CN107254589B - A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern - Google Patents

A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern Download PDF

Info

Publication number
CN107254589B
CN107254589B CN201710545778.4A CN201710545778A CN107254589B CN 107254589 B CN107254589 B CN 107254589B CN 201710545778 A CN201710545778 A CN 201710545778A CN 107254589 B CN107254589 B CN 107254589B
Authority
CN
China
Prior art keywords
extraction
phase
bambp
salt lake
rubidium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201710545778.4A
Other languages
Chinese (zh)
Other versions
CN107254589A (en
Inventor
赵存良
孙玉壮
王金喜
李彦恒
石志祥
孟志强
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hebei University of Engineering
Original Assignee
Hebei University of Engineering
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hebei University of Engineering filed Critical Hebei University of Engineering
Priority to CN201710545778.4A priority Critical patent/CN107254589B/en
Publication of CN107254589A publication Critical patent/CN107254589A/en
Application granted granted Critical
Publication of CN107254589B publication Critical patent/CN107254589B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10Obtaining alkali metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/262Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds using alcohols or phenols
    • 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
    • Y02P10/20Recycling

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses the rubidium caesiums in a kind of t-BAMBP extraction separation and Extraction salt lake bittern, using t-BAMBP as extractant, using the rubidium caesium in box-reflux type extraction and separation salt lake bittern;Include the following steps: that A. detects ion concentration;B. it is acidified section: using t-BAMBP as extraction phase, extraction phase and mixed acid solution being subjected to adverse current acidification in box extraction tank;C. the extraction phase after acidification and the salt lake bittern containing rubidium and caesium extraction section: are subjected to counter-current extraction in box extraction tank;D. anti-phase washing washing section: is carried out to the rubidium caesium solution of extraction;E. anti-phase back extraction stripping section: is carried out to the extraction phase after washing;F. anti-phase washing, removal of impurities are carried out to extraction phase extracted, resulting efflux flows out extraction phase and be recycled as trash discharge.Extracting process simple process, the reagent consumption that the present invention uses are few and isolate and purify that effect is good, and yield and the purity for obtaining rubidium caesium liquid are higher, non-environmental-pollution and high financial profit.

