperature of the aging step is 60-100 ℃, and the time of the aging step is 30-350 min; the temperature of the drying step is 70-120 ℃, and the time of the drying step is 120-350 min. After the precipitation reaction, stirring a product system of the precipitation reaction at a slower speed, and performing aging treatment at a specific temperature and within a specific time, so that the precipitation efficiency of scandium oxalate is further improved, and the yield of scandium oxide is further improved. The drying step is favorable for removing moisture in the scandium oxalate, and the drying process at the drying temperature and within the drying time is favorable for further improving the removal efficiency of the moisture in the scandium oxalate and reducing the risk of scandium oxalate agglomeration. The second stirring rate is selected from 30r/min, 50r/min, 100r/min, 150r/min, 200r/min, 250r/min and 300r/min, and the stirring time is selected from 15min, 30min, 45min, 60min, 75min and 90 min. The temperature of the aging step can be selected from 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, and 100 deg.C, and the time of the aging step can be selected from 30min, 60min, 120min, 180min, 240min, 300min, and 350 min; the temperature of the drying step can be selected from 70 deg.C, 80 deg.C, 90 deg.C, 100 deg.C, 110 deg.C, and 120 deg.C, and the time of the drying step can be selected from 120min, 150min, 180min, 210min, 240min, 270min, 300min, and 350 min.
Through research on the second stirring speed and stirring time, the aging temperature and aging time, and the drying temperature and drying time, the inventors found that the three groups of parameters have a certain correlation, because the particle size of scandium oxide can be further reduced by optimizing the three groups of parameters. In a preferred embodiment, the second stirring speed is 80-150 r/min; stirring for 30-60 min; the temperature of the aging step is 80-90 ℃; the time of the aging step is 60-300 min; the temperature of the drying step is 80-100 ℃, and the time of the drying step is 180-300 min.
The application also provides superfine scandium oxide, which is prepared by the preparation method, or the superfine scandium oxide has the particle size of 30-80 nm and the specific surface area of 200-500 m2/g。
The introduction of microwaves in the preparation process of scandium oxide can quickly raise the temperature of a reaction system in a short time, and reduce the probability of heated agglomeration of scandium oxide particles. In the presence of a specific anionic surfactant, oxalic acid and oxalate are taken as precipitating agents to carry out precipitation reaction with a scandium-containing soluble salt solution, and the anionic surfactant can be bonded to the surface of the precipitation product scandium oxalate precipitation. The anionic surfactant has good acid and alkali resistance, large steric hindrance and abundant surface charges, so that scandium oxalate precipitates in a precipitation reaction product system have good dispersibility and stability. Therefore, scandium oxalate can obtain scandium oxide with small particle size, high specific surface area and uniform particle size after being roasted. Meanwhile, the process also has the advantages of short flow, simple preparation method, lower cost and the like.
The application further provides an application of the superfine scandium oxide prepared by the method in a laser, a superconducting material or an electrolyte material of a solid fuel cell.
The scandium oxide has the advantages of small particle size, high specific surface area, uniform particle size and the like, so that the scandium oxide can be applied to the fields of lasers, superconducting materials, electrolyte materials of solid fuel cells and the like, and the related performance of the scandium oxide can be greatly improved.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
Mixing 1.0mol/L scandium chloride solution with an anionic surfactant (the weight ratio of sodium dodecyl sulfate to sodium dodecyl sulfate is 1:2) at the reaction temperature of 90 ℃ and under the microwave radiation condition of 600W, wherein the using amount of the anionic surfactant is 0.2g/L, and obtaining a mixed solution; then, under a first stirring speed of 450r/min, a precipitator (oxalic acid) is dropwise added into the mixed solution according to the mole ratio of scandium ions to the precipitator of 1: 2. And after the precipitant is added, continuously stirring the product system of the precipitation reaction at a second stirring speed of 200r/min for 30min, and finishing the reaction.
Aging the product system of the precipitation reaction at 90 deg.C for 60min, centrifuging the obtained product system, washing with ethanol and pure water for 3 times, and placing the obtained precipitate in a vacuum drying oven. Drying at 100 deg.C for 180 min; placing the dried sample in a corundum crucible, roasting for 250min at 850 ℃ by using a microwave muffle furnace, and cooling the sample to normal temperature along with the furnace; the scandium oxide powder material with the nano-scale spherical structure is prepared under the condition, the particle size is 30-40 nm, and the specific surface area is 450 ∞500m2The particle size distribution is narrow.
