阅读说明：本技术 制备球形氧化钪的方法 (Method for preparing spherical scandium oxide ) 是由 付国燕 李晓艳 王玮玮 付云枫 杜尚超 于 2019-09-27 设计创作，主要内容包括：公开一种制备球形氧化钪的方法,包括：形成溶液步骤,配制含钪离子的溶液；沉淀步骤,在微波辐射条件下,添加乙二醇分散剂后,以碳酸盐为沉淀剂添加到所述溶液中进行沉淀反应；陈化步骤,对沉淀反应完成后的体系进行陈化；及焙烧步骤,将制得的沉淀物经过洗涤干燥后焙烧。本发明以碳酸盐作为晶粒成核剂,聚乙二醇为分散剂,在微波辐射条件下,通过控制一定反应工艺条件,制备出球形氧化钪。本发明的方法可以实现制备球形氧化钪粉体材料,增强了氧化钪多功能性及拓宽了氧化钪的应用范围,可用于制备高效激光器、超导材料、固体燃料电池的电解质材料等方面。(Disclosed is a method for preparing spherical scandium oxide, which comprises the following steps: a solution forming step of preparing a solution containing scandium ions; a precipitation step, adding a glycol dispersant under the condition of microwave radiation, and then adding carbonate serving as a precipitator into the solution to perform precipitation reaction; an aging step, aging the system after the precipitation reaction is finished; and a roasting step, namely washing and drying the prepared precipitate and roasting. According to the invention, spherical scandium oxide is prepared by taking carbonate as a grain nucleating agent and polyethylene glycol as a dispersing agent under the microwave radiation condition and controlling certain reaction process conditions. The method can realize the preparation of spherical scandium oxide powder materials, enhances the multifunctionality of scandium oxide, widens the application range of scandium oxide, and can be used for preparing high-efficiency lasers, superconducting materials, electrolyte materials of solid fuel cells and the like.)

1. A method of preparing spherical scandium oxide, comprising:

a solution forming step of preparing a solution containing scandium ions;

a precipitation step, adding a glycol dispersant under the condition of microwave radiation, and then adding carbonate serving as a precipitator into the solution to perform precipitation reaction;

an aging step, aging the system after the precipitation reaction is finished; and

and a roasting step, namely washing and drying the prepared precipitate and roasting.

2. The method for preparing spherical scandium oxide according to claim 1, wherein in the step of forming the solution, a scandium content in the solution is 0.05 to 0.5mol/l, preferably 0.1 to 0.3 mol/l.

3. The method for preparing spherical scandium oxide according to claim 1, wherein in the precipitation step, the radiation power of the microwave radiation is 500 to 700W.

4. The method for preparing spherical scandium oxide according to claim 1, wherein in the precipitation step, the ratio of scandium ions to the precipitating agent is 1: 2-1: 5, dropwise adding a precipitator into the reaction system according to the molar ratio; the temperature of the reaction system is maintained at 20-50 ℃, and preferably 25-40 ℃; the pH value of the reaction system is maintained at 4-8, preferably 5-7; the stirring speed is 50-300 r/min, preferably 100-200 r/min; the stirring time is 15-90 min, preferably 30-80 min.

5. The method for preparing spherical scandium oxide according to claim 1, wherein in the aging step, an aging temperature is 20 to 70 ℃, preferably 30 to 50 ℃; the aging time is 30-200 min, preferably 60-180 min.

6. The method for preparing spherical scandium oxide according to claim 5, wherein the system after aging is subjected to solid-liquid separation, the separated solid matter is washed and dried, the drying temperature is 70-120 ℃, preferably 80-100 ℃, and the drying time is 180-420 min, preferably 200-350 min.

7. The method for preparing spherical scandium oxide according to claim 1, wherein in the roasting step, the roasting temperature is 600 to 1100 ℃, preferably 700 to 1000 ℃; the roasting time is 100-400 min, preferably 120-300 min.

Technical Field

The invention belongs to the field of compound preparation, and particularly relates to a method for preparing spherical scandium oxide.

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 existing process and method for preparing scandium oxide cannot effectively solve the problem of preparing spherical scandium oxide with uniform granularity. In the precipitation process, the reaction process conditions of the scandium salt are complex and difficult to operate and control, and the nonuniform mixing of the material and the precipitant causes the pH value in a local area to be too small or too large, so that the size of scandium oxide crystal grains is different, the stability of a scandium oxide powder material product is seriously influenced, and the production cost is increased. Meanwhile, due to the non-uniformity of the particle size of the product, the performance of the scandium-based material is seriously influenced, so that the application of the scandium oxide powder material is limited.

Disclosure of Invention

In order to overcome the defects, the invention provides a method for preparing spherical scandium oxide.

