CN108018435A - 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 PDFInfo
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- CN108018435A CN108018435A CN201711166131.7A CN201711166131A CN108018435A CN 108018435 A CN108018435 A CN 108018435A CN 201711166131 A CN201711166131 A CN 201711166131A CN 108018435 A CN108018435 A CN 108018435A
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- Y—GENERAL 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses the preparation method of a kind of high pure metal rubidium and caesium, comprise the following steps：(1) the pre- heat dehydration of rubidium cesium compound；(2) once reduction obtains metal caesium and once reduces 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) will once reduce 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) by metal caesium, the isolated vacuum distillation product of metal rubidium vacuum distillation and vinasse；(6) rectifying product twice and high pure metal rubidium will be obtained after vacuum distillation product under an inert atmosphere rectifying twice.The rubidium cesium compound of mixing of the method for the present invention especially suitable for being mixed from rubidium caesium separates and recovers to obtain high pure metal rubidium and high pure metal caesium.
Description
Technical field
The invention belongs to non-ferrous metal preparation field, more particularly to the preparation method of a kind of metal rubidium and caesium.
Background technology
Yichuan possesses the lepidolite ore of Fia, it contains abundant lithium, rubidium, caesium, potassium, sodium etc., not only Li2O
Content up to more than 4.5%, rubidium, the content of caesium are also up to 1.5% or so, and 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 obtain energy and be escaped from metal surface and produce 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, there is larger development in the past 10 years.In addition, at some
New application field, particularly in some high-tech areas, also show more and more important effect, 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.
At present, the application of developed country's caesium and rubidium is concentrated mainly on high-tech area, and the rubidium and 70% caesium for having 80% are used
In exploitation new and high technology, only 20% rubidium and 30% caesium are used for traditional application field.Since world energy sources is increasingly in short supply, people
All seeking new energy transformation method, with improve efficiency and save fuel, reduce environmental pollution.Caesium and rubidium turn in new energy
Application in changing shows the prospect of light, and causes gazing at for world energy sources circle.
At present, 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 reduce 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-state ore deposit such as pollucite, lepidolite, its extraction process is more multiple
Miscellaneous, of high cost, energy consumption is big.In addition, the rubidium cesium compound of the mixing mixed for rubidium caesium does not separate and recover well
The method of rubidium and caesium.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, there is provided a kind of
The rubidium cesium compound of mixing especially suitable for being mixed 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 is：
A kind of preparation method of high pure metal rubidium and caesium, 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, be heated under an inert atmosphere
500-560 DEG C of reduction obtains metal caesium and once reduces residue；
(3) the metal caesium obtained in step (2) is obtained once smart 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, the secondary fine that will be obtained in the once reduction residue obtained in step (2) and step (3)
Evaporate residue and be 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 reducing rubidium in step (2), using the reduction of higher
Temperature adds more reducing agents, to improve total recovery；
(5) it is the 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) the 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 is to be based on following principle：Rubidium cesium compound proportional difference mainly is utilized in step (2), and
Reducing agent reduces 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, make full use of the boiling range difference of rubidium, caesium, remove can obtain after impurity rubidium, magnesium it is high-purity
Metal caesium.Once reduction residue in step (2) in a rectification residue in step (3), secondary rectification residue with also containing
More rubidium and caesium, metal caesium, metal rubidium steam can be obtained by being reduced after it is mixed with secondary reduction agent, be recycled 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 to step (2) after distillation, recycles rubidium, the boiling range difference of caesium, gold
Belong to rubidium to carry out that after two stage rectification removes impurity high pure metal caesium can be obtained again.
In above-mentioned preparation method, it is preferred that a reducing agent be calcium, magnesium, barium, zirconium, aluminium and lithium in one kind or
Several, the secondary reduction agent is the one or more in calcium, zirconium, aluminium, silicon, lithium, sodium and potassium, and used in reduction process twice
To the species of reducing agent differ.Found by studying, partial reduction agent is only reacted with caesium, or is more likely to anti-with caesium
Should, in the present invention reducing agent and the selection of secondary reduction agent have large effect to experimental result, when reducing agent is chosen
Choose suitable reducing agent.
