CN108018435B - A kind of preparation method of high pure metal rubidium and caesium - Google Patents

A kind of preparation method of high pure metal rubidium and caesium Download PDF

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CN108018435B
CN108018435B CN201711166131.7A CN201711166131A CN108018435B CN 108018435 B CN108018435 B CN 108018435B CN 201711166131 A CN201711166131 A CN 201711166131A CN 108018435 B CN108018435 B CN 108018435B
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rubidium
caesium
high pure
metal
rectifying
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CN201711166131.7A
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CN108018435A (en
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姚胜兰
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湖南中大技术创业孵化器有限公司
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Process efficiency
    • Y02P10/21Process efficiency by recovering materials
    • Y02P10/212Recovering metals from waste
    • Y02P10/234Recovering metals from waste by hydro metallurgy

Abstract

The invention discloses the preparation methods of a kind of high pure metal rubidium and caesium, comprising the following steps: (1) the pre- heat dehydration of rubidium cesium compound;(2) primary reduction obtains metal caesium and primary reduction residue;(3) by the rectifying under an inert atmosphere of metal caesium, a rectifying product and a rectification residue are obtained, then secondary rectifying obtains high pure metal caesium and secondary rectification residue under an inert atmosphere by a rectifying product;(4) it will once restore residue, a rectification residue, secondary rectification residue to mix and mix with secondary reduction agent again, secondary reduction obtains metal caesium, metal rubidium and secondary reduction residue;(5) isolated vacuum distillation product and vinasse is evaporated in vacuo in metal caesium, metal rubidium;(6) rectifying product twice and high pure metal rubidium will be obtained after vacuum distillation product under an inert atmosphere rectifying twice.The method of the present invention separates and recovers to obtain high pure metal rubidium and high pure metal caesium especially suitable for the mixed rubidium cesium compound mixed from rubidium caesium.

Description

A kind of preparation method of high pure metal rubidium and caesium

Technical field

The invention belongs to non-ferrous metal preparation field more particularly to a kind of preparation methods of metal rubidium and caesium.

Background technique

Yichuan possesses the lepidolite ore of Fia, lithium rich in, rubidium, caesium, potassium, sodium etc., not only Li2O Content up to 4.5% or more, rubidium, caesium content be also up to 1.5% or so, comprehensive development and utilization is carried out to it to be had very Important Economic and strategic value.

People have found the important properties of caesium and rubidium at first, are because they are the metals of " long eyes " --- have excellent Photoelectric properties.Due to there is the very strong free electron of activity in the crystal of alkali metal, thus they have good electric conductivity, Thermal conductivity, under the action of certain wavelength light, the free electron of caesium and rubidium can get energy and escape from metal surface and generate light Electrical effect.

Since caesium and rubidium have unique property, this makes them have important purposes in different field.Such as electronics device The traditional fields such as part, catalyst, special glass, biochemistry and medicine have biggish development in the past 10 years.In addition, some New application field also shows increasingly important role especially in some high-tech areas, as magnetic fluid is sent out Electricity, thermion conversion power generation, ion propulsion rocket, laser converting electrical energy device, the communication of cesium ion cloud etc., caesium and rubidium are shown Powerful vitality.

Currently, the application of developed country's caesium and rubidium is concentrated mainly on high-tech area, there are 80% rubidium and 70% caesium to use In exploitation new and high technology, only 20% rubidium and 30% caesium are used for traditional application field.Since world energy sources are increasingly in short supply, people All seeking new energy transformation method, to improve efficiency and save fuel, reduce environmental pollution.Caesium and rubidium turn in new energy Application in changing shows bright prospect, and causes gazing at for world energy sources circle.

Currently, rubidium or cesium compound separating and extracting process mainly have the precipitation method, ion-exchange and solvent extraction etc..It is pure Metal rubidium can restore pollucite, lepidolite ore etc. with active metal, then be obtained with vacuum distillation.Other methods be heat chemistry also Former pure rubidium or cesium compound, according to following reaction:

2RbOH+Mg→Mg(OH)2+2Rb

Rb2CO3+3Mg→3MgO+C+2Rb

For the industrial base stock of rubidium, caesium mainly based on the solid-states mine such as pollucite, lepidolite, extraction process is more multiple Miscellaneous, at high cost, energy consumption is high.In addition, not separated and recovered well for the mixed rubidium cesium compound that rubidium caesium mixes The method of rubidium and caesium.