Description

A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern
Technical field
The present invention relates to rubidium caesium extractive technique field, more particularly to a kind of t-BAMBP extraction separation and Extraction Rubidium caesium in salt lake bittern.
Background technique
Rubidium, the caesium content in the earth's crust are rich, occupy the 16th and the 40th respectively by elemental abundance arrangement, two kinds of elements are certainly It is often accompanied in right boundary, is stored in the solid minerals such as lepidolite and pollucite and salt lake halogen with elements symbiosis, main richnesses such as lithium, potassium In water.Rubidium, caesium are not only widely used in the biography such as Industrial Catalysis, medicine and special glass as important rare alkali metal resource System industry, and powerful vitality is also showed that in high-technology fields such as information technology, new energy and aerospaces.Industrially Production rubidium, caesium base stock be mainly pollucite, lepidolite, but its extraction process is complicated, at high cost and energy consumption greatly;Salt lake halogen Rubidium, caesium exist in the form of an ion in water, relatively easy to its extraction process, at low cost, and it is current rubidium, caesium industry skill that energy consumption is few Art development trend.
Separation and Extraction rubidium, caesium method mainly have fractional precipitation, fractional crystallization, ion exchange, chromatographic isolation and solvent extraction It takes, is handled with the precipitation method and isolated effect is poor, and precipitation process is more complex, both at home and abroad in the separation and Extraction of rubidium, caesium On more research has been carried out to solvent extraction.
Application No. is the patent documents of CN 201510703793.8 to disclose a kind of side that rubidium caesium is extracted from acid brine Method, although the separation and Extraction of the rubidium cesium ion in removal radioactivity water body may be implemented in this method, but the above method needs elder generation Calcium ion and magnesium ion are adsorbed by ammonium type chelating resin adsorption column, then by the efflux in resin through t-BAMBP, kerosene or Sulfonated kerosene extracts rubidium caesium, finally also needs to be stripped with hydrochloric acid, can just obtain chloride containing rubidium and cesium chloride, it is seen that purifying technique compared with Complexity is not suitable for industrialized production.
In view of this, application No. is the patent document of CN201611231035.1, to provide a kind of purifying technique simple, applicable The method of industrialized production and yield and the higher extration resin purification rubidium caesium liquid of purity, although existing rubidium caesium liquid is overcome to purify Purifying technique present in method is more complex, is not suitable for the defect of industrialized production, but the extration resin method of purification belongs to list Grade extraction process, extraction efficiency are low.
Therefore, how to provide a kind of extracting process for the separation and Extraction rubidium caesium that method and process is simple, extraction efficiency is high is this The problem of field technical staff's urgent need to resolve.
Summary of the invention
In view of this, the present invention provides the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern, this method Simple process, reagent consumption are few and isolate and purify that effect is good, and yield and the purity for obtaining rubidium caesium liquid are higher, non-environmental-pollution and High financial profit.
To achieve the goals above, the present invention adopts the following technical scheme:
Rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern, using t-BAMBP as extractant, using case Rubidium caesium in formula-reflux type extraction and separation salt lake bittern;Include the following steps:
A. it detects ion concentration: detecting each element ion concentration in the salt lake bittern using atomic absorption spectrography (AAS), Wherein Rb+Concentration be 0.5 ~ 8g/L, Cs+Concentration be 0.3 ~ 7g/L, K+Concentration be 0.02 ~ 0.15g/mL, Mg2+Concentration For 5 ~ 15g/mL, SO4 2-Concentration be 1 ~ 5g/mL, Cl-Concentration be 200 ~ 350g/L;
B. it is acidified section: t-BAMBP and mixed acid solution being placed in box extraction tank and carry out adverse current acidification, when acidification, with T-BAMBP is as extraction phase, using mixed acid solution as being acidified sour phase, and extraction phase and acidification acid phase be comparably 3 ~ 6:2 ~ 3, the extraction phase after being acidified is spare;