Example 2
Mixing 0.5mol/L scandium chloride solution with an anionic surfactant (the weight ratio of sodium dodecyl sulfate to sodium dodecyl sulfate is 1:2) at the reaction temperature of 70 ℃ and under the microwave radiation condition of 500W, wherein the dosage of the anionic surfactant is 0.2g/L, and obtaining a mixed solution; then, under a first stirring speed of 300r/min, the precipitator (ammonium oxalate) is slowly dropped into the mixed solution according to the mole ratio of scandium ions to the precipitator of 1: 3. And after the precipitant is added, continuously stirring the product system of the precipitation reaction at a second stirring speed of 100r/min for 60min, and finishing the reaction.
Aging the product system of the precipitation reaction at 70 ℃ for 180min, carrying out suction filtration treatment on the obtained product system, washing the product system for 3 times by using ethanol and water respectively, and placing the obtained precipitate in a vacuum drying oven. Drying at 80 deg.C for 300 min; placing the dried sample in a corundum crucible, roasting in a microwave muffle furnace at 700 ℃ for 300min, and cooling the sample to normal temperature along with the furnace; the nano-scale spherical scandium oxide powder material is prepared under the condition, the particle diameter is 50-60 nm, and the specific surface area is 380-420 m2(g), the particle size distribution is uniform.
Example 3
Mixing 1.5mol/L scandium chloride solution and an anionic surfactant (the weight ratio of sodium dodecyl sulfate to sodium dodecyl sulfate is 1:2) at 80 ℃ under 500W microwave radiation condition, wherein the dosage of the anionic surfactant is 0.2g/L, and obtaining a mixed solution; then, under a first stirring speed of 200r/min, a precipitant (oxalic acid) is dropwise added into the mixed solution according to the molar ratio of scandium ions to the precipitant of 1: 5. And after the precipitant is added, continuously stirring the product system of the precipitation reaction at a second stirring speed of 50r/min for 45min, and finishing the reaction.
Aging the product system of precipitation reaction at 80 deg.C for 300min, vacuum filtering, washing with ethanol and water for 3 times, and precipitatingThe material was placed in a vacuum drying oven. Drying at 90 deg.C for 240 min; placing the dried sample in a corundum crucible, roasting for 200min at 800 ℃ in a muffle furnace by using the muffle furnace, and cooling the sample to normal temperature along with the furnace; the method is obtained by testing and analyzing a sample, and the nano spherical scandium oxide powder material with uniform particle size and nano spherical scandium oxide powder structure is prepared under the condition, the particle size is 40-60 nm, and the specific surface area is 380-485 m2The particle size distribution spans a large amount, and the particle size of the nanoparticles prepared in examples 1 and 2 is not uniform.
Example 4
The differences from example 1 are: the amount of the anionic surfactant used was 0.005 g/L.
When the dosage of the surfactant is less, the particle size is 30-70 nm, the particle size distribution of the reaction product is larger, and the specific surface area is 260-340 m2The nanospherical structures are incomplete, in which non-spherical structures can be doped.
Example 5
The differences from example 1 are:
in the precipitation reaction process, the second stirring speed is 80r/min, and the stirring time is 60 min; the frequency of the microwave is 300W, and the reaction temperature is 80 ℃; the temperature of the aging step is 90 ℃, and the time of the aging step is 120 min; the temperature of the drying step is 80 ℃, and the time of the drying step is 240 min.
Compared with the example 1, the second stirring speed is slowed, the particle size of the product is 30-50 nm, and the specific surface area is 420-500 m2The particle size distribution is wide.
Example 6
The differences from example 1 are:
in the precipitation reaction process, the second stirring speed is 150r/min, and the stirring time is 60 min; the frequency of the microwave is 700Hz, and the reaction temperature is 90 ℃; the temperature of the aging step is 80 ℃, and the time of the aging step is 120 min; the temperature of the drying step is 100 ℃, and the time of the drying step is 240 min.
Compared with the example 1, the second stirring speed is too fast, the particle size is 30-40 nm, and the specific surface area is 450-500 m2Per g, but partially scandiaThe spherical structure is incomplete.
Example 7
The differences from example 1 are:
in the precipitation reaction process, the second stirring speed is 200r/min, and the stirring time is 60 min; the frequency of the microwave is 300W, and the reaction temperature is 70 ℃; the temperature of the aging step is 70 ℃, and the time of the aging step is 120 min; the temperature of the drying step is 120 ℃, and the time of the drying step is 240 min.
