CN108677006A - A method of extracting rubidium chloride from Kaolin Tailings - Google Patents
A method of extracting rubidium chloride from Kaolin Tailings Download PDFInfo
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- CN108677006A CN108677006A CN201810587165.1A CN201810587165A CN108677006A CN 108677006 A CN108677006 A CN 108677006A CN 201810587165 A CN201810587165 A CN 201810587165A CN 108677006 A CN108677006 A CN 108677006A
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/262—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds using alcohols or phenols
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The method that the invention discloses a kind of to extract rubidium chloride from Kaolin Tailings, Kaolin Tailings progress mill is crushed first, be sieved, obtains kaolin mineral fine, kaolin mineral fine is uniformly mixed with leaching agent, uniformly mixed powder is poured into the acid solution heated in advance, Ore Leaching is carried out, acid leaching liquor is obtained.Obtained leachate is adjusted into pH close to neutrality, deliming is then carried out, obtains the leachate containing rubidium.It is extracted using 4 tertiary butyl 2 (α methylbenzyls) phenol solutions after adding sulfonated kerosene to dilute, carries out the technique such as being stripped using hydrochloric acid solution, obtain thick rubidium product salt, the rubidium product salt of high-purity is dissolved, be recrystallized to give to it.The present invention provides a kind of rubidium salt extraction process of non-chlorinated roasting, simple and practicable, the at low cost, green non-pollution with technical process is suitable for industrialized advantage.
Description
Technical field
The invention belongs to mineral to purify field, and in particular to a method of extracting rubidium chloride from Kaolin Tailings.
Background technology
Since rubidium has unique performance so that its is widely used, and accounts for critical role in national economy, either exists
Traditional field, or all play an important role in new application field, the effect especially in high-tech area is more
Obviously.In traditional field, such as catalyst, special glass, electronic device, biomaterial field, there is larger hair in recent years
Exhibition.In frontier, such as rubidium atomic clock, magnetohydrodynamic generator, energy field, even more show powerful vitality.Currently,
In developed country, rubidium reaches 80% for the accounting of high frontier, and rubidium is 20% for traditional field accounting.Rubidium is manufacture electronics
Device (photomultiplier, photoelectric tube), spectrophotometer, automatically control, spectroscopic assay, color film, color TV, radar,
The important source material of laser and glass, ceramics, electronic clock etc.；In terms of space technology, ion propeller and thermion can turn
Parallel operation needs a large amount of rubidium；The hydroxide and boride of rubidium can make propellant of high energy；Radioactivity rubidium can measure the mineral age；
In addition, the compound of rubidium is applied to pharmacy, paper-making industry；Rubidium is alternatively arranged as the getter of vacuum system.
Rubidium is a kind of very active rare alkaline metal, and the content in the earth's crust is 0.028%, is extremely disperseed, without single
Only mineral reserve, main preservation is in lepidolite (KRbLi (OH, F) Al2Si3O10), carnallite (KClMgCl2·6H2O) etc. solids
In ore and salt lake bittern.The rubidium resource in China 55% is stored in lepidolite, Yichuan, Hunan, Hubei, Henan, Guangdong
And the main enrichment of Sichuan China Deng Didoushi rubidium resource.The salt lake bittern and underground halogen on the ground such as Qinghai, Tibet plateau
Also very abundant still since the metal ion property that chemical property and other of rubidium coexist is similar, leads to work to rubidium content in water
Industry separation is difficult so that making full use of for rubidium resource is restricted, and the yield of rubidium is relatively low.