C. extraction section: the extraction phase after acidification obtained by step B is placed in the salt lake bittern containing rubidium and caesium jointly box In extraction tank, it is (0.1 ~ 2) that volume ratio is added thereto: 1 diluent, the extractant t- that concentration is 1.0 ~ 1.3mol/L BAMBP, and 1.0 ~ 1.4mol/L NaOH is added and carries out counter-current extraction, and is kept for 25 DEG C ~ 50 DEG C of extraction temperature;
D. washing section: right using the mixed acid solution of hydrochloric acid and nitric acid that total free acidity is 3 ~ 7mol/L as cleaning solution The extraction phase rubidium caesium solution obtained through step C carries out anti-phase washing, until the rubidium caesium solution concentration of outflow is less than 0.01g/L Only;
E. stripping section: being 1mol dilute hydrochloric acid below, dilute sulfuric acid, dust technology as strip liquor using fresh water or concentration, to warp Extraction phase after step D washing carries out anti-phase back extraction;
F. clean section: using the aqueous solution for containing 0 ~ 2mol/L nitric acid as removal of impurities liquid, to the extraction phase after step E back extraction Carry out anti-phase washing, removal of impurities, obtained in efflux be used as trash discharge, outflow extraction phase recycling.
Preferably, the t-BAMBP(purity > 95%): Beijing Rui Lekang separates Co., Ltd;NaOH(analysis is pure): at Dou Kelong chemical reagent work;HCl(analysis is pure): Chengdu Ke Long chemical reagent work.
Preferably, the mixed solution that acid solution is hydrochloric acid and nitric acid is acidified in the step B, and mixed acid solution is total Free acidity is 4 ~ 8mol/L.
Preferably, when step C is extracted, using salt lake bittern as water phase, and extraction phase and water phase be comparably 2.0 ~ 4.0:1~1.5。
Preferably, in step C, it is the basicity in order to adjust salt lake bittern that NaOH, which is added, increases the extraction yield of rubidium, caesium.
Preferably, in step C, the diluent is any one in dimethylbenzene, sulfonated kerosene or industrial naptha.
Preferably, in step D washing section, extraction phase is comparably 3 ~ 6:1 ~ 1.5 with washing phase.
Preferably, in step E stripping section, extraction phase is comparably 3 ~ 6:0.5 ~ 0.8 with back extraction phase.
Preferably, in step F removal of impurities section, extraction phase is comparably 3 ~ 6:1 ~ 1.5 with except miscellaneous phase.
Preferably, each section of extraction series is respectively as follows: 3 ~ 5 grades of section of acidification, 3 ~ 7 grades of extraction section, 2 ~ 8 grades of washing section, is stripped 3 ~ 5 grades of section cleans 2 ~ 5 grades of section.
It can be seen via above technical scheme that compared with prior art, the present disclosure provides a kind of t-BAMBP extractions It is extractant that rubidium caesium in method separation and Extraction salt lake bittern, the first present invention, which select t-BAMBP, and t-BAMBP is a kind of common rubidium Caesium extractant, and there is preferable effect to purification rubidium caesium, it can be improved rubidium caesium extraction efficiency;
Secondly box extraction tank is applied to salt lake bittern and extracts rubidium caesium, get through whole set process process, and realize industrialization Large-scale production;
Then box extraction tank is simple with equipment, low cost, stable, easy to operate, the later period maintenance operation are simple Singly, the features such as maintenance cost is cheap greatly alleviates the capital investment at enterprise construction initial stage, and box extraction line is for producing The control of quality is more stable effectively;
The last present invention is using not only high income after box extraction tank, but also obtained product is high-purity rubidium chloride and chlorine Change caesium, the performance of enterprises is good, and whole set process is continuous, production cost is low.
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 only this The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is method flow schematic diagram of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
The embodiment of the invention discloses the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern, use is box Extraction tank extracts the rubidium and caesium in salt lake bittern, and advanced optimizes process route, and this method equipment investment is small, and having can connect The advantages that continuous operation, concentration ratio height, high income.
