CN103045861A - Extraction method of rubidium - Google Patents
Extraction method of rubidium Download PDFInfo
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- CN103045861A CN103045861A CN2013100106213A CN201310010621A CN103045861A CN 103045861 A CN103045861 A CN 103045861A CN 2013100106213 A CN2013100106213 A CN 2013100106213A CN 201310010621 A CN201310010621 A CN 201310010621A CN 103045861 A CN103045861 A CN 103045861A
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- rubidium
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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
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Abstract
The invention discloses an extraction method of rubidium, which comprises the steps of raw material treatment, alkali leaching, extraction and back extraction. The method specifically comprises the following steps: taking the raw material rubidium-containing feldspar, and pulverizing for later use; adding an alkaline solution of which the liquid-to-solid ratio is 1-6 into the treated raw material, mixing, and adding the mixture into a pressurized reaction kettle to carry out reaction to form a slurry, and filtering, wherein the filter residue is used as the raw material for producing cement, and the filtrate is for later use; adding an extractant t-BAMBP of which the volume ratio is 1-5 into the filtrate to carry out extraction, thereby obtaining a rubidium-carried organic phase; and adding HCl of which the volume ratio is 1-8 into the rubidium-carried organic phase to carry out back extraction, thereby obtaining rubidium chloride. By carrying out alkaline leaching on the raw material rubidium-containing feldspar in the pressurized reaction kettle, the invention can obviously enhance the leaching rate of rubidium (up to higher than 98%), has the advantage of short reaction time (min 0.5 hour), and provides conditions for comprehensive utilization of rubidium-containing feldspar.
Description
Technical field
The invention belongs to the non-ferrous metal metallurgy technical field, be specifically related to a kind of extracting method of rubidium.
Background technology
Rubidium is very important rare noble metal resource, important in inhibiting on economy, strategy.It has important purposes in the traditional field such as electron device, photocell, catalyzer, special glass, biological chemistry and medicine, and in some high-tech areas, such as aspects such as magnetohydrodynamic generator, thermion conversion power generation, ion propulsion rocket, laser converting electrical energy devices, also demonstrated more and more important effect.The thermoelectric generator of particularly making of rubidium, as with the reactor coupling, can realize the thermion thermonuclear power generation in the inside of reactor.
Various resources relatively deficient today in the world, rubidium is expanded its range of application as a kind of metal of containing relative affluent resources, improves its utilization of resources and is worth, and has important practical significance.On the earth's crust, rubidium rich in mineral resources, elemental abundance are arranged and are occupied the 16th.But rubidium seldom forms independently mineral or ore body, usually composes to exist in other mineral, and often coexists with various metals such as caesium, lithium, potassium.The world contains the rubidium resource and mainly comprises: lithionite, pollux, Cs lepidolite, natural carnallitite, potassium ore deposit, GEOTHERMAL WATER, salt lake brine and seawater etc.Some typical rubidium resource and content contain rubidium 3% such as potassium felspar sand in the potassium ore deposit, white mica 2.1%, biotite 4.1%, sylvite 0.2% etc.; Though and rubidium content is not high in seawater and the carnallitite, total reserves is large.
Current, the extracting method of rubidium mainly contains: the multiple rubidium techniques of carrying such as fractionation crystallization, the precipitator method, ion exchange method, solvent extration, these rubidium extracting method mostly are from containing the high bittern of rubidium amount, contain the rubidium lithionite or contain the rubidium pollux and extract rubidium, the occurrence form rubidium feldspar that contains wide, that reserves are larger also not being had a kind of preferably method.Therefore, develop a kind of method that can from contain the rubidium ore, effectively extract rubidium, be very important for the utilization of rubidium resource.
Summary of the invention
The object of the present invention is to provide a kind of extracting method of rubidium.
The object of the present invention is achieved like this, comprise that raw material is processed, alkali soaks,, extraction, back extraction step, specifically comprise:
A, raw material process: get raw material and contain the rubidium feldspar and pulverize for subsequent use;
B, alkali soak: insert in the compressive reaction still after the basic solution that adds liquid-solid ratio 1 ~ 6 in raw material after treatment mixes and react, form slip, filter, filter residue is as cement producting material, filtrate for later use;
C, extraction: the extraction agent t-BAMBP that filtrate adds volume ratio 1 ~ 5 extracts, and obtains the rubidium load organic phases;
D, back extraction: the HCl that adds volume ratio 1 ~ 8 in the rubidium load organic phases carries out back extraction and obtains rubidium chloride.
The present invention adopts the compressive reaction still that raw material is contained the rubidium feldspar to carry out alkaline leaching, can significantly improve the leaching yield of rubidium, and leaching yield reaches more than 98%, and the reaction times is short, and the shortest time is 0.5h, for the comprehensive utilization that contains the rubidium feldspar provides condition.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing, but never in any form the present invention is limited, and any conversion or replacement based on training centre of the present invention is done all belong to protection scope of the present invention.