Currently, the enterprise of domestic production rubidium chloride and other rubidium salt is more, yield is all little, and main preparation approach is from lithium
It is extracted in byproduct in salt smelting process and in Kaolin Tailings, extracting method is mostly and is roasted after villaumite mixing granulation
It burning, carrying out water logging after the mineral after roasting are crushed goes out, and then carries out the techniques such as deliming, extraction, back extraction and prepares rubidium product salt,
Long, of high cost, in sintering process the energy loss of such methods technological process also will produce greatly, in roasting process pollution air
Chlorine.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide one kind to carry from Kaolin Tailings
The method for taking rubidium chloride has many advantages, such as that technological process is short, at low cost, environmental pollution is small.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A method of it extracting rubidium chloride from Kaolin Tailings, includes the following steps：
(1) Kaolin Tailings be crushed, be sieved, obtaining kaolin mineral fine；
(2) acidleach is carried out to the kaolin mineral fine, filtered, washing obtains acid leaching liquor；
(3) deliming is carried out to the acid leaching liquor, obtains the leachate containing rubidium；
(4) leaching containing rubidium is basified, extraction, obtains the solution rich in rubidium；
(5) purified obtain of solution for being rich in rubidium refines rubidium chloride.
Above-mentioned method, it is preferred that in the step (2), acid that acidleach process uses for the sulfuric acid of concentration 10-50% or
0.5-4mol/L hydrochloric acid solutions；The purpose that sulfuric acid or hydrochloric acid solution is added is in order to which H is added+.The leaching agent that acidleach process uses
For CaF2、NaCl、CaCl2、CaSO4And Na2SO4At least one of；Leaching agent is crushed, 300 mesh screens is crossed, obtains -300 mesh
Leaching agent.The temperature of Ore Leaching is 70-95 DEG C, and the time of leaching is 3-10h；Increasing extraction temperature and extending extraction time has
Conducive to leaching, 70-95 DEG C is high-temperature that aqueous solution can reach under conditions of low energy consumption, and explorative experiment shows when leaching
Between do not promoted further higher than leaching rate after 10 hours.The quality of leaching agent is the 2%~20% of kaolin mineral fine quality,
The dosage 50-500ml of acid.Explorative experiment shows to continue to increase leaching agent ratio, leaching rate improvement effect unobvious, economy effect
Ying Bugao.Pass through the etching reaction of leaching agent and acid so that the rubidium ion in Kaolin Tailings enters in solution.
Above-mentioned method, it is preferred that in the step (2), during acidleach, first mix kaolin mineral fine with leaching agent
After closing uniformly, then with the acid solution reaction that is heated to 70-95 DEG C.During acidleach, acid and leaching agent needs are added separately to, if
It mixes before, acid and leaching agent can react first, and the effect for decomposing mineral is not achieved.First miberal powder is mixed with leaching agent, then
Acid solution one is added to react, achievees the effect that decompose mineral.
Above-mentioned method, it is preferred that in the step (2), the concrete operations being filtered, washed are：By acquired solution not
Completely under conditions of cooling, a vacuumizing filtration is carried out, the leached mud of gained is subjected to mashing washing 20-40min, liquid solid
Product ratio 4：1~1：1, second of vacuumizing filtration is then carried out, while being eluted with deionized water, collects filtrate.By solution
It is just filtered at high temperature, leached mud will be obtained and carry out mashing washing, further improve leaching rate.
Above-mentioned method, it is preferred that in the step (1), kaolin mineral fine is that -300 mesh contents are thin more than 95%
Miberal powder.Fine powder is conducive to improve leaching rate, continues to reduce powder size to leaching rate improvement effect unobvious.
Above-mentioned method, it is preferred that in the step (3), the concrete operations that deliming is carried out to the acid leaching liquor are：To
It is added highly basic in the acid leaching liquor, neutralizes the hydrogen ion in solution, solution is made to be in neutrality, then to carbonate is added in solution
Or bicarbonate so that remaining calcium ions precipitate in solution stops being added after solution is transparent.
Above-mentioned method, it is preferred that in the step (4), the extractant used in extraction process is 4- tertiary butyls -2-
(α-methylbenzyl) phenol and sulfonated kerosene；The back washing agent used in extraction process is hydrochloric acid solution；A concentration of 0.8- of extractant
1.5mol/L；A concentration of 0.5-3mol/L of back washing agent hydrochloric acid solution.The extractant extracts rubidium ion efficiency highest, using sulfonation
Kerosene is minimum as diluent cost, and the concentration range of extractant is that explorative experiment obtains, is controlled while ensureing extraction yield
Cost.