Below in conjunction with specific embodiment, the present invention is further described, and table 1 is production salt lake bittern composition used, says The effect of extracting process of the present invention in bright specific embodiment.
Certain salt lake bittern of table 1 composition
Embodiment one
A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern, includes the following steps:
A. 50 liters of acidification mixed acid solutions are prepared: 10 liters of hydrochloric acid (chemistry is pure, and concentrated hydrochloric acid acidity is 12mol/L) is added, is added 6 liters of nitric acid (chemistry is pure, and concentrated nitric acid acidity is 16mol/L), is added 34 liters of deionized water, stirs evenly, measurement is acidified the total of acid Free acidity is 4.32mol/L;
B. the mixed acid solution prepared t-BAMBP and step A presses the ratio compared to 4.8:3, in box extraction tank into Row adverse current is acidified, and acidification series is n=4, and extraction phase is fed from the first order, and acidification nitration mixture is fed from the third level, is exported in the first order Efflux dissociates acidacidity always for 3.5mol/L;
C. the extraction phase after acidification obtained by step B and the salt lake bittern containing rubidium and caesium are placed in box extraction tank jointly In, thereto be added volume ratio be 1.5:1 diluent, concentration be 1.2mol/L extractant t-BAMBP, and be added 1.2mol/L NaOH carries out counter-current extraction, extracts series n=6, and kept for 30 DEG C of extraction temperature;
D. 30 liters of washing solution are prepared: 2 liters of hydrochloric acid (chemistry is pure, and concentrated hydrochloric acid acidity is 12mol/L) is added, nitric acid 7 is added (chemistry is pure, and concentrated nitric acid acidity is 16mol/L) is risen, 21 liters of deionized water is added, stirs evenly, measures the total free of washing solution Acidity is 4.53mol/L;
E. washing section: the mixed acid solution of the hydrochloric acid and nitric acid that are 4.53mol/L with total free acidity that step D is prepared is made For cleaning solution, wherein extraction phase carries out the extraction phase rubidium caesium solution obtained through step C with the ratio for washing the mutually 4.8:1 compared with Anti-phase washing, washs series n=4, until the rubidium caesium solution concentration of outflow is less than 0.01g/L;
F. stripping section: being 1mol dilute hydrochloric acid below, dilute sulfuric acid, dust technology as strip liquor using fresh water or concentration, wherein Extraction phase carries out anti-phase back extraction to the extraction phase after step E washing with the ratio for being stripped the mutually 4.8:0.5 compared with, is stripped series n=4;
G. clean section: using the aqueous solution for containing 1.2mol/L nitric acid as removal of impurities liquid, wherein extraction phase presses phase with miscellaneous phase is removed Anti-phase washing, removal of impurities are carried out to the extraction phase after step F back extraction than 4.8:1, clean series n=4, resulting efflux conduct Trash discharge, outflow extraction phase are recycled.
The t-BAMBP that the embodiment of the present invention 1 provides is 81% to the purifying rate of the rubidium in salt lake bittern, and the purifying rate of caesium is 86%。
Embodiment two
A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern, includes the following steps:
A. 60 liters of acidification mixed acid solutions are prepared: 15 liters of hydrochloric acid (chemistry is pure, and concentrated hydrochloric acid acidity is 12mol/L) is added, is added 11.25 liters of nitric acid (chemistry is pure, and concentrated nitric acid acidity is 16mol/L), is added 33.75 liters of deionized water, stirs evenly, measurement acidification Total free acidity of acid is 6mol/L;
B. mixed acid solution t-BAMBP and step A prepared is carried out in box extraction tank in the ratio for comparing 3:2 Adverse current is acidified, and acidification series is n=3, and extraction phase is fed from the first order, and acidification nitration mixture is fed from the third level, in first order outlet stream Liquid dissociates acidacidity always for 4mol/L out;
C. the extraction phase after acidification obtained by step B and the salt lake bittern containing rubidium and caesium are placed in box extraction tank jointly In, thereto be added volume ratio be 1.5:1 diluent, concentration be 1.2mol/L extractant t-BAMBP, and be added 1.2mol/L NaOH carries out counter-current extraction, extracts series n=6, and kept for 35 DEG C of extraction temperature;