In above-mentioned preparation method, it is preferred that the dosage of a reducing agent in order to 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 in order to control the mixing residue with it is secondary
The molar ratio of reducing agent is 0.55-0.75：1.The dosage difference of reducing agent and secondary reduction agent can be with ingenious elder generation 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
Into steam, make 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 extracted from lepidolite ore rubidium chloride,
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 in thing, rubidium sulfate cesium compound and acetic acid rubidium cesium compound, and contain caesium at the same time 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 higher than rubidium to ensure once to reduce when utilize rubidium cesium compound proportional difference, and reducing agent 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), it is 5 × 10 that when vacuum, which controls 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 to step (1) twice
Physics and chemistry compound.Single flash raffinate and rectifying product return to step (2) twice can be returned further as pre-treatment compound
Receive using single flash raffinate and kish caesium rubidium in rectifying product twice, further to lift comprehensive recovery.
Compared with prior art, the advantage of the invention is that：
1st, preparation method of the present invention can be used for the processing rubidium cesium compound containing caesium and rubidium at the same time, because metal rubidium caesium fusing point,
Boiling point and property are similar, extremely difficult under normal temperature and pressure to be separated, and chemistry is combined with Physical by the present invention, step by step to caesium with
Rubidium is reduced, 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 simple metal rubidium and caesium.
2nd, the method for the present invention have technique simple, 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 the metal rubidium finally obtained up to more than 99.98%, the purity of gained metal caesium can
To more than 99.99%, comprehensive recovery can meet the requirement that Alkali Metal Rb caesium is directly prepared under the conditions of heat-treating up to 96%.
3rd, applicable raw materials scope 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
Ji benefit higher.
4th, raw material needed for the present invention has the excellent properties such as performance is stable and environmental-friendly, before having good commercial Application
Scape.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, drawings in the following description are 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.
Embodiment
For the ease of understanding the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood implication 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 domain.
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.
The high-purity rubidium cesium salt used in following embodiments extracts gained from the tantalum niobium lithium ore deposit lepidolite that Yichuan produces,
Reducing agent is high-purity level, and each component 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, comprises the following steps：
(1) sample A01 is placed in vacuum reactor, handles and be dehydrated through low-temperature prewarming, it is 200 DEG C to control dehydration temperaturre,
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 dispensing, then in argon atmosphere vacuum glove box be uniformly mixed, cake of press and dress sample；
(3) high temperature reduction：The all product that fill obtained in step (2) are placed in stainless copper reactor, then by reactor
Sealing, is evacuated to -0.025~0.03MPa, and it is 0.45~0.50MPa to then pass to inert gas to reactor, this operation weight
It is multiple three times, to ensure gas atmosphere as inertia, then 600 DEG C are warming up to 5 DEG C/min, with 1.5 DEG C/min liters after constant temperature 30min
Temperature makes metal rubidium form metallic vapour to 800~805 DEG C；
(4) high pure metal rubidium is prepared：After the metallic vapour obtained in step (3) is cooled down, send into rectifying reactor, control
Temperature processed is 700~750 DEG C, and the metal rubidium steam obtained by rectifying is sent into rectifying reactor again after cooling, control temperature
To spend for 680~700 DEG C, 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) is prepared as metal rubidium；
(5) pack：The high pure metal rubidium that final rectifying goes out is cooled to 60 DEG C or so, sampling analysis, product is qualified to carry out
Vacuum packaging.