Above-mentioned method, it is preferred that in the step (4), the volume ratio of leachate containing rubidium and extractant is organic phase/water
Phase (O/A)=1：1~1：4；The volume ratio of obtained organic phase and back washing agent is organic phase/water phase (O/A)=4：1~1：1.This
Extraction yield and economic benefits reach optimal compromise value under ratio.Concrete operations are：Rubidium leachate will be contained with extractant according to organic
Phase/water phase (O/A)=1：1~1:4 mixing, are stirred, and are stood, and water phase and organic phase is waited for be kept completely separate, collect respectively water phase and
Obtained water phase and new organic phase are mixed organic phase, and obtained organic phase and new water phase are mixed, according to
Before the step of, and so on, until no longer containing rubidium ion in water phase, organic phase extracted until water phase and organic phase are kept completely separate
Saturation is taken, load organic phases are obtained.Obtained organic phase is mixed with strip liquor, according to organic phase/water phase (O/A)=4:1~
1：1 is mixed, and stands to water phase and organic phase and is kept completely separate, and water phase and organic phase is collected respectively, respectively by gained organic phase
Be mixed with new strip liquor, water phase and new organic phase be mixed, according to before the step of until water phase and organic
It is mutually kept completely separate, and so on, analysis is sampled to organic phase, until wherein no longer containing rubidium ion, finally by gained water
Solution merges, and obtains the solution rich in rubidium.
Above-mentioned method, it is preferred that in the step (5), the purified solution rich in rubidium, which obtains, refines the specific of rubidium chloride
Operation is：The solution that will be enriched in rubidium is evaporated crystallization, obtains thick rubidium product salt, then to the thick rubidium product salt of gained add water,
After rising temperature for dissolving, alkalization, extraction, back extraction obtain strip liquor, are crystallized after concentrated, filtering, sodium chloride and the potassium overwhelming majority is made to stay
In mother liquor；Using potassium chloride and sodium chloride can be a small amount of molten and principle that rubidium chloride is insoluble in absolute alcohol, rubidium chloride crystallization use
Absolute alcohol foam washing twice, obtains refined rubidium chloride.
Compared with the prior art, the advantages of the present invention are as follows：
1. the present invention is eliminated common granulation and roasting process, is shortened technique by the way of direct Ore Leaching
Flow has saved cost, reduces the energy loss in sintering process, reduces the chlorine generated during chloridising roasting to sky
The pollution of gas is more advantageous to the protection to environment, is suitable for industrialization.
2. common Ore Leaching leaching rate is relatively low, and generally below 50%.The present invention uses tailing before carrying out Ore Leaching
Carry out mill is broken, mineral are mixed with leaching agent after mix, be filtered in the case where solution is high temperature, to leaching with acid solution again
Slag carries out the modes such as mashing washing and improves Acid Leaching-out Ratio.
3. the present invention obtains the optimum process condition of direct Ore Leaching by a series of explorative experiment, ensure leaching rate
Meanwhile utmostly having compressed economic cost.
Description of the drawings
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 technology 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 scanning electron microscope sem photo of 1 Kaolin Tailings of the embodiment of the present invention：(a) amplify 100 times；(b) amplify
1000 times.
Fig. 2 is that acid directly leaches flow chart in the embodiment of the present invention 1.
Fig. 3 is the X-ray diffraction analysis photo of 1 Kaolin Tailings of the embodiment of the present invention.
Fig. 4 is 1 leached mud X-ray diffraction analysis photo of the embodiment of the present invention.
Fig. 5 is that rubidium chloride stereoscan photograph is prepared in the embodiment of the present invention 1.
Fig. 6 is that rubidium chloride X-ray diffraction analysis photo is prepared in the embodiment of the present invention 1.
Specific implementation mode
To facilitate the understanding of the present invention, it is done more entirely below in conjunction with Figure of description and preferred embodiment to inventing herein
Face meticulously describes, but protection scope of the present invention is not limited to following specific examples.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention's
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.
