CN106702156A - Method for adsorbing and separating rubidium by using Levextrel resin - Google Patents
Method for adsorbing and separating rubidium by using Levextrel resin Download PDFInfo
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- CN106702156A CN106702156A CN201611230971.0A CN201611230971A CN106702156A CN 106702156 A CN106702156 A CN 106702156A CN 201611230971 A CN201611230971 A CN 201611230971A CN 106702156 A CN106702156 A CN 106702156A
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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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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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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- 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
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Abstract
The invention belongs to the technical field of rubidium solution purification and particularly provides a method for adsorbing and separating rubidium by using Levextrel resin. The method comprises t-BAMBP Levextrel resin preparation, an adsorption process of a rubidium solution and a desorption process of rubidium, namely firstly, uniformly mixing macroporous resin, t-BAMBP and a diluent, and carrying out stirring, filtering and drying to prepare t-BAMBP Levextrel resin; placing the rubidium solution and the t-BAMBP Levextrel resin into a vessel, regulating the alkalinity of the rubidium solution to be 1.1-1.5mol/L, and carrying out filtration to obtain rubidium-adsorbed t-BAMBP Levextrel resin; and adding a desorption agent into the rubidium-adsorbed t-BAMBP Levextrel resin, and carrying out stirring and filtering to obtain a purified rubidium solution. The method disclosed by the invention is simple; and when petroleum ether is selected as the diluent and 1.0mol/L of hydrochloric acid is selected as the desorption agent, the rubidium separation and enrichment effects are best.
Description
Technical field
The invention belongs to rubidium liquid purification technique field, and in particular to a kind of method that Adsorption by Extracting Resins separates rubidium.
Technical background
Rubidium content in the earth's crust is rich, and the 16th is occupied by elemental abundance arrangement, and main preservation is in lepidolite and pollucite etc.
In solid mineral and salt lake bittern.Rubidium have very strong chemism and excellent photoelectric properties, electronic device, catalyst,
There is larger development in the tradition application field such as special glass.In recent years, as to the deep understanding of rubidium, it sends out in magnetic fluid
In the emerging application fields such as electricity, thermion conversion power generation and ion propulsion engine, powerful vitality is also show.
Rubidium is a kind of dispersed elements, potassium symbiosis often very big with otheralkali metal element particularly abundance, therefore long in potassium
Usually contain micro rubidium element, but the physics and chemical property of potassium and rubidium in stone mine tailing very close to this is the separation of rubidium, carries
Pure and mild product deep processing brings very big difficulty, also increases rubidium extraction, the complexity of purifying technique, and the method for purification of rubidium is from most
Traditional fractionation crystallization starts, and progressively develops that the precipitation method, ion-exchange and solvent extraction etc. are various to put forward rubidium technique, and
Still studying other effective extracting methods.
For example, the A of Chinese patent literature CN 105154670 disclose a kind of side from separation and concentration rubidium in mine tailing containing rubidium
Method, the method will contain rubidium mine tailing with hydrochloric acid solution by solid-to-liquid ratio 1 first:1~1:10 stir leaching in stirred tank, after filtering
Obtain solution containing rubidium;After the solution containing rubidium is done into adsorbent absorption through the carrier of overload ammonium phosphomolybdate, ammonium chloride solution solution is used
The pregnant solution of rubidium is obtained after analysis.The above method takes full advantage of the rubidium resource in mine tailing containing rubidium, realizes the comprehensive utilization of resource,
Production process does not produce pollution, and institute can be recycled using adsorbent and desorbed solution.But above-mentioned technology is using load ammonium phosphomolybdate
Carrier make adsorbent, the preparation method of this adsorbent is complicated, does not apply to industrial amplification production, and artificial input cost is high.Cause
This, is improved significant to existing rubidium liquid method of purification.