The present invention includes that raw material is processed, alkali soaks, extraction, back extraction step, specifically comprise:
A, raw material process: get raw material and contain the rubidium feldspar and pulverize for subsequent use;
B, alkali soak: insert in the compressive reaction still after the basic solution that adds liquid-solid ratio 1 ~ 6 in raw material after treatment mixes and react, form slip, filter, filter residue is as cement producting material, filtrate for later use;
C, extraction: the extraction agent t-BAMBP that filtrate adds volume ratio 1 ~ 5 extracts, and obtains the rubidium load organic phases;
D, back extraction: the HCl that adds volume ratio 1 ~ 8 in the rubidium load organic phases carries out back extraction and obtains rubidium chloride.
Pulverizing in the described A step was 80 ~ 400 mesh sieves.
Described B step neutral and alkali solution is one or more of yellow soda ash, salt of wormwood, sodium hydroxide, potassium hydroxide.
Described basic solution concentration is 80 ~ 260g/L.
Compressive reaction still pressure is 0 ~ 3Mpa in the described B step, and temperature is 80 ~ 260 ℃.
The reaction times is 0.5 ~ 6h in the described B step.
The thinner of extraction agent t-BAMBP is dimethylbenzene in the described C step, and extraction phase is 1:10 ~ 10:1 than (O/A).
Extraction time is 1 ~ 10min in the described C step, and extraction progression is 1 ~ 10 grade.
The concentration of reverse-extraction agent HCl is 1 ~ 6mol/L in the described D step, and back extraction is compared (O/A) and is 1:1～10:1.
The back extraction time is 1 ~ 10min in the described D step, and back extraction progression is 1 ~ 7 grade.
The invention will be further described with embodiment for the below.
In all following embodiment, the raw material of use be domestic certain real estate contain rubidium feldspar, its chemical ingredients such as table 1.In the present invention leaching contains the used alkali lye of rubidium feldspar and prepares with analytical pure sodium hydroxide and analytical pure salt of wormwood.
The analysis of table 1 material composition
| Composition | SiO 2 | K 2O | Al 2O 3 | Na 2O | Fe 2O 3 | CaO | MgO | Rb 2O |
| Content/% | 58.64 | 12.11 | 13.24 | 6.32 | 0.67 | 1.02 | 0.64 | 0.2 |
Embodiment 1
Get sample ore 100 order 100g and 500ml 120g/L NaOH solution is sized mixing, then join in the compressive reaction still, temperature is 160 ℃, and the time is 1h.Filter after leaching, filter residue can be used as cement raw material, and filtrate contains Rb0.342g/L, and the leaching yield of rubidium reaches 84.79%.Above-mentioned filtrate is carried out solvent extraction, and extraction agent is that t-BAMBP and dimethylbenzene consumption are that 1:2, extraction phase are that 3min, extraction progression are 3 grades than (O/A) for 3:1, extraction time, and gained Rb load organic phases contains Rb0.21g/L; Percentage extraction is 92.23%.Adopt HCl to carry out back extraction the Rb load organic phases and obtain RbCl solution; The back extraction acid concentration is 2mol/L, and the back extraction time is 3min, and back extraction progression is that 3 grades, back extraction are compared (O/A) and are 7:1.Water-phase component is after the back extraction: Rb 2.45g/L.
Embodiment 2
Get 160 order sample ore 100g and 500ml160g/L NaOH solution is sized mixing, then join in the compressive reaction still, temperature is 180 ℃, and the time is 3h.Filter after leaching, filter residue can be used as cement raw material, and filtrate contains Rb0.356g/L, and the leaching yield of rubidium reaches 86.7 %.Above-mentioned filtrate is carried out solvent extraction, extraction agent is that t-BAMBP and dimethylbenzene consumption are that 1:2, extraction phase are that 5min, extraction progression are 5 grades than (O/A) for 7:1, extraction time, contain Rb 0.81g/L after the washing of gained Rb load organic phases, percentage extraction is 99.3%.To wash back loading Rb organic phase adopts HCl to carry out back extraction to obtain RbCl solution; The back extraction acid concentration is 5mol/L, and the back extraction time is 8min, and back extraction progression is that 5 grades, back extraction are compared (O/A) and are 3:1.Water-phase component is after the back extraction: Rb 4.53g/L.