Embodiment 1：
The mineral containing rubidium through ore-dressing technique output that experiment is provided using Changsha Mining ＆ Metallurgy Inst, sample ore are ground after drying
Mine, sample ore heap density are 1.13g/cm3, real density 2.4g/cm3, sample ore pattern is as shown in Figure 1, Ore Leaching flow such as Fig. 2 institutes
Show, object phase composition through National Key Laboratory of powder metallurgy research institute of Central South University icp analysis as shown in figure 3, test the sample ore
In contain rubidium 0.2%.
The method that rubidium chloride is extracted in the slave Kaolin Tailings of the present embodiment, includes the following steps：
(1) vibromill 4min in vibration disc mill is added in sample ore, crosses 300 mesh screens, obtains the miberal powder of -300 mesh 95%；
By leaching agent CaF2It is broken to carry out mill, crosses 300 mesh screens；Take 200g miberal powders and 30g CaF2Leaching agent mixes, and is then added
In the sulfuric acid solution of 400ml mass fractions 40%；
(2) leaching condition：The calcirm-fluoride of the sulfuric acid of mass fraction 40% and mass fraction 15% be (calcirm-fluoride and miberal powder
Mass ratio) it leaches, calcirm-fluoride is added and discharges F with sulfuric acid reaction-, F-Miberal powder decomposition is acted, liquid-solid ratio (sulfuric acid：(mine
Powder+calcirm-fluoride)) 2:1, (sulfuric acid is added, the quality of calcirm-fluoride is matter with the mineral containing rubidium in 95 DEG C, extraction time 6h of extraction temperature
Amount is radix) so that the rubidium ion in mixture fully leaches, filtered powder sample X-ray diffraction analysis result such as Fig. 4
It is shown, chief component SiO2；
Using calcirm-fluoride and sulfuric acid may be in reacting of occurring of high-temperature region as leaching agent：
3Rb2O+2CaF2+4SiO2+2Al2O3+H2SO4=2CaAl2Si2O8+4RbF+Rb2SO4+H2O
3Rb2O+2SiO2+2CaF2+H2SO4=2CaSiO3+4RbF+Rb2SO4+H2O
7Rb2O+6CaF2+2Al2O3+H2SO4=2Ca3Al2O6+12RbF+Rb2SO4+H2O
(3) solution obtained in step (2) is subjected to vacuumizing filtration under conditions of completely not cooling, gained is leached
Slag mashing washed once that (liquid consolidates volume ratio 1.5:1), time 30min then carries out second of vacuumizing filtration, hot water elution two
Secondary (each leaching quantity is about 50mL), obtains the leachate of water white transparency；
(4) NaOH is added in the leachate obtained into step (3), leachate is neutralized to PH=7；
(5) it takes 400mL leachates to be slowly added to soda ash solution while stirring, gradually adjusts pH value of solution and be slightly larger than 7.0, control
Terminal pH continues to stir 50min after stablizing, stands 10min, be subsequently vacuumed out filtering, deliming slag total amount 100mL water wash three
It is secondary；
(6) by gained leachate 500mL in (5), it is concentrated by evaporation the leachate that rubidium enrichment is obtained to 50mL；
(7) by broken-acidleach-washing-neutralization-deliming-evaporation process, the rate of recovery of rubidium reaches 83%, has higher
Metal rate；
(8) concentrate is incorporated after the sodium hydroxide alkalization of 20g/L as extraction feed liquid, organic phase is t-BAMBP and sulphur
Change kerosene composition, a concentration of 1.2mol/L of t-BAMBP.450mL extraction phases are prepared according to above-mentioned formula, while preparing 5g/L
NaOH solution 200mL is as detergent and 1mol/L HCl strip liquors 300mL；
(9) by the extractant of above-mentioned preparation and concentrate according to volume ratio O/A=1：3 are mixed, after stratification, point
Not Shou Ji water phase and organic phase, then by new organic phase and water phase proportionally 1：3 are mixed, and are received respectively after stratification
Collect water phase and organic phase, counter-current extraction 3 times, obtain load organic phases repeatedly；
(10) load organic phases for obtaining (9) and the detergent prepared in (8) are according to O/A=8:1 mixing, washing, washing