The content of the invention
The technical problems to be solved by the invention are to overcome adsorbing agent carrier system existing for existing rubidium liquid method of purification
Preparation Method is complicated, inapplicable industrial amplification production and artificial input cost defect high, and then provides a kind of purifying technique letter
Method that is single, being applicable industrialized production, extraction yield and desorption efficiency Adsorption by Extracting Resins separation rubidium higher.
The present invention solve the technical scheme that uses of above-mentioned technical problem for:
The present invention provides the method that Adsorption by Extracting Resins separates rubidium, comprises the following steps:
(1) preparation of t-BAMBP extration resins
Macroreticular resin, t-BAMBP and diluent are well mixed, 10~12h is stirred at room temperature, filtered, after filtering
Resin drying, that is, be obtained the t-BAMBP extration resins;
(2) adsorption process of rubidium liquid
Rubidium solution and t-BAMBP extration resins are placed in container, above-mentioned rubidium solution basicity is adjusted with sodium hydroxide solution
It is 1.1~1.5mol/L, vibration 6~10h of stirring, filtering obtains adsorbing the t-BAMBP extration resins of rubidium;
(3) desorption process of rubidium
Strippant is added in t-BAMBP extration resins to absorption rubidium, vibration 6~10h of stirring, filtering is purified
Rubidium liquid.
Preferably, the macroreticular resin is polystyrene macroporous resin or polystyrene-divinylbenzene type macroreticular resin.
It is further preferred that the macroreticular resin is polystyrene-divinylbenzene type macroreticular resin.
Preferably, the diluent is petroleum ether, dichloroethanes or ethanol.
It is further preferred that the diluent is petroleum ether.
The t-BAMBP is 1 with the volume ratio of the diluent:(1~5).
Preferably, the strippant is deionized water, sodium chloride or hydrochloric acid.
It is further preferred that the strippant is hydrochloric acid.
Above-mentioned technical proposal of the invention has the following advantages that:
The method that Adsorption by Extracting Resins of the present invention separates rubidium, preparation of the method including t-BAMBP extration resins,
, be well mixed for macroreticular resin, t-BAMBP and diluent first by the adsorption process of rubidium liquid and the desorption process of rubidium, stirring, mistake
Filter, drying is obtained the t-BAMBP extration resins;Rubidium solution and t-BAMBP extration resins are placed in container, hydrogen-oxygen is used
Change sodium solution to adjust above-mentioned rubidium solution basicity is 1.1~1.5mol/L, and vibration stirring, filtering obtains adsorbing the t-BAMBP extractions of rubidium
Drench resin;Strippant is added in t-BAMBP extration resins to absorption rubidium, is stirred, filtering obtains purifying rubidium liquid, the present invention
Methods described is simple, extration resin it is repeatable utilize, separation and concentration effect it is good, and extraction yield by method of the present invention rubidium can
To reach more than 89%, desorption efficiency can reach more than 85%, realize and efficiently separated with other heteroions.
Specific embodiment
Technical scheme will be clearly and completely described below, it is clear that described embodiment is this hair
Bright a part of embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
There is the every other embodiment made and being obtained under the premise of creative work, belong to the scope of protection of the invention.Additionally, below
As long as in described different embodiments of the present invention involved technical characteristic do not constitute each other conflict just can be mutual
With reference to.
