CN112941340A - High-purity metal strontium and preparation method thereof - Google Patents
High-purity metal strontium and preparation method thereof Download PDFInfo
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- CN112941340A CN112941340A CN202110116526.6A CN202110116526A CN112941340A CN 112941340 A CN112941340 A CN 112941340A CN 202110116526 A CN202110116526 A CN 202110116526A CN 112941340 A CN112941340 A CN 112941340A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
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Abstract
The invention discloses a preparation method of high-purity metal strontium, which is characterized by comprising the following steps: the method comprises the following steps of (1) preparing brick-shaped blanks by adding water into powdery strontium carbonate serving as a raw material, drying the blanks, then calcining the dried blanks in calcining equipment to obtain brick-shaped strontium oxide, crushing the brick-shaped strontium oxide in a crusher, screening and grading the crushed brick-shaped strontium oxide, and storing the crushed brick-shaped strontium oxide in a strontium oxide storage tank; adding aluminum particles into the screened strontium oxide, uniformly mixing, pressing into flat spheres in a ball making machine, and then selecting flat-sphere mixture with a preset particle size and filling the mixture into a charging bucket and feeding the mixture into a reduction tank; under the vacuum condition, the strontium oxide is reduced into metal strontium by aluminum; cooling the metal strontium in a 5N argon environment; and forming and packaging to obtain a high-purity metal strontium product, wherein the mass percent of the purity of the product is higher than 99.9%, and the mass percent of other impurities is as follows: fe is less than or equal to 0.001 percent, Mg is less than or equal to 0.003 percent, Ca is less than or equal to 0.04 percent, Ba is less than or equal to 0.05 percent, and the total content of other impurities is less than or equal to 0.006 percent. The method has the advantages of low requirement on raw materials, high conversion rate, high product purity, simple process and convenience in realizing large-scale production.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to high-purity metal strontium and a preparation method thereof.
Background
Strontium is an alkaline earth metal with yellow luster in silver-white color band, is the element with the least abundance in the alkaline earth metals (except beryllium), and exists in a compound state in nature. The metal strontium has wide application in the industries of electronic information, chemical industry, light industry, medicine, ceramics, metallurgy and the like. At present, the metal strontium required by domestic and international markets is mainly common metal strontium with the strontium content of more than 99.5 percent, but along with the development of high-end industrialization, high-purity metal strontium with the strontium content of more than 99.9 percent and high-purity metal strontium with different shapes are also required to a certain extent. The traditional preparation method of the metal strontium mainly comprises a molten salt electrolysis method and a vacuum thermal reduction method, wherein the molten salt electrolysis method has the problems of high raw material price, environment pollution caused by generated chlorine, large volatilization loss of strontium salt, serious corrosion of electrolysis equipment and the like; the vacuum thermit reduction method mainly comprises an aluminothermic method and a silicothermic method, wherein the vacuum thermit reduction method is the main method for preparing metal strontium at present, the problem of high impurities generally exists in the metal strontium prepared by applying the traditional method, and secondary distillation purification is generally required when high-purity metal strontium with the purity of more than 99.6 percent is produced, so the production cost can be greatly increased.
Disclosure of Invention
Aiming at the problems, the technical problem to be solved by the invention is to provide a preparation method of high-purity metal strontium, which adopts common powdery strontium carbonate as a raw material, and the high-purity metal strontium is obtained through calcination, reduction and cooling.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of high-purity metal strontium is characterized by comprising the following steps: the method adopts powdery strontium carbonate as a raw material and comprises the following steps:
firstly, adding water into powdery strontium carbonate to prepare a brick-shaped blank, drying the brick-shaped blank, and then calcining the dried brick-shaped blank in calcining equipment to obtain brick-shaped strontium oxide;
secondly, after the brick-shaped strontium oxide enters a crusher to be crushed, screening and grading the brick-shaped strontium oxide and storing the brick-shaped strontium oxide in a strontium oxide storage tank;
thirdly, adding aluminum particles into the screened strontium oxide, uniformly mixing, pressing into oblate spheres by a ball making machine, and then selecting oblate mixture with a preset particle size and filling the mixture into a charging bucket to enter a reduction tank;
fourthly, under the vacuum condition, the strontium oxide is reduced into metal strontium by aluminum;
fifthly, cooling the metal strontium in a 5N argon environment;
and sixthly, forming and packaging to obtain the high-purity metal strontium product.
Furthermore, the calcining equipment is a tunnel kiln, the brick-shaped strontium carbonate before entering the tunnel kiln is dried, the moisture content of the brick-shaped strontium carbonate is less than 5%, the calcining temperature in the tunnel kiln is 1400 +/-20 ℃, the calcining time is 12-15 hours, and the content of the calcined strontium oxide is more than or equal to 97%.