Time 5min, washes twice repeatedly, and wash water is back to step (6) crystallization；
(11) strip liquor obtained in the organic phase and step (8) after will be washed is according to volume ratio O/A=3：1 mixing is stirred
5min is mixed, collects water phase and organic phase after stratification respectively, 5min then is mixed in new strip liquor and organic phase, it is quiet
Water phase and organic phase are collected respectively after setting layering, and countercurrent reextraction 3 times repeatedly obtain the water phase of rubidium enrichment；
(12) it is taken by multi-stage counter current extraction-washing-countercurrent reextraction, the rate of recovery of rubidium reaches 97%, rubidium in extraction process
Loss very little；
(13) water phase obtained in step (11) is evaporated crystallization, obtain compared to refined rubidium chloride impurity content compared with
High thick rubidium chloride；
(14) it alkalizes, extraction, be stripped after the thick rubidium product salt obtained in step (13) being added water rising temperature for dissolving
Crystallization, filtering, make sodium chloride and the potassium overwhelming majority stay in mother liquor after liquid is concentrated.It can be a small amount of molten using potassium chloride and sodium chloride
And principle of the rubidium chloride insoluble in absolute alcohol, rubidium chloride crystallization twice, obtain refined rubidium chloride with absolute alcohol foam washing.Scanning
Electromicroscopic photograph such as Fig. 5, X-ray diffraction analysis such as Fig. 6.The purity of refined rubidium chloride is as shown in table 1.
Table 1 refines the purity of rubidium chloride
The rate of recovery of each stage mineral containing rubidium：Broken-acidleach-washing-neutralization-deliming-evaporation stage, the rate of recovery of rubidium
Reach 83%；Extraction-washing-is counter to quench the stage, and the rate of recovery of rubidium is up to 97%；The rate of recovery of condensing crystallizing purification phase, rubidium reaches
98.8%；The whole process overall recovery of mineral test containing rubidium reaches 79.54%.
Embodiment 2：
The embodiment difference from Example 1 is step (2), and the sulfuric acid that mass fraction is 40% is replaced with quality
The sulfuric acid that score is 30%, analyzes, is operated by acidleach after tested, and the leaching rate of rubidium is 75% in mineral, and most of rubidium is
It leaches.
Embodiment 3：
The embodiment difference from Example 1 is step (2), and 15% calcirm-fluoride is replaced with to 10% fluorination
Calcium is analyzed after tested, is operated by acidleach, and the rubidium leaching rate in miberal powder is 73%, and most of rubidium has leached.
Embodiment 4：
The embodiment difference from Example 1 is step (2), and the sulfuric acid that mass fraction is 40% is replaced with
The HCl of 2mol/L, is analyzed after testing, is operated by acidleach, and the rubidium leaching rate in miberal powder is 20%, compared to being added without Ore Leaching
Agent, the leaching rate of rubidium, which has, slightly to be improved.
Embodiment 5：
The embodiment difference from Example 1 is step (2), and 15% calcirm-fluoride is replaced with identical mass fraction
NaCl, CaCl2、CaSO4And Na2SO4One or more of, it analyzes, is operated by acidleach after testing, the leaching of rubidium in miberal powder
Extracting rate increases compared to not adding leaching agent.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of method for extracting rubidium chloride from Kaolin Tailings, which is characterized in that include the following steps：
(1) Kaolin Tailings be crushed, be sieved, obtaining kaolin mineral fine；
(2) acidleach is carried out to the kaolin mineral fine, filtered, washing obtains acid leaching liquor；
(3) deliming is carried out to the acid leaching liquor, obtains the leachate containing rubidium；
(4) leaching containing rubidium is basified, extraction, obtains the solution rich in rubidium；
(5) purified obtain of solution for being rich in rubidium refines rubidium chloride.