Embodiment 1
The method that the Adsorption by Extracting Resins that the present embodiment is provided separates rubidium comprises the following steps:
(1) preparation of t-BAMBP extration resins
To be placed in polystyrene-divinylbenzene type macroreticular resin 20g and the 20mL t-BAMBP after washes of absolute alcohol
In container, 20mL petroleum ethers are subsequently adding, 10h is stirred at room temperature, filtered, in drying, prepared petroleum ether under 90 DEG C of baking ovens
The t-BAMBP extration resins for the treatment of;
(2) adsorption process of rubidium liquid
The t-BAMBP extration resins that the rubidium solution that 40mL concentration is 357mg/L adds the treatment of 20g petroleum ethers are taken, hydrogen is used
The basicity that sodium oxide molybdena adjusts above-mentioned rubidium solution is 1.5mol/L, and vibration stirring 6h, filtering, the t-BAMBP extractions for obtaining adsorbing rubidium are drenched
Resin;
(3) desorption process of rubidium
To addition 40mL concentration in the t-BAMBP extration resins of absorption rubidium for 1.0mol/L HCl strippants are desorbed,
Vibration stirring 10h, filtering takes filtrate, as desorbs rubidium liquid, the extration resin that the present embodiment is provided to the extraction yield of rubidium solution and
Desorption efficiency is as shown in table 1.
Extraction yield and desorption efficiency of the extration resin of table 1 to rubidium solution
As shown in Table 1, when extration resin is with petroleum ether as diluent, with 1.0mol/L HCl as strippant, extraction now
It is 89.0% to drench resin to the rubidium extraction yield of rubidium solution, and rubidium desorption efficiency is 89.1%.
Embodiment 2
The method that the Adsorption by Extracting Resins that the present embodiment is provided separates rubidium comprises the following steps:
(1) preparation of t-BAMBP extration resins
To be placed in polystyrene-divinylbenzene type macroreticular resin 20g and the 20mL t-BAMBP after washes of absolute alcohol
In container, 40mL dichloroethanes is subsequently adding, 12h is stirred at room temperature, filtered, in drying, prepared dichloro under 80 DEG C of baking ovens
The t-BAMBP extration resins of ethane treatment;
(2) adsorption process of rubidium liquid
The t-BAMBP extration resins that the rubidium solution that 40mL concentration is 576mg/L adds the treatment of 20g dichloroethanes are taken, is used
The basicity that NaOH adjusts above-mentioned rubidium solution is 1.3mol/L, and vibration stirring 10h, filtering obtains adsorbing the t-BAMBP extractions of rubidium
Drench resin;
(3) desorption process of rubidium
To addition 40mL concentration in the t-BAMBP extration resins of absorption rubidium for 1.0mol/L HCl strippants are desorbed,
Vibration stirring 6h, filtering takes filtrate, as desorbs rubidium liquid, the extration resin that the present embodiment is provided to the extraction yield of rubidium solution and
Desorption efficiency is as shown in table 2.
Extraction yield and desorption efficiency of the extration resin of table 2 to rubidium solution
As shown in Table 2, when extration resin is with dichloroethanes as diluent, with 1.0mol/L HCl as strippant, now
Extration resin is 75.5% to the rubidium extraction yield of rubidium solution, and rubidium desorption efficiency is 81.3%.
Embodiment 3
The method that the Adsorption by Extracting Resins that the present embodiment is provided separates rubidium comprises the following steps:
(1) preparation of t-BAMBP extration resins
To be placed in polystyrene-divinylbenzene type macroreticular resin 20g and the 20mL t-BAMBP after washes of absolute alcohol
In container, 100mL ethanol is subsequently adding, 11h is stirred at room temperature, filtered, in drying, prepared Ethanol Treatment under 50 DEG C of baking ovens
T-BAMBP extration resins;
(2) adsorption process of rubidium liquid
The t-BAMBP extration resins that the rubidium solution that 40mL concentration is 738mg/L adds 20g Ethanol Treatments are taken, hydrogen-oxygen is used
The basicity for changing the sodium above-mentioned rubidium solution of regulation is 1.2mol/L, and vibration stirring 8h, filtering obtains the t-BAMBP extration resins of absorption rubidium;
(3) desorption process of rubidium
To addition 40mL concentration in the t-BAMBP extration resins of absorption rubidium for 1.0mol/L HCl strippants are desorbed,
Vibration stirring 8h, filtering takes filtrate, as desorbs rubidium liquid, the extration resin that the present embodiment is provided to the extraction yield of rubidium solution and
Desorption efficiency is as shown in table 3.