Furthermore, the brick-shaped blank has the size of 200-250 mm 100-150 mm 50-80 mm.
Further, the mixing ratio of the strontium oxide to the aluminum particles is 100: 15-100: 17.
Further, the vacuum degree of a reduction tank for reducing strontium oxide is 2-8 Pa, the reaction temperature is 1230-1260 ℃, and the reaction time is 18-24 h.
Further, the grain diameter of the aluminum particles added in the third step is 20-100 meshes, and the grain diameter of the pressed oblate mixed material is more than or equal to 10 mm.
Furthermore, the equipment contacted with the strontium carbonate, the strontium oxide, the oblate mixture and the metal strontium is made of stainless steel.
The high-purity metal strontium prepared by the method is characterized in that: the mass percent of the purity of the product is higher than 99.9%, and the mass percent of other impurities is as follows: fe is less than or equal to 0.001 percent, Mg is less than or equal to 0.003 percent, Ca is less than or equal to 0.04 percent, Ba is less than or equal to 0.05 percent, and the total content of other impurities is less than or equal to 0.006 percent.
The invention has the beneficial effects that: the raw material cost is low, the purity of the finished product is high, the process is simple, and the large-scale production is convenient to realize.
Drawings
Fig. 1 is a schematic perspective view of a preferred embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments and the accompanying drawings.
The preparation method of high-purity metal strontium is shown in figure 1, and is characterized in that: the method adopts powdery strontium carbonate as a raw material and comprises the following steps:
firstly, adding water into powdery strontium carbonate to prepare a brick-shaped blank, drying the brick-shaped blank, and then calcining the dried brick-shaped blank in calcining equipment to obtain brick-shaped strontium oxide;
secondly, after the brick-shaped strontium oxide enters a crusher to be crushed, screening and grading the brick-shaped strontium oxide and storing the brick-shaped strontium oxide in a strontium oxide storage tank;
thirdly, adding aluminum particles into the screened strontium oxide, uniformly mixing, pressing into oblate spheres by a ball making machine, and then selecting oblate mixture with a preset particle size and filling the mixture into a charging bucket to enter a reduction tank;
fourthly, under the vacuum condition, the strontium oxide is reduced into metal strontium by aluminum;
fifthly, cooling the metal strontium in a 5N argon environment;
and sixthly, forming and packaging to obtain the high-purity metal strontium product.
Furthermore, the calcining equipment is a tunnel kiln, the brick-shaped strontium carbonate before entering the tunnel kiln is dried, the moisture content is less than 5%, the calcining temperature in the tunnel kiln is 1400 ℃, the calcining time is 13h, and the content of the calcined strontium oxide is more than or equal to 97%.
Further, the brick blank size is 240 × 115 × 65 mm.
Further, the mixing ratio of the strontium oxide to the aluminum particles is 100: 15-100: 17.
Furthermore, the vacuum degree of a reduction tank for reducing the strontium oxide is 5Pa, the reaction temperature is 1240 ℃, and the reaction time is 20 h.
Further, the grain diameter of the aluminum particles added in the third step is 20-100 meshes, and the grain diameter of the pressed oblate mixed material is more than or equal to 10 mm.
Furthermore, the equipment contacted with the strontium carbonate, the strontium oxide, the oblate mixture and the metal strontium is made of stainless steel.
The high-purity metal strontium prepared by the method is characterized in that: the mass percent of the purity of the product is higher than 99.9%, and the mass percent of other impurities is as follows: fe is less than or equal to 0.001 percent, Mg is less than or equal to 0.003 percent, Ca is less than or equal to 0.04 percent, Ba is less than or equal to 0.05 percent, and the total content of other impurities is less than or equal to 0.006 percent.
The raw material of the preparation method adopts powdery strontium carbonate, water is added to prepare the strontium carbonate brick, the size of the strontium carbonate brick is 240 x 115 x 65mm, the drying and calcining are convenient, compared with other similar processes, the powdery strontium carbonate has lower requirements on the particle size of the raw material, and the purchase cost of the raw material is saved. The prepared strontium carbonate brick is loaded on a kiln car at certain intervals, preheated and dried until the moisture content is lower than 5 percent, and then sent into a tunnel kiln for calcination, wherein the calcination temperature is controlled at 1400 degrees. And after the calcination is finished, the strontium carbonate is converted into strontium oxide, and the strontium carbonate is fully converted due to the calcination in the tunnel kiln, and the content of the strontium oxide is higher than 97 percent. And (3) crushing the qualified calcined strontium oxide brick in a crusher, grading by using an automatic vibrating screen, and selecting proper granular strontium oxide to enter a strontium oxide storage tank for storage. Adding aluminum particles into the screened strontium oxide, uniformly mixing in a mixer, sending into a ball press to press into oblate spherical particles, then entering a screening machine to automatically screen, selecting oblate mixed materials with proper particle sizes to be barreled, sending the barrels into a reduction tank, adopting an aluminothermic vacuum element-changing method, reducing strontium in the strontium oxide by aluminum, producing high-purity strontium metal, wherein the vacuum degree in the reduction tank is 5Pa, the reduced strontium metal is cooled in a 5N argon environment, adopting 5N argon protection in the whole process, preventing the strontium metal from being oxidized again in the cooling process, and influencing the product purity.