Summary of the invention

The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, one kind is provided Mixed rubidium cesium compound especially suitable for mixing from rubidium caesium separates and recovers to obtain high pure metal rubidium and high pure metal Caesium, in order to solve the above technical problems, technical solution proposed by the present invention are as follows:

A kind of preparation method of high pure metal rubidium and caesium, comprising the following steps:

(1) the pre- heat dehydration of rubidium cesium compound vacuum is obtained into pre-treatment compound;

(2) pre-treatment compound obtained in step (1) is mixed with a reducing agent, is heated under an inert atmosphere 500-560 DEG C of reduction obtains metal caesium and primary reduction residue;

(3) metal caesium obtained in step (2) is obtained into primary essence under an inert atmosphere in a 500-500 DEG C of rectifying Product and a rectification residue are evaporated, then a rectifying product is obtained in 450-500 DEG C of secondary rectifying under an inert atmosphere high-purity Metal caesium and secondary rectification residue;

(4) rectification residue, a secondary fine obtained in residue and step (3) will be once restored obtained in step (2) It evaporates residue and is mixed to get mixing residue, then mixing residue is mixed with secondary reduction agent, be heated to 750-850 under an inert atmosphere DEG C reduction obtains metal caesium, metal rubidium and secondary reduction residue;It is mainly used for restoring rubidium in step (4), using higher reduction Temperature adds more reducing agents, to improve total recovery;

(5) metal caesium obtained in step (4), metal rubidium is isolated in 250-300 DEG C of vacuum distillation in a vacuum Product and vinasse is evaporated in vacuo;

(6) vacuum distillation product obtained in step (5) is obtained after 650-750 DEG C twice rectifying under an inert atmosphere Rectifying product and high pure metal rubidium twice.

Above-mentioned preparation method be based on the principle that mainly using rubidium cesium compound proportional difference in step (2), and Reducing agent restores sex differernce to rubidium caesium, and by a low-temperature reduction, ingenious utilize first isolates the higher metal caesium steam of purity, Again by metal caesium steam through two stage rectification, the boiling range difference of rubidium, caesium is made full use of, it is available high-purity after removal impurity rubidium, magnesium Metal caesium.Primary reduction residue in step (2) in step (3) a rectification residue, also contain in secondary rectification residue More rubidium and caesium restores available metal caesium, metal rubidium steam after mixing it with secondary reduction agent, recycle true Rubidium highly volatile characteristic under empty, cryogenic conditions, by metal rubidium, metal caesium steam carry out cryogenic vacuum distillation can by metal rubidium, The isolated metal rubidium of metal caesium steam, the vinasse return step (2) after distillation recycle the boiling range difference of rubidium, caesium, gold Belong to rubidium and carries out available high pure metal rubidium after two stage rectification removal impurity again.

In above-mentioned preparation method, it is preferred that a reducing agent be one of calcium, magnesium, barium, zirconium, aluminium and lithium or Several, the secondary reduction agent is one or more of calcium, zirconium, aluminium, silicon, lithium, sodium and potassium, and used in reduction process twice The type of the reducing agent arrived is not identical.By the study found that partial reduction agent is only reacted with caesium, or it is more likely to anti-with caesium It answers, the selection of a reducing agent and secondary reduction agent has large effect to experimental result in the present invention, when reducing agent is chosen Choose suitable reducing agent.

In above-mentioned preparation method, it is preferred that the dosage of a reducing agent be control the pre-treatment compound with The molar ratio of reducing agent is 1.25-1.55:1, the dosage of the secondary reduction agent be control the mixing residue with it is secondary The molar ratio of reducing agent is 0.55-0.75:1.Reducing agent and the dosage difference of secondary reduction agent can be with ingenious elder generations from rubidium caesium The higher metal caesium steam of purity is isolated in compound.Make rubidium cesium salt excessive in reduction process, to keep the preferential shape of caesium At steam, makes reducing agent excessive during secondary reduction, keep rubidium caesium high-recovery.

In above-mentioned preparation method, it is preferred that the rubidium cesium compound be the rubidium chloride extracted from lepidolite ore, Cesium chloride, rubidium carbonate, cesium carbonate, acetic acid rubidium, cesium acetate, rubidium sulfate, cesium sulfate, rubidium chloride cesium compound, rubidium carbonate caesium chemical combination One or more of object, rubidium sulfate cesium compound and acetic acid rubidium cesium compound, and contain caesium simultaneously in the rubidium cesium compound And rubidium.