Extraction yield and desorption efficiency of the extration resin of table 3 to rubidium solution
As shown in Table 3, when extration resin is with ethanol as diluent, with 1.0mol/L HCl as strippant, extraction now is drenched
Resin is 38.9% to the rubidium extraction yield of rubidium solution, and rubidium desorption efficiency is 80.3%.
Embodiment 4
The method that the Adsorption by Extracting Resins that the present embodiment is provided separates rubidium comprises the following steps:
(1) preparation of t-BAMBP extration resins
To be placed in polystyrene-divinylbenzene type macroreticular resin 20g and the 20mL t-BAMBP after washes of absolute alcohol
In container, 20mL petroleum ethers are subsequently adding, 10h is stirred at room temperature, filtered, in drying, prepared petroleum ether under 50 DEG C of baking ovens
The t-BAMBP extration resins for the treatment of;
(2) adsorption process of rubidium liquid
The t-BAMBP extration resins that the rubidium solution that 40mL concentration is 148mg/L adds the treatment of 20g petroleum ethers are taken, hydrogen is used
The basicity that sodium oxide molybdena adjusts above-mentioned rubidium solution is 1.1mol/L, and vibration stirring 10h, filtering, the t-BAMBP extractions for obtaining adsorbing rubidium are drenched
Resin;
(3) desorption process of rubidium
To adding 40mL deionized water strippants to be desorbed in the t-BAMBP extration resins of absorption rubidium, 6h is stirred in vibration,
Filtering, takes filtrate, as desorbs rubidium liquid, extraction yield and desorption efficiency such as table 4 of the extration resin that the present embodiment is provided to rubidium solution
It is shown.
Extraction yield and desorption efficiency of the extration resin of table 4 to rubidium solution
As shown in Table 4, when extration resin is with petroleum ether as diluent, with deionized water as strippant, extraction now drenches tree
Fat is 89.1% to the rubidium extraction yield of rubidium solution, and rubidium desorption efficiency is 40.6%.
Embodiment 5
The method that the Adsorption by Extracting Resins that the present embodiment is provided separates rubidium comprises the following steps:
(1) preparation of t-BAMBP extration resins
To be placed in polystyrene-divinylbenzene type macroreticular resin 20g and the 20mL t-BAMBP after washes of absolute alcohol
In container, 20mL petroleum ethers are subsequently adding, 10h is stirred at room temperature, filtered, in drying, prepared petroleum ether under 90 DEG C of baking ovens
The t-BAMBP extration resins for the treatment of;
(2) adsorption process of rubidium liquid
The t-BAMBP extration resins that the rubidium solution that 40mL concentration is 96mg/L adds the treatment of 20g petroleum ethers are taken, hydrogen-oxygen is used
The basicity for changing the sodium above-mentioned rubidium solution of regulation is 1.3mol/L, and vibration stirring 8h, filtering, the t-BAMBP extractions for obtaining absorption rubidium drench tree
Fat;
(3) desorption process of rubidium
To addition 40mL concentration in the t-BAMBP extration resins of absorption rubidium for 1.0mol/L NaCl strippants are desorbed,
Vibration stirring 6h, filtering takes filtrate, as desorbs rubidium liquid, the extration resin that the present embodiment is provided to the extraction yield of rubidium solution and
Desorption efficiency is as shown in table 5.
Extraction yield and desorption efficiency of the extration resin of table 5 to rubidium solution
As shown in Table 5, when extration resin is with petroleum ether as diluent, with 1.0mol/L NaCl as strippant, extraction now
It is 89.1% to drench resin to the rubidium extraction yield of rubidium solution, and rubidium desorption efficiency is 40.6%.
