Superfine scandium oxide as well as preparation method and application thereof

Abstract

The invention provides superfine scandium oxide as well as a preparation method and application thereof. The preparation method comprises the steps that in the presence of microwaves and an anionic surfactant, a scandium-containing soluble salt solution and a precipitant are subjected to a precipitation reaction, scandium oxalate precipitate is obtained, and the precipitant is oxalic acid or oxalate; roasting the scandium oxalate precipitate to obtain superfine scandium oxide; the anionic surfactant comprises but is not limited to a sulfate surfactant and / or a sulfonate surfactant. The temperature of a reaction system can be rapidly increased within a short time through microwaves, and when oxalic acid and oxalate are used as precipitants to be subjected to precipitation reaction with a scandium-containing soluble salt solution, due to the fact that the anionic surfactant has good acid and alkali resistance, large steric hindrance and rich surface charges, the scandium-containing soluble salt solution can be rapidly precipitated. And after being combined to the surface of the scandium oxalate precipitate, the scandium oxalate has better dispersity and stability. And scandium oxide with small particle size, high specific surface area and uniform particle size can be obtained through roasting.

Description

technical field

[0001] The invention relates to the field of material chemistry, in particular to an ultrafine scandium oxide, its preparation method and application. Background technique

[0002] Scandium oxide (Sc 2 o 3 ) is one of the more important products in scandium products. sc 2 o 3 It is a white powder, relatively stable in air at room temperature, with a melting point of 920°C and a density of 3.864g / cm 3 , belonging to the cubic crystal form. Under certain external conditions, Sc 2 o 3 It can be made into metal scandium, salts (scandium chloride, scandium fluoride, scandium iodide, scandium oxalate, etc.) and products of various scandium alloys. sc 2 o 3 Some of its characteristics make it have good application in aluminum alloy, electric light source, laser, catalyst, activator, ceramics and aerospace, etc., and its development prospect is very broad. Among them, the ultra-fine scandium oxide powder has a particle size of 10-100 nanometers, which can ...

Examples

preparation example Construction

[0021] 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 above-mentioned technical problems, the application provides a method for preparing ultrafine scandium oxide, the preparation method comprising: in the presence of microwaves and anionic surfactants, the soluble salt solution containing scandium is subjected to precipitation reaction with a precipitant to obtain Scandium oxalate precipitation, the precipitating agent is oxalic acid or oxalate; the scandium oxalate precipitation is roasted to obtain ultrafine scandium oxide; anionic surfactants include but not limited to sulfate ester surfactants and / or sulfonate lipid surfactants .

[0022] Taking oxalate as an example, the reaction principle of the above preparation method is as follows:

[0023] sc 3+ +C 2 o 4 2- →S C2 (C 2 o 4 ) 3

[0024] S C2 (C 2 o 4 ) 3...

Embodiment 1

[0039] Under the condition of reaction temperature 90 ℃, 600W microwave radiation, the scandium chloride solution of 1.0mol / L and anion surface active agent (the weight ratio of sodium lauryl sulfate and sodium dodecylsulfonate are 1:2 ) mixing, the consumption of anionic surfactant is 0.2g / L, obtains mixed solution; Then under the first stirring rate of 450r / min, according to scandium ion and precipitant molar ratio is 1:2, to above-mentioned mixed solution Add a precipitant (oxalic acid) dropwise. After the precipitating agent is added, the product system of the precipitation reaction is continuously stirred for 30 min at the second stirring speed of 200 r / min, and the reaction ends.

[0040] After aging the product system of the precipitation reaction at 90° C. for 60 min, the obtained product system was centrifuged, washed three times with ethanol and pure water respectively, and the obtained precipitate was placed in a vacuum drying oven. Drying treatment at 100°C for 18...

Embodiment 2

[0042] Under the microwave radiation condition of reaction temperature 70 ℃, 500W, the scandium chloride solution of 0.5mol / L and anionic surface active agent (the weight ratio of sodium lauryl sulfate and sodium dodecylsulfonate are 1:2 ) mixed, the consumption of anionic surfactant is 0.2g / L, obtains mixed solution; Then under the first stirring rate of 300r / min, according to scandium ion and precipitant molar ratio is 1:3 in above-mentioned mixed solution Slowly add the precipitant (ammonium oxalate) dropwise. After the precipitating agent is added, the product system of the precipitation reaction is continuously stirred for 60 min at the second stirring rate of 100 r / min, and the reaction ends.