The nano spherical scandium oxide powder material has a particle size of 50-70 nm and a specific surface area of 350-420 m2The particle size distribution span is larger.
Comparative example 1
The differences from example 1 are: the surfactant is polyethylene glycol nonionic surfactant (the manufacturer is national drug group chemical reagent Co., Ltd.).
The nano spherical scandium oxide powder material is of a layered structure, the particle size distribution is 3-15 mu m, and the specific surface area is 12-23 m2/g。
Comparative example 2
The differences from example 1 are: no surfactant is added in the preparation process.
The prepared scandium oxide is of a strip-shaped structure, the particle size distribution is 3-20 mu m, and the specific surface area is 9-20 m2The particle size distribution is relatively wide.
Comparative example 3
The differences from example 1 are: the preparation process is not carried out under microwave conditions.
Compared with example 1, when the reaction is carried out under the condition of no microwave radiation, the prepared scandium oxide has wider and nonuniform particle size distribution and small specific surface area.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: by adopting the preparation method provided by the application, the spherical scandium oxide with small particle size, high specific surface area and uniform particle size can be obtained. Meanwhile, the process also has the advantages of short flow, simple preparation method, lower cost and the like.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those described or illustrated herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The preparation method of the superfine scandium oxide is characterized by comprising the following steps:
carrying out precipitation reaction on a scandium-containing soluble salt solution and a precipitator in the presence of microwaves and an anionic surfactant to obtain scandium oxalate precipitate, wherein the precipitator is oxalic acid or oxalate;
roasting the scandium oxalate precipitate to obtain the superfine scandium oxide; the anionic surfactant is selected from sulfate surfactants and/or sulfonate surfactants.
2. The production method according to claim 1, wherein the sulfate-based surfactant is one or more selected from the group consisting of sodium lauryl sulfate, sodium dodecylbenzene sulfate and condensed alkylphenyl ether sulfate; the sulfonate surfactant is selected from one or more of the group consisting of sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate and lignosulfonate;
preferably, the weight ratio of the sulfate surfactant to the sulfonate surfactant is 1 (2-5).
3. The method according to claim 1 or 2, wherein the scandium ion content in the scandium-containing soluble salt solution is 0.1 to 2.0mol/L, and the anionic surfactant content is 0.01 to 2 g/L;
preferably, the content of scandium ions in the scandium-containing soluble salt solution is 0.5-1.5 mol/L.
4. The production method according to any one of claims 1 to 3, wherein the precipitation reaction step includes:
mixing the scandium-containing soluble salt solution with the anionic surfactant, and adjusting the pH of a reactant system of a precipitation reaction to 1-5 by using a pH regulator to obtain a mixed solution;
adding the precipitant into the mixed solution for reaction to obtain scandium oxalate precipitate;
preferably, the precipitant is added to the mixed solution at a first stirring speed, and the first stirring speed is 150 to 500r/min, preferably 200 to 450 r/min.
5. The preparation method according to claim 1, wherein in the precipitation reaction, the frequency of the microwave is 300-700W, preferably 450-600W; the reaction temperature is 60-100 ℃, and preferably 80-90 ℃.
6. The method according to claim 5, wherein the temperature of the roasting step is 600 to 900 ℃, preferably 700 to 850 ℃; the time of the roasting step is 120-400 min, preferably 220-300 min.
7. The method of claim 4, further comprising, prior to the firing step:
continuously stirring a product system of the precipitation reaction at a second stirring speed, and then aging and drying to obtain scandium oxalate precipitate;
wherein the second stirring speed is 30-300 r/min, and the stirring time is 15-90 min; the temperature of the aging step is 60-100 ℃, and the time of the aging step is 30-350 min; the temperature of the drying step is 70-120 ℃, and the time of the drying step is 120-350 min.
8. The preparation method according to claim 7, wherein the second stirring rate is 80 to 150 r/min; stirring for 30-60 min; the temperature of the aging step is 80-90 ℃; the time of the aging step is 60-300 min; the temperature of the drying step is 80-100 ℃, and the time of the drying step is 180-300 min.
9. The superfine scandium oxide, which is prepared by the preparation method of any one of claims 1 to 8, or has a particle size of 30 to 80nm and a specific surface area of 200 to 500m2/g。
10. Use of the ultrafine scandia according to claim 9 in a laser, a superconducting material, or an electrolyte material of a solid fuel cell.
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