Embodiment 6
The dynamic experiment method adsorbs rubidium
The method that the Adsorption by Extracting Resins that the present embodiment is provided separates rubidium comprises the following steps:
(1) preparation of t-BAMBP extration resins
To be placed in polystyrene-divinylbenzene type macroreticular resin 20g and the 20mL t-BAMBP after washes of absolute alcohol
In container, 20mL petroleum ethers are subsequently adding, 10h is stirred at room temperature, filtered, in drying, prepared petroleum ether under 90 DEG C of baking ovens
The t-BAMBP extration resins for the treatment of;
(2) desorption process of the adsorption process of rubidium liquid and rubidium
Above-mentioned t-BAMBP extration resins are placed in resin-column, take 40ml concentration be 357mg/L rubidium solution in perseverance
In pressure titration pipe, control rate of titration is instilled in extration resin exchange column, and efflux is extraction extraction raffinate, treats rubidium solution in 20min
After dripping off, then the rubidium concentration of measurement extraction extraction raffinate desorbed with the HCl strippants that concentration is 1.0mol/L, and flow velocity is 2mL/
Min, collects stripping liquid.
The rubidium concentration for determining extraction extraction raffinate is 38.5mg/L, and rubidium extraction yield is 89.2%;Stripping liquid rubidium concentration is
286.7mg/L, rubidium desorption efficiency is 90.9%.
To sum up, when diluent selects petroleum ether, and strippant selects 1.0mol/L hydrochloric acid, to the separation and concentration effect of rubidium most
Good, now extration resin is 89.2% to the optimal rubidium extraction yield of rubidium solution, and optimal rubidium desorption efficiency is 90.9%.
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of implementation method.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need and unable to be enumerated to all of implementation method.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (8)
1. a kind of method that Adsorption by Extracting Resins separates rubidium, it is characterised in that comprise the following steps:
(1) preparation of t-BAMBP extration resins
Macroreticular resin, t-BAMBP and diluent are well mixed, 10~12h is stirred at room temperature, filtered, by the tree after filtering
Fat is dried, that is, the t-BAMBP extration resins are obtained;
(2) adsorption process of rubidium liquid
Rubidium solution and t-BAMBP extration resins are placed in container, it is 1.1 to adjust above-mentioned rubidium solution basicity with sodium hydroxide solution
~1.5mol/L, vibration 6~10h of stirring, filtering obtains adsorbing the t-BAMBP extration resins of rubidium;
(3) desorption process of rubidium
Strippant is added in t-BAMBP extration resins to absorption rubidium, vibration 6~10h of stirring, filtering obtains purifying rubidium liquid.
2. the method that Adsorption by Extracting Resins according to claim 1 separates rubidium, it is characterised in that the macroreticular resin is poly-
Styrene type macroporous resin or polystyrene-divinylbenzene type macroreticular resin.
3. the method that Adsorption by Extracting Resins according to claim 2 separates rubidium, it is characterised in that the macroreticular resin is poly-
Styrene-divinylbenzene type macroreticular resin.
4. the method that Adsorption by Extracting Resins according to claim 1 separates rubidium, it is characterised in that the diluent is oil
Ether, dichloroethanes or ethanol.
5. the method that Adsorption by Extracting Resins according to claim 4 separates rubidium, it is characterised in that the diluent is oil
Ether.
6. the method that Adsorption by Extracting Resins according to claim 1 separates rubidium, it is characterised in that the t-BAMBP and institute
The volume ratio for stating diluent is 1:(1~5).
7. the method that Adsorption by Extracting Resins according to claim 1 separates rubidium, it is characterised in that the strippant for go from
Sub- water, sodium chloride or hydrochloric acid.
8. the method that Adsorption by Extracting Resins according to claim 7 separates rubidium, it is characterised in that described strippant is salt
Acid.
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Cited By (1)
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CN115717200A (en) * | 2022-11-23 | 2023-02-28 | 华东理工大学 | Selective lithium extraction method from levextrel resin |
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Application publication date: 20170524 |
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RJ01 | Rejection of invention patent application after publication |