In above-mentioned preparation method, it is preferred that the content of caesium is higher than rubidium in the rubidium cesium compound.Caesium in rubidium cesium compound Content be higher than rubidium to guarantee once to restore when using rubidium cesium compound proportional difference and reducing agent it is poor to rubidium caesium reproducibility It is different, first isolate the higher metal caesium steam of purity.

In above-mentioned preparation method, it is preferred that the temperature of the pre- heat dehydration is 150-250 DEG C, time 60- 180min.Pre- heat dehydration can reduce influence of the moisture to preparation process in raw material.

In above-mentioned preparation method, it is preferred that when under the inert atmosphere, the pressure for controlling the inert atmosphere is 0.3-0.5MPa。

In above-mentioned preparation method, it is preferred that in the step (5), control vacuum degree is 5 × 10 when the vacuum-3~6 ×10-3Pa。

In above-mentioned preparation method, it is preferred that the vinasse is used as pre- place with rectifying product return step (1) twice Manage compound.Single flash raffinate, which is used as pre-treatment compound with rectifying product return step (2) twice, further to return It receives using single flash raffinate and kish caesium rubidium in rectifying product twice, further to promote comprehensive recovery.

Compared with the prior art, the advantages of the present invention are as follows:

1, preparation method of the present invention can be used for handling the rubidium cesium compound containing caesium and rubidium simultaneously, because metal rubidium caesium fusing point, Boiling point and property are similar, extremely difficult under normal temperature and pressure to be separated, and the present invention combines with physical method chemistry, step by step to caesium with Rubidium is restored, is distilled, and solving traditional extraction, complexing and coprecipitation cannot be from the isolated height of rubidium cesium compound of caesium and rubidium The problem of pure metal rubidium and caesium.

2, the method for the present invention have simple process, easy controlled operation, rubidium or the caesium rate of recovery are high, product purity is high, performance is stable, The excellent properties such as three-waste free discharge, for the purity of finally obtained metal rubidium up to 99.98% or more, the purity of gained metal caesium can To 99.99% or more, comprehensive recovery can meet the requirement that Alkali Metal Rb caesium is directly prepared under the conditions of heat-treating up to 96%.

3, applicable raw materials range of the present invention is wide, can industrialized production, greatly increase by-product value, improve rubidium in lepidolite Caesium utilization rate solves the bottleneck that current rubidium caesium salt-mixture is only used for traditional sulfuric acid industry, substantially increases resource utilization, warp Benefit of helping is higher.

4, raw material needed for the present invention has the excellent properties such as performance is stable and environmental-friendly, before having good industrial application Scape.

Detailed description of the invention

In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention Some embodiments for those of ordinary skill in the art without creative efforts, can also basis These attached drawings obtain other attached drawings.

Fig. 1 is the preparation technology flow chart of high pure metal of embodiment of the present invention rubidium and caesium.

Specific embodiment

To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.

Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention Protection scope.

Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city Field is commercially available or can be prepared by existing method.

High-purity rubidium cesium salt used in following embodiments extracts gained from the tantalum niobium lithium mine lepidolite that Yichuan produces, Reducing agent is high-purity grade, and each ingredient of raw and auxiliary material is shown in Table 1.

Table 1: raw and auxiliary material forms (wt.%)

Sample K Na Rb Cs Ca Li Fe Mn Ni Cl H2O A01 0.012 0.0025 70.26 0.0015 0.0005 0.0008 0.0006 0.0005 0.0004 29.15 0.51 A02 0.011 0.0028 0.0016 78.54 0.0004 0.0003 0.0004 0.0003 0.0002 20.95 0.49 A03 0.0012 0.0035 12.31 57.06 0.0015 0.0007 0.0002 0.0001 0.0001 20.32 10.32 A04 0.0009 0.0057 18.46 49.94 0.0012 0.0012 0.0007 0.0004 0.0005 20.97 10.65

Embodiment 1:

A kind of preparation method of high pure metal rubidium, comprising the following steps:

(1) sample A01 being placed in vacuum reactor, handles and is dehydrated through low-temperature prewarming, control dehydration temperaturre is 200 DEG C, Time is 120min, obtains pre-treatment compound;

(2) material is blended: by pre-treatment compound A01 and reducing agent magnesium metal, calcium, lithium stoichiometrically 0.75: 0.95:0.04:0.01 ingredient, then in argon atmosphere vacuum glove box be uniformly mixed, cake of press and dress sample;

