CN1594616A - Primary vacuum reduction distillation production process by thermit process and metallic strontium - Google Patents
Primary vacuum reduction distillation production process by thermit process and metallic strontium Download PDFInfo
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- CN1594616A CN1594616A CN 200410041401 CN200410041401A CN1594616A CN 1594616 A CN1594616 A CN 1594616A CN 200410041401 CN200410041401 CN 200410041401 CN 200410041401 A CN200410041401 A CN 200410041401A CN 1594616 A CN1594616 A CN 1594616A
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Abstract
Aluminothermy one-time vacuum reduction distillation process used in industrialized production of high purity strontium is provided. Industrial strontium carbonate powder is used as material. After high temperature calcining and decomposition, SrO powder is obtained, then mixed with Al powder according to a certain mol ratio, then pelletized, suspended in vacuum tank and placed in reduction furnace. At last SrO is reduced to Sr by Al under a certain vacuum degree and high temperature, and distilled and purified. Purity of metal strontium is higher or equal to 99.7%, impurity of Ca lower or equal to 0.05%, Ba<=0.10%, Fe<=0.01%, and other impurity is lower or equal to 0.05%. The invention shortens the production cycle, needing only one time reduction and distillation, reduces the production cost.
Description
Technical field
The present invention relates to a kind of thermite reduction and distillation and purify and to produce the method for industrial high pure metal strontium and the Preparation of Metallic Strontium that obtains of method thus thereof, relate in particular to a kind of vacuum reducing distilling producing process of thermite process and Preparation of Metallic Strontium of Preparation of Metallic Strontium.
Technical background
At present, the industrial preparation method of Preparation of Metallic Strontium has two kinds of fused salt electrolysis process and vacuum aluminium powder hot reducing methods.Calcium, strontium, barium claim alkaline-earth metal together, rank II-A family element in the periodictable, and chemical property is close, and containing normal in the type of ore deposit at it is concomitant product, and regular meeting follows and takes other two elements formation impurity phases out of when extracting the one element, reduces the purity of extract.As the raw material SrCO that extracts Preparation of Metallic Strontium
3, the general carbonate impurity that all contains Ca, Ba, thermit reduction suitability for industrialized production Preparation of Metallic Strontium often adopts general industry SrCO
3Powder is made raw material, and it is cheap, but Ca, Ba foreign matter content are also higher, must take second distillation to purify when the industrial high pure metal strontium of production purity Sr＞99.6% and just can reach.Can produce industrial high-purity strontium with vacuum reducing distillation though adopt high-purity strontium carbonate to make raw material, cost of material is wanted high nearly four times, and the product price of production can not be accepted for market.Fused salt electrolysis process is produced and is adopted SrCl2 to make raw material; because the decomposition voltage of SrCl2 is higher slightly than KCl; and strontium solubleness in himself molten chloride is significantly higher than calcium metal; therefore; only should adopt contact cathode method and liquid alloy cathode method electrolysis SrCl2 to produce strontium and alloy thereof; the former can obtain to contain the strontium rod of strontium nearly 81%; again through remelting ingot casting under argon shield; can get the strontium ingot that purity reaches 97%-98%; the latter can only obtain the certain density strontium alloy (matrix metal is answered the less vapour pressure of tool and more low-melting strontium alloy) that contains, and needs to separate the strontium of purifying metals with vacuum distillation method again.China extensively adopts aluminium powder hot reducing method suitability for industrialized production Preparation of Metallic Strontium, it is to make raw material with industrial SrCO3 (purity 96%-97%) powder, make SrO in high-temperature calcination decomposition more than 1100 ℃, pulverize back and the mixed of aluminium powder by 2: 1 (mol), the group of pressure, under vacuum condition, in high temperature more than 850-1000 ℃, SrO is reduced into strontium by liquid aluminium, and formation strontium steam, enter that solidification and crystallization becomes the strontium piece in the water cooled condenser, reaction product Sr (AlO) 2 (solid-state) remains in slagging group reject in the agglomerate, and gained Preparation of Metallic Strontium purity reaches 99%, as the Preparation of Metallic Strontium of need acquisition purity 99.6%, must adopt distillation for the second time to purify and just can reach.
Summary of the invention
The present invention proposes a kind of vacuum reducing distilling producing process of thermite process and Preparation of Metallic Strontium of Preparation of Metallic Strontium of high-efficiency and low-cost.
The present invention adopts following technical scheme:
A kind of vacuum reducing distilling producing process of thermite process that is used for suitability for industrialized production industry high pure metal strontium:
The first step: adopt industrial Strontium carbonate powder powder to make raw material, decompose, make the SrO powder in 1100～1400 ℃ of high-temperature calcinations;
Second step: with the SrO powder: the Al powder is by (1.5～2.0): 1 mol ratio mixing is pressed into agglomerate;
The 3rd step: agglomerate is hung vacuum tank place reduction furnace, in (1～20) * 10
-1Mm H
2Under the hot conditions of O vacuum tightness and 1000～1450 ℃, making SrO is strontium and the distillation strontium of purifying metals by aluminium reducing.