2. the method according to claim 1 for extracting rubidium chloride from Kaolin Tailings, which is characterized in that the step
(2) in, the acid that acidleach process uses is the sulfuric acid of concentration 10-50% or the hydrochloric acid solution of 0.5-4mol/L；Acidleach process uses
Leaching agent be CaF2、NaCl、CaCl2、CaSO4And Na2SO4At least one of；The temperature of Ore Leaching is 70-95 DEG C, is leached
Time be 3-10h；The quality of leaching agent is the 2%~20% of kaolin mineral fine quality, and sour dosage is 50-500ml.
3. the method according to claim 1 for extracting rubidium chloride from Kaolin Tailings, which is characterized in that the step
(2) in, during acidleach, after mixing by kaolin mineral fine and leaching agent first, then with the acid solution that is heated to 70-95 DEG C
Reaction.
4. the method according to claim 1 for extracting rubidium chloride from Kaolin Tailings, which is characterized in that the step
(2) in, the concrete operations being filtered, washed are：By acquired solution under conditions of completely not cooling, progress once vacuumized
The leached mud of gained is carried out mashing washing 20-40min by filter, and liquid consolidates volume ratio 4：1~1：1, then vacuumized for the second time
Filtering, while being eluted with deionized water, collect filtrate.
5. the method according to claim 1 for extracting rubidium chloride from Kaolin Tailings, which is characterized in that the step
(1) in, kaolin mineral fine is the mineral fine that -300 mesh contents are more than 95%.
6. the method according to claim 1 for extracting rubidium chloride from Kaolin Tailings, which is characterized in that the step
(3) in, the concrete operations that deliming is carried out to the acid leaching liquor are：Highly basic is added into the acid leaching liquor, neutralizes in solution
Hydrogen ion, so that solution is in neutrality, then to carbonate or bicarbonate are added in solution so that remaining calcium ion in solution
Precipitation stops being added after solution is transparent.
7. the method according to claim 1 for extracting rubidium chloride from Kaolin Tailings, which is characterized in that the step
(4) in, the extractant used in extraction process is 4- tertiary butyls -2- (α-methylbenzyl) phenol and sulfonated kerosene；In extraction process
The back washing agent used is hydrochloric acid solution；A concentration of 0.8-1.5mol/L of extractant；A concentration of 0.5- of back washing agent hydrochloric acid solution
3mol/L。
8. the method according to claim 1 for extracting rubidium chloride from Kaolin Tailings, which is characterized in that the step
(4) in, the volume ratio of leachate containing rubidium and extractant is organic phase/water phase (O/A)=1：1~1：4；Obtained organic phase with it is anti-
The volume ratio for extracting agent is organic phase/water phase (O/A)=4：1~1：1.
9. the method according to claim 1 for extracting rubidium chloride from Kaolin Tailings, which is characterized in that the step
(5) in, the concrete operations that the purified solution rich in rubidium obtains refined rubidium chloride are：The solution that will be enriched in rubidium is evaporated crystallization,
Thick rubidium product salt is obtained, after then adding water, rising temperature for dissolving to the thick rubidium product salt of gained, alkalization, is stripped extraction
Liquid crystallizes, filtering after concentrated, obtains refined rubidium chloride.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109777948A (en) * | 2019-02-25 | 2019-05-21 | 广东省矿产应用研究所 | Technological method for extracting rubidium by flash cycle leaching of silicate |
| CN110835687A (en) * | 2018-08-15 | 2020-02-25 | 中国科学院过程工程研究所 | Method for extracting rubidium and cesium from steel smoke dust and/or volatile dust |