(3) it high temperature reduction: is placed in all product are filled obtained in step (2) in stainless copper reactor, then by reactor Sealing, is evacuated to -0.025~0.03MPa, and then passing to inert gas to reactor is 0.45~0.50MPa, this operation weight It is multiple three times, to ensure that gas atmosphere as inertia, is then warming up to 600 DEG C with 5 DEG C/min, with 1.5 DEG C/min liter after constant temperature 30min Temperature makes metal rubidium form metallic vapour to 800~805 DEG C;

(4) it prepares high pure metal rubidium: after the cooling of metallic vapour obtained in step (3), sending into rectifying reactor, control Temperature processed is 700~750 DEG C, and the resulting metal rubidium steam of rectifying is sent into rectifying reactor again after cooling, control temperature Degree is 680~700 DEG C, and rectifying obtains high pure metal rubidium, wherein rectifying atmosphere is inert atmosphere twice, and rectification residue returns twice Return the raw material that step (2) are prepared as metal rubidium;

(5) it packs: the high pure metal rubidium that final rectifying goes out being cooled to 60 DEG C or so, sampling analysis, product qualification carries out Vacuum packaging.

Embodiment 2:

A kind of preparation method of high pure metal caesium, comprising the following steps:

(1) sample A02 being placed in vacuum reactor, handles and is dehydrated through low-temperature prewarming, control dehydration temperaturre is 200 DEG C, Time is 120min, obtains pre-treatment compound;

(2) material is blended: by pre-treatment compound A02 and reducing agent magnesium metal, calcium, lithium stoichiometrically 1.35: 0.90:0.06:0.04 ingredient, then in argon atmosphere vacuum glove box be uniformly mixed, cake of press and dress sample;

(3) it high temperature reduction: is placed in all product are filled obtained in step (2) in stainless copper reactor, then by reactor Sealing, is evacuated to -0.02~0.025MPa, and then passing to inert gas to reactor is 0.45~0.50MPa, this operation weight It is multiple three times, to ensure that gas atmosphere as inertia, is then warming up to 300 DEG C with 5 DEG C/min, with 1.0 DEG C/min liter after constant temperature 30min Temperature makes metal caesium form metallic vapour to 555~560 DEG C;

(4) it prepares high pure metal caesium: after the cooling of metallic vapour obtained in step (3), sending into rectifying reactor, control Temperature processed is 545~550 DEG C, and the resulting metal caesium steam of rectifying is sent into rectifying reactor again after cooling, control temperature Degree is 495~500 DEG C, and rectifying obtains high pure metal caesium, wherein rectifying atmosphere is inert atmosphere twice, and rectification residue returns twice Return the raw material that step (2) are prepared as metal caesium;

(5) it packs: the high pure metal caesium that final rectifying goes out being cooled to 60 DEG C or so, sampling analysis, product qualification carries out Vacuum packaging.

Embodiment 3:

As shown in Figure 1, a kind of preparation method of high pure metal rubidium and caesium, comprising the following steps:

(1) sample A03 being placed in vacuum reactor, handles and is dehydrated through low-temperature prewarming, control dehydration temperaturre is 200 DEG C, Time is 120min, obtains pre-treatment compound;

(2) material is blended: by pre-treatment compound A03, stoichiometrically 1.55:1 matches with a reducing agent magnesium metal Expect, then uniformly mixed, cake of press and dress sample in argon atmosphere vacuum glove box;

(3) high temperature reductions: being placed in all product are filled obtained in step (2) in stainless copper reactor, then will be anti- It answers device to seal, is evacuated to -0.025~0.03MPa, then passing to inert gas to reactor is 0.35~0.45MPa, this behaviour Make in triplicate, to ensure that gas atmosphere as inertia, is then warming up to 300 DEG C with 5 DEG C/min, after constant temperature 30min with 1.0 DEG C/ Min is warming up to 555~560 DEG C, and metal caesium is made to form metallic vapour and primary reduction residue;

(4) prepare high pure metal caesium: by metallic vapour obtained in step (3) it is cooling after, send into rectifying reactor into Rectifying of row is sent the resulting metal caesium steam of rectifying anti-to rectifying again after cooling controlled at 545~550 DEG C It answers and carries out secondary rectifying in device, controlled at 485~495 DEG C, rectifying obtains high pure metal caesium and a rectification residue, secondary Rectification residue, wherein rectifying atmosphere is inert atmosphere twice;