By the Preparation of Metallic Strontium that aforesaid method makes, its purity is: Sr 〉=99.7%; Impurity Ca≤0.05%, Ba≤0.10%, Fe≤0.01%, other impurity summation≤0.05%.
Compared with prior art, the present invention has following advantage:
The present invention is based on following principle: the present invention is the thermodynamic property according to reaction system, in conjunction with Sr, Ca, the temperature variant difference of Ba vapour pressure, selects to determine reaction distillation temperature and vacuum condition.Under the vacuum technology condition of reduction reaction, from thermodynamics, its complexity is followed successively by Ca, Sr, Ba.Therefore in process of production, by control vacuum tightness and temperature of reaction the reduction reaction of SrO is carried out smoothly, and the reduction reaction of CaO is suppressed to some extent.On the other hand, the fusing point of Sr, Ca, Ba is respectively about 777,842 and 727 ℃, and atmospheric boiling point is respectively about 1382,1487 and 1897 ℃.In quite wide temperature range, its vapour pressure size is followed successively by Sr, Ca, Ba.As when the 1600K, according to calculating, the vapour pressure 5.04kPa of Ba, the vapour pressure 35.48kPa of Ca, the vapour pressure 86.70KPa of Sr, because Ba and Al easily form alloy, its vapour pressure also should descend to some extent.Therefore with regard to still-process, Sr relatively easily separates with Ba.Adopt vacuum state, not only help the reduction process of oxide compound, also reduced the boiling point of metal, help distillation.In the present invention, can select optimum matching, make the preferential fractionation by distillation of Sr, suppress the content of Ca, Ba impurity, improve the purity of Sr by optimizing processing parameters such as vacuum tightness and reaction distillation temperature.Facts have proved, can reach the component target that the present invention proposes fully.The present invention adopts a vacuum reducing of thermite process distillation purification manufacture high pure metal strontium, and have the following advantages compared with the production method that adopts second distillation to purify: (1) only need once reduce and distill purification, has shortened the production cycle, has improved production efficiency; (2) save energy consumption, labor hour and the tooling device loss of second distillation, greatly reduced production cost; (3) can save the facility investment that second distillation is purified.Experimental results show that: purity wiry 〉=99.7% that adopts the present invention to make, and compose direct-reading spectrometer (IRIS INTREPID) by the quality inspection station entirely by inductively coupled plasma and detect, the results are as follows: Ba0.09, Ca0.048, Fe0.006, Mg0.012, Na0.01, P0.0006, Sr99.8.
Embodiment
1 one kinds of vacuum reducing distilling producing process of thermite process that are used for suitability for industrialized production industry high pure metal strontium of embodiment:
The first step: adopt industrial Strontium carbonate powder powder to make raw material, decompose, make the SrO powder in 1100～1400 ℃ of high-temperature calcinations, it is the industrial Strontium carbonate powder powder of GB/T10660 that present embodiment adopts industrial Strontium carbonate powder powder, and calcining temperature is chosen as: 1350 ℃, and 1100 ℃, 1400 ℃, 1250 ℃ or 1186 ℃;
Second step: with the SrO powder: the Al powder is by (1.5～2.0): 1 mol ratio mixing, be pressed into agglomerate, in the present embodiment, with the SrO of mixing and the Al powder moulding stamper of packing into, with pressing machine it is pressed into hangable shape, for example: SrO can be become platform scale counterweight shape with the Al powder compression, the ratio of above-mentioned SrO and Al powder can be selected 1.5: 1,2.0: 1,1.65: 1,1.8: 1 or 1.95: 1;
The 3rd step: agglomerate is hung vacuum tank place reduction furnace, in (1～20) * 10
-1Mm H
2Under the hot conditions of O vacuum tightness and 1000～1450 ℃, making SrO is strontium and the distillation strontium of purifying metals by aluminium reducing, and SrO at first forms strontium steam by aluminium reducing the time, enter the condenser solidification and crystallization, grows up into the strontium piece, and present embodiment can be selected: 20 * 10
-1Mm H
2O vacuum tightness and 1000 ℃, 1 * 10
-1Mm H
2O vacuum tightness and 1450 ℃, 15 * 10
-1Mm H
2O vacuum tightness and 1130,8 * 10
-1Mm H
2O vacuum tightness and 1250 ℃, 12 * 10
-1Mm H
2O vacuum tightness and 1200 ℃, perhaps, 3 * 10
-1Mm H
2Carry out under the condition of O vacuum tightness and 1420 ℃;
Present embodiment also can be opened the vacuum tank condenser after the reduction distillation purification is finished, take out the strontium piece, and the sealing of running into tank applying argon gas is preserved.