Embodiment 2：
A kind of preparation method of high pure metal caesium, comprises the following steps：
(1) sample A02 is placed in vacuum reactor, handles and be dehydrated through low-temperature prewarming, it is 200 DEG C to control dehydration temperaturre,
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 dispensing, then in argon atmosphere vacuum glove box be uniformly mixed, cake of press and dress sample；
(3) high temperature reduction：The all product that fill obtained in step (2) are placed in stainless copper reactor, then by reactor
Sealing, is evacuated to -0.02~0.025MPa, and it is 0.45~0.50MPa to then pass to inert gas to reactor, this operation weight
It is multiple three times, to ensure gas atmosphere as inertia, then 300 DEG C are warming up to 5 DEG C/min, with 1.0 DEG C/min liters after constant temperature 30min
Temperature makes metal caesium form metallic vapour to 555~560 DEG C；
(4) high pure metal caesium is prepared：After the metallic vapour obtained in step (3) is cooled down, send into rectifying reactor, control
Temperature processed is 545~550 DEG C, and the metal caesium steam obtained by rectifying is sent into rectifying reactor again after cooling, control temperature
To spend for 495~500 DEG C, 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) is prepared as metal caesium；
(5) pack：The high pure metal caesium that final rectifying goes out is cooled to 60 DEG C or so, sampling analysis, product is qualified to carry out
Vacuum packaging.
Embodiment 3：
As shown in Figure 1, the preparation method of a kind of high pure metal rubidium and caesium, comprises the following steps：
(1) sample A03 is placed in vacuum reactor, handles and be dehydrated through low-temperature prewarming, it is 200 DEG C to control dehydration temperaturre,
Time is 120min, obtains pre-treatment compound；
(2) material is blended：By pre-treatment compound A03 and a reducing agent magnesium metal stoichiometrically 1.55:1 matches somebody with somebody
Expect, then uniformly mixed, cake of press and dress sample in argon atmosphere vacuum glove box；
(3) high temperature reductions：The all product that fill obtained in step (2) are placed in stainless copper reactor, then will be anti-
Answer device to seal, be evacuated to -0.025~0.03MPa, it is 0.35~0.45MPa to then pass to inert gas to reactor, this behaviour
Make in triplicate, to ensure gas atmosphere as inertia, be 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, metal caesium is formed metallic vapour and is once reduced residue；
(4) high pure metal caesium is prepared：By the metallic vapour obtained in step (3) cool down after, send into rectifying reactor into
Rectifying of row, controlled at 545~550 DEG C, the metal caesium steam obtained by rectifying is sent again after cooling anti-to rectifying
Answer and secondary rectifying is carried out 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 reduces：It is once smart by what is obtained in the once reduction residue obtained in step (3) and step (4)
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
Measure ratio 0.6:0.8:0.15:0.05 mixing, 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 set to form metallic vapour and secondary reduction residue；
(6) it is evaporated in vacuo：By the metallic vapour obtained in step (5) vacuum be 6 × 10-3Pa, temperature for 255~
The isolated vacuum distillation product metal rubidium of space vacuum distillation and vinasse at 265 DEG C；
(7) high pure metal rubidium is prepared：After the vacuum distillation product metal rubidium obtained in step (6) is cooled down, send to rectifying
In reactor, controlled at 670~700 DEG C, the metal rubidium steam obtained by rectifying is sent to rectification process again after cooling
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 to step (2) is used as raw material；
(8) pack：High pure metal caesium that final rectifying goes out and high pure metal rubidium are 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, comprises the following steps：
(1) sample A04 is placed in vacuum reactor, handles and be dehydrated through low-temperature prewarming, it is 200 DEG C to control dehydration temperaturre,
Time is 120min, obtains pre-treatment compound；
(2) material is blended：By pre-treatment compound A04 and a reducing agent magnesium metal stoichiometrically 1.25:1 matches somebody with somebody
Expect, then uniformly mixed, cake of press and dress sample in argon atmosphere vacuum glove box；
(3) high temperature reductions：The all product that fill obtained in step (2) are placed in stainless copper reactor, then will be anti-
Answer device to seal, be evacuated to -0.025~0.03MPa, it is 0.35~0.45MPa to then pass to inert gas to reactor, this behaviour
Make in triplicate, to ensure gas atmosphere as inertia, be 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, metal caesium is formed metallic vapour and is once reduced residue；
(4) high pure metal caesium is prepared：By the metallic vapour obtained in step (3) cool down after, send into rectifying reactor into