The invention provides a method for preparing spherical scandium oxide, which comprises the following steps: a solution forming step of preparing a solution containing scandium ions; a precipitation step, adding a glycol dispersant under the condition of microwave radiation, and then adding carbonate serving as a precipitator into the solution to perform precipitation reaction; an aging step, aging the system after the precipitation reaction is finished; and a roasting step, namely washing and drying the prepared precipitate and roasting.

According to an embodiment of the present invention, in the step of forming the solution, the scandium content in the solution is 0.05 to 0.5mol/l, preferably 0.1 to 0.3 mol/l.

According to another embodiment of the present invention, in the precipitation step, the radiation power of the microwave radiation is 500 to 700W.

According to another embodiment of the invention, in the precipitation step, the scandium ions are mixed with a precipitating agent in a ratio of 1: 2-1: 5, dropwise adding a precipitator into the reaction system according to the molar ratio; the temperature of the reaction system is maintained at 20-50 ℃, and preferably 25-40 ℃; the pH value of the reaction system is maintained at 4-8, preferably 5-7; the stirring speed is 50-300 r/min, preferably 100-200 r/min; the stirring time is 15-90 min, preferably 30-80 min.

According to another embodiment of the present invention, in the aging step, the aging temperature is 20 to 70 ℃, preferably 30 to 50 ℃; the aging time is 30-200 min, preferably 60-180 min.

According to another embodiment of the invention, the solid-liquid separation is carried out on the aged system, the separated solid matter is washed and dried, the drying temperature is 70-120 ℃, preferably 80-100 ℃, and the drying time is 180-420 min, preferably 200-350 min.

According to another embodiment of the present invention, in the roasting step, the roasting temperature is 600 to 1100 ℃, preferably 700 to 1000 ℃; the roasting time is 100-400 min, preferably 120-300 min.

According to the method, spherical scandium oxide is prepared by taking carbonate as a precipitator and polyethylene glycol as a dispersing agent under the microwave radiation condition and controlling certain reaction process conditions. The method can realize the preparation of spherical scandium oxide powder materials, enhances the multifunctionality of scandium oxide, widens the application range of scandium oxide, and can be used for preparing high-efficiency lasers, superconducting materials, electrolyte materials of solid fuel cells and the like.

Drawings

The above and other features and advantages of the present invention will become more apparent by describing in detail exemplary embodiments thereof with reference to the attached drawings.

Fig. 1 is a schematic flow chart of the method for preparing spherical scandium oxide according to the present invention.

Fig. 2 is an SEM photograph of the spherical scandium oxide prepared in example 1.

Fig. 3 is an SEM photograph of the spherical scandium oxide prepared in example 2.

Fig. 4 is an SEM photograph of the spherical scandium oxide prepared in example 3.

Detailed Description

The present invention will be described in detail with reference to the following embodiments.

As shown in fig. 1, the method for preparing spherical scandium oxide of the present invention includes: s1 solution forming step, preparing a solution containing scandium ions; s2 precipitation, adding glycol dispersant under microwave radiation, and adding carbonate as precipitant into the solution to perform precipitation reaction; an S3 aging step, aging the system after the precipitation reaction is finished; and S4 roasting step, washing and drying the obtained precipitate, and roasting.

In step S1, a solution is prepared from a soluble compound containing scandium. 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. The scandium content in the solution is 0.05-0.5 mol/l, preferably 0.1-0.3 mol/l.

The step S2 is performed under microwave irradiation conditions. And (3) the microwave radiation intensity is 500-700W, and a precipitating agent is added under the microwave radiation condition for precipitation reaction to generate a scandium-containing precipitate precursor. The precipitant may be sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, potassium carbonate, potassium bicarbonate, etc. The radiation power of the microwave radiation is 500-700W. In step S2, scandium ions and a precipitant are mixed in a ratio of 1: 2-1: 5mol ratio, adding a precipitant dropwise into the reaction system. In the reaction process, the temperature of the reaction system is maintained at 20-50 ℃, and preferably 25-40 ℃. The pH value of the reaction system is maintained at 4-8, preferably 5-7. The stirring speed is 50 to 300r/min, preferably 100 to 200 r/min. The stirring time is 15-90 min, preferably 30-80 min.

In the step S3, the aging temperature is 20-70 ℃, preferably 30-50 ℃. The aging time is 30-200 min, preferably 60-180 min.

And (4) performing solid-liquid separation on the aged system, washing the separated solid matter and drying. The drying temperature is 70-120 ℃, and preferably 80-100 ℃. The drying time is 180-420 min, preferably 200-350 min.

Finally, the S5 baking step is performed. In the step, the roasting temperature is 600-1100 ℃, and preferably 700-1000 ℃. The roasting time is 100-400 min, preferably 120-300 min.