The Preparation of Metallic Strontium that embodiment 2 is made by embodiment 1 described method, its purity is: Sr 〉=99.7%; Impurity Ca≤0.05%, Ba≤0.10%, Fe≤0.01%, other impurity summation≤0.05%.
Claims (3)
1, a kind of vacuum reducing distilling producing process of thermite process that is used for suitability for industrialized production industry high pure metal strontium is characterized in that:
The first step: adopt industrial Strontium carbonate powder powder to make raw material, decompose, make the SrO powder in 1100～1400 ℃ of high-temperature calcinations;
Second step: with the SrO powder: the Al powder is by (1.5～2.0): 1 mol ratio mixing is pressed into agglomerate;
The 3rd step: agglomerate is hung vacuum tank place reduction furnace, in (1～20) * 10
-1MmH
2Under the hot conditions of O vacuum tightness and 1000～1450 ℃, making SrO is strontium and the distillation strontium of purifying metals by aluminium reducing.
2, vacuum reducing distilling producing process of thermite process according to claim 1 is characterized in that opening the vacuum tank condenser after the reduction distillation purification is finished, and takes out the strontium piece, and the sealing of running into tank applying argon gas is preserved.
3, a kind of Preparation of Metallic Strontium that is made by claim 1 is characterized in that its purity is: Sr 〉=99.7%; Impurity Ca≤0.05%, Ba≤0.10%, Fe≤0.01%, other impurity summation≤0.05%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410041401 CN1594616A (en) | 2004-07-16 | 2004-07-16 | Primary vacuum reduction distillation production process by thermit process and metallic strontium |
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| CN 200410041401 CN1594616A (en) | 2004-07-16 | 2004-07-16 | Primary vacuum reduction distillation production process by thermit process and metallic strontium |
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| CN1594616A true CN1594616A (en) | 2005-03-16 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100398679C (en) * | 2006-04-17 | 2008-07-02 | 重庆大学 | Method of preparing Mg, Sr alloy by vacuum heat reduction |
| CN105063375A (en) * | 2015-09-02 | 2015-11-18 | 班辉 | Method for preparing high-purity metal rubidium cesium through vacuum thermal reduction |
| GB2532784A (en) * | 2014-11-28 | 2016-06-01 | Hugh D'arcy-Evans Donald | Reduction furnace method and apparatus |
| CN106702178A (en) * | 2016-11-21 | 2017-05-24 | 厦门稀纯材料科技有限公司 | Preparation method of high-purity metallic strontium and high-purity metallic strontium prepared through same |
| CN108070727A (en) * | 2016-11-15 | 2018-05-25 | 镇江市润州金山金属粉末厂 | A kind of preparation facilities of Preparation of Metallic Strontium |
| CN109022825A (en) * | 2018-07-12 | 2018-12-18 | 五台云海镁业有限公司 | A kind of high purity metal strontium and its preparation process |
| CN112941340A (en) * | 2021-01-28 | 2021-06-11 | 重庆庆龙新材料科技有限公司 | High-purity metal strontium and preparation method thereof |
-
2004
- 2004-07-16 CN CN 200410041401 patent/CN1594616A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100398679C (en) * | 2006-04-17 | 2008-07-02 | 重庆大学 | Method of preparing Mg, Sr alloy by vacuum heat reduction |
| GB2532784A (en) * | 2014-11-28 | 2016-06-01 | Hugh D'arcy-Evans Donald | Reduction furnace method and apparatus |
| CN105063375A (en) * | 2015-09-02 | 2015-11-18 | 班辉 | Method for preparing high-purity metal rubidium cesium through vacuum thermal reduction |
| CN105063375B (en) * | 2015-09-02 | 2017-06-23 | 班辉 | A kind of method of vacuum-thermal reduction mode high-purity metal caesium |
| CN108070727A (en) * | 2016-11-15 | 2018-05-25 | 镇江市润州金山金属粉末厂 | A kind of preparation facilities of Preparation of Metallic Strontium |
| CN106702178A (en) * | 2016-11-21 | 2017-05-24 | 厦门稀纯材料科技有限公司 | Preparation method of high-purity metallic strontium and high-purity metallic strontium prepared through same |
| CN109022825A (en) * | 2018-07-12 | 2018-12-18 | 五台云海镁业有限公司 | A kind of high purity metal strontium and its preparation process |
| CN112941340A (en) * | 2021-01-28 | 2021-06-11 | 重庆庆龙新材料科技有限公司 | High-purity metal strontium and preparation method thereof |
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