In the process, all equipment and facilities which contact the raw material strontium carbonate and the intermediate material metal strontium, aluminum particles, the mixed material and the metal strontium are made of stainless steel, so that the contact between the materials and iron is avoided, and the contact between the iron and impurities in the iron and the impurities in the iron into the materials is prevented, so that the content of the iron in the metal strontium is not influenced.
The invention has the beneficial effects that the powdery strontium carbonate is added with water to be made into a brick shape, the size of the brick is 240 x 115 x 65mm, the strontium carbonate brick is arranged on a special kiln car and is stacked according to certain size and interval requirements, after preheating and drying, the moisture of the strontium carbonate brick entering a tunnel kiln is controlled to be below 5 percent, the calcination temperature is controlled to be about 1400 ℃, and the content of the calcined strontium oxide reaches above 97 percent. The process has wide requirement on the grain size of the strontium carbonate for making bricks, and can reduce the cost of raw materials.
The technical solutions provided by the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained herein by using specific examples, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, for a person skilled in the art, according to the embodiments of the present invention, there may be variations in the specific implementation manners and application ranges, and in summary, the content of the present description should not be construed as a limitation to the present invention.
Claims (8)
1. A preparation method of high-purity metal strontium is characterized by comprising the following steps: the method adopts powdery strontium carbonate as a raw material and comprises the following steps:
firstly, adding water into powdery strontium carbonate to prepare a brick-shaped blank, drying the brick-shaped blank, and then calcining the dried brick-shaped blank in calcining equipment to obtain brick-shaped strontium oxide;
secondly, after the brick-shaped strontium oxide enters a crusher to be crushed, screening and grading the brick-shaped strontium oxide and storing the brick-shaped strontium oxide in a strontium oxide storage tank;
thirdly, adding aluminum particles into the screened strontium oxide, uniformly mixing, pressing into oblate spheres by a ball making machine, and then selecting oblate mixture with a preset particle size and filling the mixture into a charging bucket to enter a reduction tank;
fourthly, under the vacuum condition, the strontium oxide is reduced into metal strontium by aluminum;
fifthly, cooling the metal strontium in a 5N argon environment;
and sixthly, forming and packaging to obtain the high-purity metal strontium product.
2. The method for preparing high-purity strontium metal according to claim 1, wherein the method comprises the following steps: the calcining equipment is a tunnel kiln, the brick-shaped strontium carbonate before entering the tunnel kiln is dried, the moisture content is less than 5%, the calcining temperature in the tunnel kiln is 1400 +/-20 ℃, the calcining time is 12-15 h, and the content of the calcined strontium oxide is more than or equal to 97%.
3. The method for preparing high-purity strontium metal according to claim 1, wherein the method comprises the following steps: the brick-shaped blank has the size of 200-250 mm 100-150 mm 50-80 mm.
4. The method for preparing high-purity strontium metal according to claim 1, wherein the method comprises the following steps: the mixing ratio of the strontium oxide to the aluminum particles is 100: 15-100: 17.
5. The method for preparing high-purity strontium metal according to claim 1, wherein the method comprises the following steps: the vacuum degree of a reduction tank for reducing strontium oxide is 2-8 Pa, the reaction temperature is 1230-1260 ℃, and the reaction time is 18-24 h.
6. The method for preparing high-purity strontium metal according to claim 1, wherein the method comprises the following steps: the grain diameter of the aluminum particles added in the third step is 20-100 meshes, and the grain diameter of the pressed oblate mixed material is more than or equal to 10 mm.
7. The method for preparing high-purity strontium metal according to claim 1, wherein the method comprises the following steps: the equipment contacted with the strontium carbonate, the strontium oxide, the oblate mixture and the metal strontium is made of stainless steel.
8. A high purity strontium metal produced by the process of claim 1, wherein: the mass percent of the purity of the product is higher than 99.9%, and the mass percent of other impurities is as follows: fe is less than or equal to 0.001 percent, Mg is less than or equal to 0.003 percent, Ca is less than or equal to 0.04 percent, Ba is less than or equal to 0.05 percent, and the total content of other impurities is less than or equal to 0.006 percent.
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Application publication date: 20210611 |