D. 30 liters of washing solution are prepared: 1.65 liters of hydrochloric acid (chemistry is pure, and concentrated hydrochloric acid acidity is 12mol/L) is added, nitre is added 7.35 liters of acid (chemistry is pure, and concentrated nitric acid acidity is 16mol/L), is added 21 liters of deionized water, stirs evenly, measurement washing solution Total free acidity is 4.58mol/L;
E. washing section: the mixed acid solution of the hydrochloric acid and nitric acid that are 4.58mol/L with total free acidity that step D is prepared is made For cleaning solution, wherein extraction phase carries out the extraction phase rubidium caesium solution obtained through step C with the ratio for washing the mutually 5:1.2 compared with Anti-phase washing, washs series n=3, until the rubidium caesium solution concentration of outflow is less than 0.01g/L;
F. stripping section: being 1mol dilute hydrochloric acid below, dilute sulfuric acid, dust technology as strip liquor using fresh water or concentration, wherein Extraction phase with back extraction mutually the 5:0.6 in compared with ratio to through step E washing after extraction phase progress anti-phase back extraction, be stripped series n= 3;
G. clean section: using the aqueous solution for containing 1.2mol/L nitric acid as removal of impurities liquid, wherein extraction phase presses phase with miscellaneous phase is removed Anti-phase washing, removal of impurities are carried out to the extraction phase after step F back extraction than 5:1.2, clean series n=3, resulting efflux conduct Trash discharge, outflow extraction phase are recycled.
The t-BAMBP that the embodiment of the present invention 2 provides is 84.6% to the purifying rate of caesium in salt lake bittern, and the purifying rate of rubidium is 81.4%。
Embodiment three
A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern, includes the following steps:
A. 60 liters of acidification mixed acid solutions are prepared: 15 liters of hydrochloric acid (chemistry is pure, and concentrated hydrochloric acid acidity is 12mol/L) is added, is added 5 liters of nitric acid (chemistry is pure, and concentrated nitric acid acidity is 16mol/L), is added 40 liters of deionized water, stirs evenly, measurement is acidified the total of acid Free acidity is 4.3mol/L;
B. the mixed acid solution prepared t-BAMBP and step A presses the ratio compared to 5.5:3, in box extraction tank into Row adverse current is acidified, and acidification series is n=5, and extraction phase is fed from the first order, and acidification nitration mixture is fed from the third level, is exported in the first order Efflux dissociates acidacidity always for 5.1mol/L;
C. the extraction phase after acidification obtained by step B and the salt lake bittern containing rubidium and caesium are placed in box extraction tank jointly In, thereto be added volume ratio be 1.5:1 diluent, concentration be 1.1mol/L extractant t-BAMBP, and be added 1.2mol/L NaOH carries out counter-current extraction, extracts series n=6, and kept for 35 DEG C of extraction temperature;
D. 30 liters of washing solution are prepared: 2 liters of hydrochloric acid (chemistry is pure, and concentrated hydrochloric acid acidity is 12mol/L) is added, nitric acid 6 is added (chemistry is pure, and concentrated nitric acid acidity is 16mol/L) is risen, 22 liters of deionized water is added, stirs evenly, measures the total free of washing solution Acidity is 4mol/L;
E. washing section: the total free acidity prepared using step D for 4mol/L hydrochloric acid and nitric acid mixed acid solution as Cleaning solution, wherein extraction phase carries out the extraction phase rubidium caesium solution obtained through step C with the ratio for washing the mutually 5.5:1.4 compared with Anti-phase washing, washs series n=5, until the rubidium caesium solution concentration of outflow is less than 0.01g/L;
F. stripping section: being 1mol dilute hydrochloric acid below, dilute sulfuric acid, dust technology as strip liquor using fresh water or concentration, wherein Extraction phase carries out anti-phase back extraction to the extraction phase after step E washing with the ratio for being stripped the mutually 5.5:0.8 compared with, is stripped series n=5;
G. clean section: using the aqueous solution for containing 1.2mol/L nitric acid as removal of impurities liquid, wherein extraction phase presses phase with miscellaneous phase is removed Anti-phase washing, removal of impurities are carried out to the extraction phase after step F back extraction than 5.5:1.3, clean series n=5, and resulting efflux is made For trash discharge, flows out extraction phase and be recycled.
The t-BAMBP that the embodiment of the present invention 3 provides is 81.2% to the purifying rate of caesium in salt lake bittern, and the purifying rate of rubidium is 80.8%。
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest scope of cause.