[0043] After aging the product system of the precipitation reaction at 70° C. for 180 min, the obtained product system was subjected to suction filtration, washed three times with ethanol and water respectively, and the obtained precipitate was placed in a vacuum drying oven. Dry...

technical field

[0001] The invention relates to the field of material chemistry, in particular to an ultrafine scandium oxide, its preparation method and application. Background technique

[0002] Scandium oxide (Sc 2 o 3 ) is one of the more important products in scandium products. sc 2 o 3 It is a white powder, relatively stable in air at room temperature, with a melting point of 920°C and a density of 3.864g / cm 3 , belonging to the cubic crystal form. Under certain external conditions, Sc 2 o 3 It can be made into metal scandium, salts (scandium chloride, scandium fluoride, scandium iodide, scandium oxalate, etc.) and products of various scandium alloys. sc 2 o 3 Some of its characteristics make it have good application in aluminum alloy, electric light source, laser, catalyst, activator, ceramics and aerospace, etc., and its development prospect is very broad. Among them, the ultra-fine scandium oxide powder has a particle size of 10-100 nanometers, which can ...

Examples

preparation example Construction

[0021] 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 above-mentioned technical problems, the application provides a method for preparing ultrafine scandium oxide, the preparation method comprising: in the presence of microwaves and anionic surfactants, the soluble salt solution containing scandium is subjected to precipitation reaction with a precipitant to obtain Scandium oxalate precipitation, the precipitating agent is oxalic acid or oxalate; the scandium oxalate precipitation is roasted to obtain ultrafine scandium oxide; anionic surfactants include but not limited to sulfate ester surfactants and / or sulfonate lipid surfactants .

[0022] Taking oxalate as an example, the reaction principle of the above preparation method is as follows:

[0023] sc 3+ +C 2 o 4 2- →S C2 (C 2 o 4 ) 3

[0024] S C2 (C 2 o 4 ) 3...

Embodiment 1

[0039] Under the condition of reaction temperature 90 ℃, 600W microwave radiation, the scandium chloride solution of 1.0mol / L and anion surface active agent (the weight ratio of sodium lauryl sulfate and sodium dodecylsulfonate are 1:2 ) mixing, the consumption of anionic surfactant is 0.2g / L, obtains mixed solution; Then under the first stirring rate of 450r / min, according to scandium ion and precipitant molar ratio is 1:2, to above-mentioned mixed solution Add a precipitant (oxalic acid) dropwise. After the precipitating agent is added, the product system of the precipitation reaction is continuously stirred for 30 min at the second stirring speed of 200 r / min, and the reaction ends.

[0040] After aging the product system of the precipitation reaction at 90° C. for 60 min, the obtained product system was centrifuged, washed three times with ethanol and pure water respectively, and the obtained precipitate was placed in a vacuum drying oven. Drying treatment at 100°C for 18...

Embodiment 2

[0042] Under the microwave radiation condition of reaction temperature 70 ℃, 500W, the scandium chloride solution of 0.5mol / L and anionic surface active agent (the weight ratio of sodium lauryl sulfate and sodium dodecylsulfonate are 1:2 ) mixed, the consumption of anionic surfactant is 0.2g / L, obtains mixed solution; Then under the first stirring rate of 300r / min, according to scandium ion and precipitant molar ratio is 1:3 in above-mentioned mixed solution Slowly add the precipitant (ammonium oxalate) dropwise. After the precipitating agent is added, the product system of the precipitation reaction is continuously stirred for 60 min at the second stirring rate of 100 r / min, and the reaction ends.

[0043] After aging the product system of the precipitation reaction at 70° C. for 180 min, the obtained product system was subjected to suction filtration, washed three times with ethanol and water respectively, and the obtained precipitate was placed in a vacuum drying oven. Dry...

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