(5) secondary high-temperature restores: primary essence obtained in residue and step (4) will be once restored obtained in step (3) Evaporate residue, secondary rectification residue is mixed to get mixing residue, then by mixing residue with secondary reduction agent calcium, silicon, lithium based on chemistry Amount than 0.6:0.8:0.15:0.05 mix, then in argon atmosphere vacuum glove box be uniformly mixed, cake of press and dress sample, with Under the identical device of step (3) and atmosphere, 500 DEG C are warming up to 5 DEG C/min, is warming up to after constant temperature 30min with 1.5 DEG C/min 750~755 DEG C, metal rubidium, caesium is made to form metallic vapour and secondary reduction residue;

(6) be evaporated in vacuo: by metallic vapour obtained in step (5) vacuum degree be 6 × 10-3Pa, temperature be 255~ Isolated vacuum distillation product metal rubidium and vinasse is evaporated in vacuo in space at 265 DEG C;

(7) it prepares high pure metal rubidium: after vacuum distillation product metal rubidium cooling obtained in step (6), sending to rectifying In reactor, controlled at 670~700 DEG C, the resulting metal rubidium steam of rectifying is sent again after cooling to rectification process In device, controlled at 670~700 DEG C, rectifying obtains high pure metal rubidium, wherein rectifying atmosphere is inert atmosphere twice, twice Rectification residue return step (2) is used as raw material;

(8) it packs: high pure metal caesium and high pure metal rubidium that final rectifying goes out is cooled to 60 DEG C or so, sampling analysis, Product qualification is vacuum-packed.

Embodiment 4:

A kind of preparation method of high pure metal rubidium and caesium, comprising the following steps:

(1) sample A04 being placed in vacuum reactor, handles and is dehydrated through low-temperature prewarming, control dehydration temperaturre is 200 DEG C, Time is 120min, obtains pre-treatment compound;

(2) material is blended: by pre-treatment compound A04, stoichiometrically 1.25:1 matches with a reducing agent magnesium metal Expect, then uniformly mixed, cake of press and dress sample in argon atmosphere vacuum glove box;

(3) high temperature reductions: being placed in all product are filled obtained in step (2) in stainless copper reactor, then will be anti- It answers device to seal, is evacuated to -0.025~0.03MPa, then passing to inert gas to reactor is 0.35~0.45MPa, this behaviour Make in triplicate, to ensure that gas atmosphere as inertia, is then warming up to 300 DEG C with 5 DEG C/min, after constant temperature 30min with 1.0 DEG C/ Min is warming up to 545~555 DEG C, and metal caesium is made to form metallic vapour and primary reduction residue;

(4) prepare high pure metal caesium: by metallic vapour obtained in step (3) it is cooling after, send into rectifying reactor into Rectifying of row is sent the resulting metal caesium steam of rectifying anti-to rectifying again after cooling controlled at 545~550 DEG C It answers and carries out secondary rectifying in device, controlled at 485~495 DEG C, rectifying obtains high pure metal caesium and a rectification residue, secondary Rectification residue, wherein rectifying atmosphere is inert atmosphere twice;

(5) secondary high-temperature restores: primary essence obtained in residue and step (4) will be once restored obtained in step (3) Evaporate residue, secondary rectification residue is mixed to get mixing residue, then by mixing residue with secondary reduction agent calcium, silicon, lithium based on chemistry Amount than 0.8:0.9:0.05:0.05 mix, then in argon atmosphere vacuum glove box be uniformly mixed, cake of press and dress sample, with Under the identical device of step (3) and atmosphere, 600 DEG C are warming up to 5 DEG C/min, is warming up to after constant temperature 30min with 1.5 DEG C/min 800~805 DEG C, metal rubidium, caesium is made to form metallic vapour and secondary reduction residue;

(6) be evaporated in vacuo: by metallic vapour obtained in step (5) vacuum degree be 6 × 10-3Pa, temperature be 265~ Isolated vacuum distillation product metal rubidium and vinasse is evaporated in vacuo in space at 275 DEG C;

(7) it prepares high pure metal rubidium: after vacuum distillation product metal rubidium cooling obtained in step (6), sending to rectifying In reactor, controlled at 750~710 DEG C, the resulting metal rubidium steam of rectifying is sent again after cooling to rectification process In device, controlled at 750~710 DEG C, rectifying obtains high pure metal rubidium, wherein rectifying atmosphere is inert atmosphere twice, twice Rectification residue return step (2) is used as raw material;

(8) it packs: high pure metal caesium and high pure metal rubidium that final rectifying goes out is cooled to 60 DEG C or so, sampling analysis, Product qualification is vacuum-packed.