Embodiment 3
Get 260 orders this sample ore 100g and 500ml NaOH+Na
2CO
3Mixed solution (NaOH and Na
2CO
3Mass ratio 1:1), concentration is that the solution of 180g/L is sized mixing, and then joins in the compressive reaction still, and temperature is 180 ℃, and the time is 4h.Filter after leaching, filter residue can be used as cement raw material, and filtrate contains Rb0.369g/L, and the leaching yield of rubidium reaches 91.02%.Above-mentioned filtrate is carried out solvent extraction, and extraction agent is that t-BAMBP and dimethylbenzene consumption are that 1:2, extraction phase are that 2min, extraction progression are 7 grades than (O/A) for 1:1, extraction time, and gained Rb load organic phases contains Rb 0.645g/L, and percentage extraction is 99.3%.Adopt HCl to carry out back extraction the Rb load organic phases and obtain RbCl solution; The back extraction acid concentration is 4mol/L, and the back extraction time is 5min, and back extraction progression is that 7 grades, back extraction are compared (O/A) and are 1:1.Water-phase component is after the back extraction: Rb 1.31g/L.
Embodiment 4
Get 320 orders this sample ore 260g and 500ml NaOH+K
2CO
3Mixed solution (NaOH and K
2CO
3Mass ratio 1:1), concentration is that the solution of 180g/L is sized mixing, and then joins in the compressive reaction still, and temperature is 180 ℃, and the time is 4h.Filter after leaching, filter residue can be used as cement raw material, and filtrate contains Rb 0.363g/L, and the leaching yield of rubidium reaches 90.47%.Above-mentioned filtrate is carried out solvent extraction, and extraction agent is that t-BAMBP and dimethylbenzene consumption are that 1:2, extraction phase are that 3min, extraction progression are 3 grades than (O/A) for 1:5, extraction time, and gained Rb load organic phases contains Rb3.27g/L, and percentage extraction is 91.03%.Adopt HCl to carry out back extraction the Rb load organic phases and obtain RbCl solution; The back extraction acid concentration is 2mol/L, and the back extraction time is 5min, and back extraction progression is that 3 grades, back extraction are compared (O/A) and are 1:3.Water-phase component is after the back extraction: Rb 7.35g/L.
Embodiment 5
Get 400 orders this sample ore 100g and 500ml NaOH solution, concentration is that the solution of 200g/L is sized mixing, and then joins in the compressive reaction still, and temperature is 240 ℃, and the time is 3h.Filter after leaching, filter residue can be used as cement raw material, and filtrate contains Rb0.374g/L, and the leaching yield of rubidium reaches 93.26%.Above-mentioned filtrate is carried out solvent extraction, and extraction agent is that t-BAMBP and dimethylbenzene consumption are that 1:2, extraction phase, get the Rb load organic phases and contain Rb 9.56g/L for 1:9, extraction time are that 5min, extraction progression are 5 grades than (O/A), and percentage extraction is 97.32%.Adopt HCl to carry out back extraction the Rb load organic phases and obtain RbCl solution; The back extraction acid concentration is 4mol/L, and the back extraction time is 3min, and back extraction progression is that 5 grades, back extraction are compared (O/A) and are 1:5.Water-phase component is after the back extraction: Rb 10.05g/L.
Embodiment 6
Get 320 orders this sample ore 100g and 500ml NaOH solution, concentration is that the solution of 240g/L is sized mixing, and then joins in the compressive reaction still, and temperature is 260 ℃, and the time is 4h.Filter after leaching, filter residue can be used as cement raw material, and filtrate contains Rb0.391g/L, and the leaching yield of rubidium reaches 97.62%.Above-mentioned filtrate is carried out solvent extraction, and extraction agent is that t-BAMBP and dimethylbenzene consumption are that 1:2, extraction phase, get the Rb load organic phases and contain Rb 7.58g/L for 1:7, extraction time are that 7min, extraction progression are 7 grades than (O/A), and percentage extraction is 97.67%.Adopt HCl to carry out back extraction the Rb load organic phases and obtain RbCl solution; The back extraction acid concentration is 5mol/L, and the back extraction time is 8min, and back extraction progression is that 7 grades, back extraction are compared (O/A) and are 1:7.Water-phase component is after the back extraction: Rb 5.83g/L.
Claims (10)
1. the extracting method of a rubidium is characterized in that comprising that raw material is processed, alkali soaks, extraction, back extraction step, specifically comprises:
A, raw material process: get raw material and contain the rubidium feldspar and pulverize for subsequent use;
B, alkali soak: add liquid-solid ratio and be to insert in the compressive reaction still after 1 ~ 6 basic solution mixes in raw material after treatment and react, form slip, filter, filter residue is as cement producting material, filtrate for later use;
C, extraction: it is that 1 ~ 5 extraction agent t-BAMBP extracts that filtrate adds volume ratio, obtains the rubidium load organic phases;
D, back extraction: in the rubidium load organic phases, add volume ratio and be 1 ~ 8 HCl and carry out back extraction and obtain rubidium chloride.
2. the extracting method of rubidium according to claim 1 is characterized in that pulverizing was 80 ~ 400 mesh sieves in the described A step.