| CN112179896A (en) * | 2020-09-17 | 2021-01-05 | 长沙矿冶研究院有限责任公司 | Chemical phase analysis method for rubidium in metal ore |
| CN113957267A (en) * | 2020-07-21 | 2022-01-21 | 承德石油高等专科学校 | Method for extracting rubidium salt from soil |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101311A (en) * | 1986-06-06 | 1988-02-17 | 李久成 | Extracting rubidium caesium process program from acid-basicity magmatite weathering crust or ion adsorption type rare earth ore |
| CN104313349A (en) * | 2014-10-10 | 2015-01-28 | 李宇龙 | Method of extracting lithium salt from lepidolite |
| CN105154670A (en) * | 2015-08-28 | 2015-12-16 | 武汉理工大学 | Method for separation and enrichment of rubidium in rubidium-containing tailings |
| CN106086470A (en) * | 2016-06-12 | 2016-11-09 | 宋玉军 | A kind of method obtaining rubidium salt with Kaolin Tailings for raw material |
| CN106319245A (en) * | 2016-09-19 | 2017-01-11 | 福州大学 | Lepidolite continuous reaction lithium extracting method |
| CN107344725A (en) * | 2017-06-29 | 2017-11-14 | 周宇 | The preparation technology of elemental lithium in sulfuric acid straight dipping process extraction lithium ore |
| CN107354323A (en) * | 2017-07-26 | 2017-11-17 | 河北工程大学 | A kind of method of separation and Extraction rubidium, caesium from coal |
| CN107739039A (en) * | 2017-10-16 | 2018-02-27 | 福州大学 | A kind of method that defluorinate lepidolite pipeline dissolution carries lithium |
| CN107841637A (en) * | 2017-11-28 | 2018-03-27 | 北京科技大学 | A kind of method of collaboration extraction rubidium potassium in ore from rubidium |
-
2018
- 2018-06-06 CN CN201810587165.1A patent/CN108677006B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101311A (en) * | 1986-06-06 | 1988-02-17 | 李久成 | Extracting rubidium caesium process program from acid-basicity magmatite weathering crust or ion adsorption type rare earth ore |
| CN104313349A (en) * | 2014-10-10 | 2015-01-28 | 李宇龙 | Method of extracting lithium salt from lepidolite |
| CN105154670A (en) * | 2015-08-28 | 2015-12-16 | 武汉理工大学 | Method for separation and enrichment of rubidium in rubidium-containing tailings |
| CN106086470A (en) * | 2016-06-12 | 2016-11-09 | 宋玉军 | A kind of method obtaining rubidium salt with Kaolin Tailings for raw material |
| CN106319245A (en) * | 2016-09-19 | 2017-01-11 | 福州大学 | Lepidolite continuous reaction lithium extracting method |
| CN107344725A (en) * | 2017-06-29 | 2017-11-14 | 周宇 | The preparation technology of elemental lithium in sulfuric acid straight dipping process extraction lithium ore |
| CN107354323A (en) * | 2017-07-26 | 2017-11-17 | 河北工程大学 | A kind of method of separation and Extraction rubidium, caesium from coal |
| CN107739039A (en) * | 2017-10-16 | 2018-02-27 | 福州大学 | A kind of method that defluorinate lepidolite pipeline dissolution carries lithium |
| CN107841637A (en) * | 2017-11-28 | 2018-03-27 | 北京科技大学 | A kind of method of collaboration extraction rubidium potassium in ore from rubidium |
Non-Patent Citations (1)
| Title |
|---|
| 冀成庆等: "含铷云母精矿铷浸出试验研究", 《矿产综合利用》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110835687A (en) * | 2018-08-15 | 2020-02-25 | 中国科学院过程工程研究所 | Method for extracting rubidium and cesium from steel smoke dust and/or volatile dust |
| CN110835687B (en) * | 2018-08-15 | 2021-10-19 | 中国科学院过程工程研究所 | Method for extracting rubidium and cesium from steel smoke dust and/or volatile dust |
| CN109777948A (en) * | 2019-02-25 | 2019-05-21 | 广东省矿产应用研究所 | Technological method for extracting rubidium by flash cycle leaching of silicate |
| CN113957267A (en) * | 2020-07-21 | 2022-01-21 | 承德石油高等专科学校 | Method for extracting rubidium salt from soil |
| CN112179896A (en) * | 2020-09-17 | 2021-01-05 | 长沙矿冶研究院有限责任公司 | Chemical phase analysis method for rubidium in metal ore |
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