Claims (8)

1. the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern, using t-BAMBP as extractant, using it is box- Rubidium caesium in reflux type extraction and separation salt lake bittern;It is characterized by comprising the following steps:
A. it detects ion concentration: detecting each element ion concentration in the salt lake bittern using atomic absorption spectrography (AAS), wherein Rb+Concentration be 0.5~8g/L, Cs+Concentration be 0.3~7g/L, K+Concentration be 0.02~0.15g/mL, Mg2+Concentration be 5~15g/mL, SO4 2-Concentration be 1~5g/mL, Cl-Concentration be 200~350g/L;
B. it is acidified section: t-BAMBP and mixed acid solution being placed in box extraction tank and carry out adverse current acidification, when acidification, with t- BAMBP is as extraction phase, using mixed acid solution as being acidified sour phase, and extraction phase and acidification acid phase be comparably 3~6:2~ 3, the extraction phase after being acidified is spare;Wherein, described to be acidified the mixed solution that acid solution is hydrochloric acid and nitric acid, and mixed acid Total free acidity of solution is 4~8mol/L;
C. the extraction phase after acidification obtained by step B and the salt lake bittern containing rubidium and caesium extraction section: are placed in box extraction jointly In slot, it is (0.1~2) that volume ratio is added thereto: 1 diluent, the extractant t-BAMBP that concentration is 1.0~1.3mol/L, And 1.0~1.4mol/LNaOH is added and carries out counter-current extraction, and is kept for 25 DEG C~50 DEG C of extraction temperature;
D. washing section: using the mixed acid solution of hydrochloric acid and nitric acid that total free acidity is 3~7mol/L as cleaning solution, to through step The extraction phase rubidium caesium solution that rapid C is obtained carries out anti-phase washing, until the rubidium caesium solution concentration of outflow is less than 0.01g/L;
E. stripping section: being 1mol dilute hydrochloric acid below, dilute sulfuric acid, dust technology as strip liquor using fresh water or concentration, to through step D Extraction phase after washing carries out anti-phase back extraction;
F. clean section: use the aqueous solution that contains 0~2mol/L nitric acid as removal of impurities liquid, to the extraction phase after step E back extraction into Row anti-phase washing, removal of impurities, obtained in efflux be used as trash discharge, outflow extraction phase be recycled, wherein extraction phase and 3~6:1~1.5 are comparably except miscellaneous phase.
2. the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern according to claim 1, feature exist Co., Ltd is separated in the t-BAMBP: Beijing Rui Lekang;NaOH: Chengdu Ke Long chemical reagent work;HCl: Chengdu Ke Long chemical reagent work.
3. the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern according to claim 1, feature exist When, step C is extracted, using salt lake bittern as water phase, and extraction phase and water phase are comparably 2.0~4.0:1~1.5.
4. the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern according to claim 1, feature exist In in step C, it is the basicity in order to adjust salt lake bittern that NaOH, which is added, increases the extraction yield of rubidium, caesium.
5. the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern according to claim 1, feature exist In in step C, the diluent is any one in dimethylbenzene, sulfonated kerosene or industrial naptha.
6. the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern according to claim 1, feature exist In in step D washing section, extraction phase is comparably 3~6:1~1.5 with washing phase.
7. the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern according to claim 1, feature exist In in step E stripping section, extraction phase is comparably 3~6:0.5~0.8 with back extraction phase.
8. the rubidium caesium in a kind of t-BAMBP extraction separation and Extraction salt lake bittern according to claim 1, feature exist It is respectively as follows: 3~5 grades of section of acidification in, each section of extraction series, 3~7 grades of extraction section, 2~8 grades of washing section, 3~5 grades of stripping section, 2~5 grades of section of removal of impurities.
CN201710545778.4A 2017-07-06 2017-07-06 A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern Active CN107254589B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710545778.4A CN107254589B (en) 2017-07-06 2017-07-06 A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710545778.4A CN107254589B (en) 2017-07-06 2017-07-06 A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern

Publications (2)

Publication Number Publication Date
CN107254589A CN107254589A (en) 2017-10-17
CN107254589B true CN107254589B (en) 2019-02-22

Family

ID=60026387

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710545778.4A Active CN107254589B (en) 2017-07-06 2017-07-06 A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern

Country Status (1)

Country Link
CN (1) CN107254589B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109536740B (en) * 2018-12-13 2021-07-27 鑫联环保科技股份有限公司 Method for preparing cesium sulfate from salt-containing wastewater
CN110550646A (en) * 2019-10-10 2019-12-10 宜春市科远化工有限公司 preparation method of cesium sulfate and rubidium sulfate
CN111996392B (en) * 2020-07-22 2022-07-15 中国地质科学院郑州矿产综合利用研究所 Method for extracting cesium and rubidium from lepidolite

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101696468A (en) * 2009-10-23 2010-04-21 陕西晶茂投资有限公司 Acid-method regenerative organic phase process in vanadium extraction cycle
CN102557085B (en) * 2011-11-03 2014-09-03 上海离岛电子新材料有限公司 Method for extracting sodium salt in cesium salt and rubidium salt production process
CN102534213B (en) * 2012-02-17 2014-01-22 云南五鑫实业有限公司 Method for carrying out normalized treatment on P204 extraction poisoning
CN103882227A (en) * 2014-04-04 2014-06-25 成都理工大学 Novel rubidium-potassium separating extracting agent and separating method
CN204138735U (en) * 2014-10-17 2015-02-04 江西东鹏新材料有限责任公司 A kind of rubidium caesium produces special extraction tank
CN105256150B (en) * 2015-10-26 2017-12-12 中国科学院青海盐湖研究所 A kind of method that rubidium caesium is extracted from acid bittern
CN106148730B (en) * 2016-07-05 2018-05-25 广东道氏技术股份有限公司 A kind of method that alkali metal is extracted from lepidolite
CN106883262B (en) * 2017-03-28 2019-03-08 南昌航空大学 A kind of regeneration method of aging TBP organic phase

Also Published As

Publication number Publication date
CN107254589A (en) 2017-10-17

Similar Documents

Publication Publication Date Title
CN104831073B (en) A kind of technique reclaiming platinum, palladium, rhodium from spent auto-catalysts
CN107254589B (en) A kind of rubidium caesium in t-BAMBP extraction separation and Extraction salt lake bittern
CN104147929B (en) Novel reflux cascade technology for producing lithium-7 isotopes
CN104928504B (en) A kind of recovery method of aluminium scrap silicon middle rare earth
CN111057848A (en) Method for extracting lithium from lithium-containing solution by solvent extraction
CN114105171B (en) Method for comprehensively utilizing lepidolite resources and lithium hydroxide prepared by method
CN108342573B (en) A method of from extraction and separation tungsten in ammonium tungstate solution containing molybdenum
CN101955228A (en) Method for separating tantalum and niobium
CN107217156A (en) The method that rubidium cesium salt is extracted from spodumene lithium liquor
CN108103317B (en) Method for recovering lithium from lithium-containing waste liquid
CN104018012A (en) Method of extracting gallium from aluminum chloride solution
BR112018003045B1 (en) Methods for producing a scandium-containing concentrate from waste sludge, and for producing a scandium oxide of high purity
CN103060580B (en) Method for separating titanium, scandium and zirconium in scandium extraction with titanium white waste acid
CN100554445C (en) A kind of inclined to one side potassium tantalate, method of tantalum and niobium in the potassium niobate mixture partially of separating
CN111286608B (en) Method for selectively separating tantalum and niobium step by step based on floating extraction
CN109502613A (en) A method of high pure magnesium chloride is prepared from salt lake bittern
CN106929693A (en) A kind of caesium rubidium potassium extraction separating method
Jantunen et al. Separation of zinc and iron from secondary manganese sulfate leachate by solvent extraction
CN106892479B (en) Method for recovering oxalic acid and hydrochloric acid from rare earth oxalic acid precipitation wastewater
CN116404220A (en) Method for preparing high-concentration vanadium electrolyte by vanadate crystallization purification-chemical reduction
CN106521159B (en) Based on lithium in the extraction system extraction bittern containing Fe (III) and the method for recycling Fe (III)
CN103361488B (en) The recovery method of scandium in a kind of titanium dioxide wastewater
CN105087945B (en) Method for utilizing zirconium oxychloride waste acid comprehensively
CN103773962B (en) A kind of from chlorination process produce titanium dioxide produce waste hydrochloric acid recovery Pd method
CN109266852B (en) Zirconium-hafnium separation method for preferentially extracting hafnium by using organic acid

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB03 Change of inventor or designer information

Inventor after: Zhao Cunliang

Inventor after: Sun Yuzhuang

Inventor after: Wang Jinxi

Inventor after: Li Yanheng

Inventor after: Shi Zhixiang

Inventor after: Meng Zhiqiang

Inventor before: Sun Yuzhuang

Inventor before: Zhao Cunliang

Inventor before: Wang Jinxi

Inventor before: Li Yanheng

Inventor before: Shi Zhixiang

Inventor before: Meng Zhiqiang

CB03 Change of inventor or designer information
GR01 Patent grant
GR01 Patent grant