3. the extracting method of rubidium according to claim 1 is characterized in that described B step neutral and alkali solution is one or more of yellow soda ash, salt of wormwood, sodium hydroxide, potassium hydroxide.
4. according to claim 1 or the extracting method of 3 described rubidiums, it is characterized in that described basic solution concentration is 80 ~ 260g/L.
5. the extracting method of rubidium according to claim 1 is characterized in that the compressive reaction still pressure described in the B step is 0 ~ 3Mpa, and temperature is 80 ~ 260 ℃.
6. the extracting method of rubidium according to claim 1 is characterized in that the reaction times described in the B step is 0.5 ~ 6h.
7. the extracting method of rubidium according to claim 1, the thinner that it is characterized in that the extraction agent t-BAMBP described in the C step is dimethylbenzene, extraction is in a ratio of 1:10 ~ 10:1.
8. the extracting method of rubidium according to claim 1 is characterized in that the extraction time described in the C step is 1 ~ 10min, and extraction progression is 1 ~ 10 grade.
9. the extracting method of rubidium according to claim 1 is characterized in that the concentration of the reverse-extraction agent HCl described in the D step is 1 ~ 6mol/L, and back extraction is in a ratio of 1:1 ~ 10:1.
10. the extracting method of rubidium according to claim 1 is characterized in that the back extraction time described in the D step is 1 ~ 10min, and back extraction progression is 1 ~ 7 grade.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103555969A (en) * | 2013-10-21 | 2014-02-05 | 昆明冶金研究院 | New potassium-sodium separation method |
| CN103966460A (en) * | 2013-02-01 | 2014-08-06 | 中国科学院广州地球化学研究所 | Roasting leaching treatment process for recovery of metal rubidium resources from copper sulfur tailings |
| CN104789800A (en) * | 2015-05-08 | 2015-07-22 | 中国科学院青海盐湖研究所 | Method for extracting rubidium from saline lake brine |
| CN104805311A (en) * | 2015-03-24 | 2015-07-29 | 中国地质科学院矿产综合利用研究所 | Method for extracting rubidium from rubidium-containing feldspar and co-producing silicon fertilizer |
| CN106086470A (en) * | 2016-06-12 | 2016-11-09 | 宋玉军 | A kind of method obtaining rubidium salt with Kaolin Tailings for raw material |
| CN108060301A (en) * | 2017-12-05 | 2018-05-22 | 北京科技大学 | A kind of method that rubidium and by-product active calcium silicate are extracted in the ore from rubidium |
| CN111439754A (en) * | 2020-05-22 | 2020-07-24 | 四川君和环保股份有限公司 | Comprehensive utilization method of mung bean rock |
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Patent Citations (1)
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| CN101612606A (en) * | 2008-06-25 | 2009-12-30 | 灵宝市金源矿业有限责任公司 | Method for comprehensively reclaming quartz vein polymetallic oxidized ore resources |
Non-Patent Citations (1)
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966460A (en) * | 2013-02-01 | 2014-08-06 | 中国科学院广州地球化学研究所 | Roasting leaching treatment process for recovery of metal rubidium resources from copper sulfur tailings |
| CN103555969A (en) * | 2013-10-21 | 2014-02-05 | 昆明冶金研究院 | New potassium-sodium separation method |
| CN103555969B (en) * | 2013-10-21 | 2015-06-24 | 昆明冶金研究院 | New potassium-sodium separation method |
| CN104805311A (en) * | 2015-03-24 | 2015-07-29 | 中国地质科学院矿产综合利用研究所 | Method for extracting rubidium from rubidium-containing feldspar and co-producing silicon fertilizer |
| CN104805311B (en) * | 2015-03-24 | 2017-01-04 | 中国地质科学院矿产综合利用研究所 | Method for extracting rubidium from rubidium-containing feldspar and co-producing silicon fertilizer |
| CN104789800A (en) * | 2015-05-08 | 2015-07-22 | 中国科学院青海盐湖研究所 | Method for extracting rubidium from saline lake brine |
| CN106086470A (en) * | 2016-06-12 | 2016-11-09 | 宋玉军 | A kind of method obtaining rubidium salt with Kaolin Tailings for raw material |
| CN106086470B (en) * | 2016-06-12 | 2017-12-22 | 宋玉军 | A kind of method that rubidium salt is obtained using Kaolin Tailings as raw material |
| CN108060301A (en) * | 2017-12-05 | 2018-05-22 | 北京科技大学 | A kind of method that rubidium and by-product active calcium silicate are extracted in the ore from rubidium |
| CN111439754A (en) * | 2020-05-22 | 2020-07-24 | 四川君和环保股份有限公司 | Comprehensive utilization method of mung bean rock |
| CN111439754B (en) * | 2020-05-22 | 2021-01-15 | 四川君和环保股份有限公司 | Comprehensive utilization method of mung bean rock |
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