Rectifying of row, controlled at 545~550 DEG C, the metal caesium steam obtained by rectifying is sent again after cooling anti-to rectifying
Answer and secondary rectifying is carried out 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 reduces：It is once smart by what is obtained in the once reduction residue obtained in step (3) and step (4)
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
Measure ratio 0.8:0.9:0.05:0.05 mixing, 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 set to form metallic vapour and secondary reduction residue；
(6) it is evaporated in vacuo：By the metallic vapour obtained in step (5) vacuum be 6 × 10-3Pa, temperature for 265~
The isolated vacuum distillation product metal rubidium of space vacuum distillation and vinasse at 275 DEG C；
(7) high pure metal rubidium is prepared：After the vacuum distillation product metal rubidium obtained in step (6) is cooled down, send to rectifying
In reactor, controlled at 750~710 DEG C, the metal rubidium steam obtained by rectifying is sent to rectification process again after cooling
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 to step (2) is used as raw material；
(8) pack：High pure metal caesium that final rectifying goes out and high pure metal rubidium are 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 of the high pure metal rubidium that the present embodiment is prepared and high pure metal caesium is high, and the rate of recovery
Also 96% is up to, the method for the present embodiment has broad application prospects.
Claims (9)
1. the preparation method of a kind of high pure metal rubidium and caesium, it is characterised in that comprise 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 once reduce residue；
(3) the metal caesium obtained in step (2) is obtained into rectifying production under an inert atmosphere in a 500-500 DEG C of rectifying
Thing and a rectification residue, then a rectifying product is obtained into high pure metal in 450-500 DEG C of secondary rectifying under an inert atmosphere
Caesium and secondary rectification residue；
(4) it is the once reduction residue obtained in step (2) and a rectification residue being obtained in step (3), secondary rectifying 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) the 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) the 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 according to claim 1 and caesium a, it is characterised in that reducing agent is
One or more in 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 species of reducing agent used in reduction process twice differs.
3. the preparation method of high pure metal rubidium according to claim 2 and caesium a, it is characterised in that reducing agent
The molar ratio of the pre-treatment compound and a reducing agent is 1.25-1.55 to dosage in order to control：1, the secondary reduction agent
The mixing residue and the molar ratio of secondary reduction agent are 0.55-0.75 to dosage in order to control：1.
4. the preparation method of high pure metal rubidium according to any one of claim 1-3 and caesium, it is characterised in that the rubidium
Cesium compound is rubidium chloride, cesium chloride, rubidium carbonate, cesium carbonate, acetic acid rubidium, cesium acetate, the sulphur extracted from lepidolite ore
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 at the same time.
5. the preparation method of high pure metal rubidium according to claim 4 and caesium, it is characterised in that in the rubidium cesium compound
The content of caesium is higher than rubidium.
6. the preparation method of high pure metal rubidium according to any one of claim 1-3 and caesium, it is characterised 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 according to any one of claim 1-3 and caesium, it is characterised in that 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 according to any one of claim 1-3 and caesium, it is characterised in that the step
Suddenly in (5), it is 5 × 10 that when vacuum, which controls vacuum,-3~6 × 10-3Pa。
9. the preparation method of high pure metal rubidium according to any one of claim 1-3 and caesium, it is characterised in that the steaming
Evaporate raffinate and be used as pre-treatment compound with rectifying product return to step (2) twice.
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| CN108796244A (en) * | 2018-06-13 | 2018-11-13 | 中南大学 | A kind of method that one step of metal calciothermic reduction prepares high-purity rubidium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108796244A (en) * | 2018-06-13 | 2018-11-13 | 中南大学 | A kind of method that one step of metal calciothermic reduction prepares high-purity rubidium |
| CN108796244B (en) * | 2018-06-13 | 2020-01-10 | 中南大学 | Method for preparing high-purity rubidium by one-step thermal reduction of metal calcium |
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| CN108018435B (en) | 2019-08-09 |
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