The product quality such as following table of metal recovery rate and obtained high pure metal rubidium and high pure metal caesium in embodiment 1-4 Shown in 2.

Table 2: high pure metal rubidium and the high pure metal caesium rate of recovery and product chemistry performance indicator (wt.%) in embodiment 1-4

As seen from the above table, the purity is high of the present embodiment is prepared high pure metal rubidium and high pure metal caesium, and the rate of recovery Also it is up to 96%, the method for the present embodiment has broad application prospects.

Claims (9)

1. a kind of preparation method of high pure metal rubidium and caesium, which comprises the following steps:
(1) the pre- heat dehydration of rubidium cesium compound vacuum is obtained into pre-treatment compound;
(2) pre-treatment compound obtained in step (1) is mixed with a reducing agent, is heated to 500- under an inert atmosphere 560 DEG C of reduction obtain metal caesium and primary reduction residue;
(3) metal caesium obtained in step (2) is obtained into rectifying production under an inert atmosphere in a 545-550 DEG C of rectifying Object and a rectification residue, then a rectifying product is obtained into high pure metal in 485-495 DEG C of secondary rectifying under an inert atmosphere Caesium and secondary rectification residue;
(4) primary reduction residue obtained in step (2) and a rectification residue, secondary rectifying obtained in step (3) is residual Slag is mixed to get mixing residue, then mixing residue is mixed with secondary reduction agent, is heated to 750-850 DEG C under an inert atmosphere also Original obtains metal caesium, metal rubidium and secondary reduction residue;
(5) metal caesium obtained in step (4), metal rubidium are once evaporated in vacuo in 250-300 DEG C in a vacuum isolated Product and vinasse is evaporated in vacuo;
(6) vacuum distillation product obtained in step (5) is obtained twice after 650-750 DEG C twice rectifying under an inert atmosphere Rectifying product and high pure metal rubidium.
2. the preparation method of high pure metal rubidium and caesium according to claim 1, which is characterized in that a reducing agent is One or more of calcium, magnesium, barium, zirconium, aluminium and lithium, the secondary reduction agent are one in calcium, zirconium, aluminium, silicon, lithium, sodium and potassium Kind is several, and the type of reducing agent used in reduction process twice is not identical.
3. the preparation method of high pure metal rubidium and caesium according to claim 2, which is characterized in that a reducing agent Dosage is that control the pre-treatment compound and the molar ratio of a reducing agent be 1.25-1.55:1, the secondary reduction agent Dosage is that control the molar ratio of the mixing residue and secondary reduction agent be 0.55-0.75:1.
4. the preparation method of high pure metal rubidium and caesium according to any one of claim 1-3, which is characterized in that the rubidium Cesium compound is the rubidium chloride extracted from lepidolite ore, cesium chloride, rubidium carbonate, cesium carbonate, acetic acid rubidium, cesium acetate, sulphur In sour rubidium, cesium sulfate, rubidium chloride cesium compound, rubidium carbonate cesium compound, rubidium sulfate cesium compound and acetic acid rubidium cesium compound One or more, and contain caesium and rubidium in the rubidium cesium compound simultaneously.
5. the preparation method of high pure metal rubidium and caesium according to claim 4, which is characterized in that in the rubidium cesium compound The content of caesium is higher than rubidium.
6. the preparation method of high pure metal rubidium and caesium according to any one of claim 1-3, which is characterized in that described pre- The temperature of heat dehydration is 150-250 DEG C, time 60-180min.
7. the preparation method of high pure metal rubidium and caesium according to any one of claim 1-3, which is characterized in that be in institute When stating under inert atmosphere, the pressure for controlling the inert atmosphere is 0.3-0.5MPa.
8. the preparation method of high pure metal rubidium and caesium according to any one of claim 1-3, which is characterized in that the step Suddenly in (5), control vacuum degree is 5 × 10 when the vacuum-3~6×10-3Pa。
9. the preparation method of high pure metal rubidium and caesium according to any one of claim 1-3, which is characterized in that the steaming It evaporates raffinate and is used as pre-treatment compound with rectifying product return step (2) twice.
CN201711166131.7A 2017-11-21 2017-11-21 A kind of preparation method of high pure metal rubidium and caesium CN108018435B (en)

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