CN110293004A - Rubidium, the precipitate flotation separation system of caesium and its application in a kind of aqueous solution - Google Patents

Rubidium, the precipitate flotation separation system of caesium and its application in a kind of aqueous solution Download PDF

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Publication number
CN110293004A
CN110293004A CN201910583391.7A CN201910583391A CN110293004A CN 110293004 A CN110293004 A CN 110293004A CN 201910583391 A CN201910583391 A CN 201910583391A CN 110293004 A CN110293004 A CN 110293004A
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rubidium
flotation separation
flotation
aqueous solution
caesium
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Inventor
叶秀深
房得珍
刘海宁
李明珍
张慧芳
王世栋
钱志强
吴志坚
葛飞
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Qinghai Institute of Salt Lakes Research of CAS
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Qinghai Institute of Salt Lakes Research of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/02Froth-flotation processes
    • 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
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006Wet processes
    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21FPROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04Treating liquids
    • G21F9/06Processing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; specified applications
    • B03D2203/008Water purification, e.g. for process water recycling
    • 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

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  • Chemical & Material Sciences (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention discloses rubidium, the precipitate flotation separation system of caesium and its applications in a kind of aqueous solution.The precipitate flotation separation system includes: precipitating reagent, includes at least phosphomolybdate;And collecting agent and foaming agent, include at least cationic surfactant.The invention also discloses the flotation separation methods of rubidium, cesium ion in a kind of aqueous solution, it include: that reaction in the aqueous solution containing cesium ion is added in precipitating reagent, collecting agent and foaming agent to precipitate cesium ion, the precipitating reagent includes at least phosphomolybdate, and the collecting agent and foaming agent include at least cationic surfactant;The precipitating solid content collecting reaction and obtaining is handled by FLOTATION SEPARATION.The present invention passes through precipitating-floatation process combination, provide the precipitate flotation system using phosphomolybdate as precipitating reagent, the problems such as can be used for the removal of rubidium, cesium ion in the separation and Extraction or radiation waste liquid of rubidium caesium resource, the molten damage of support type ammonium phosphomolybdate adsorbent or complicated material preparation can be overcome in use process.

Description

Rubidium, the precipitate flotation separation system of caesium and its application in a kind of aqueous solution
Technical field
The present invention relates to a kind of precipitate flotation systems more particularly to a kind of using phosphomolybdate as in the aqueous solution of precipitating reagent Rubidium, caesium precipitate flotation separation system and radioactive liquid waste in rubidium, caesium minimizing technology, belong to element sepatation and environmental recovery bonds Learn technical field.
Background technique
Rubidium, cesium compound are widely used in electronics, special glass, catalyst, the energy, doctor because of its unique physicochemical property The fields such as medicine.In recent years, the especially great-leap-forward development of science and techniques of defence, three boat industries and new energy etc., to the demand of rubidium, caesium It is increasing, while will be used wider and wider rubidium, caesium.So efficient industrial separation extracts rubidium, caesium in natural resources Technology be current necessary to be also important task.
Rubidium, caesium belong to rare precious metal, since its property is active, generally coexists in mineral with other elements, typically contain Rubidium, cesium mineral include the liquid mine such as the solid minerals such as lepidolite, pollucite and salt lake bittern, GEOTHERMAL WATER, are contained in these mineral Alkali, the alkaline-earth metal that coexistence elements are closer to again with property are in the majority, and in addition some radioactivity rubidium, caesium are present in radiation In property waste liquid.The removal that either separation and Extraction of rubidium caesium resource still radiates rubidium caesium in waste liquid requires have Gao Xuan to rubidium caesium The reagent and method of selecting property.
Many scholars have conducted extensive research the extracting method of rubidium caesium in nature, typical method has extraction, inhale Attached or ion-exchange, precipitation method etc., wherein organic reagent used in extraction is relatively more, and industrially has application performance at present Preferable t-BAMBP extraction system needs to operate under alkaline condition, is not suitable for most of containing rubidium, caesium system.The precipitation method and from Son exchange (absorption) method can use identical reagent in some circumstances, wherein having high selection to rubidium, caesium with heteropolyacid salt Property is by more concern.
Ammonium phosphomolybdate is that have a kind of highly selective and exchange capacity heteropolyacid salt to rubidium and caesium, reacts generation with rubidium caesium Phosphomolybdic acid rubidium or phosphomolybdic acid caesium be indissoluble object, low content rubidium caesium Selective Separation in complex system can be come, because Rubidium, the Selective Separation aspect research of caesium are more in the solution for this, but since phosphomolybdate is powder crystal structure, so causing solid Liquid separation is difficult.
The existing technology path using ammonium phosphomolybdate progress rubidium, caesium separation and Extraction essentially loads to powder ammonium phosphomolybdate On basis material, improve the problem of it is separated by solid-liquid separation aspect.But since ammonium phosphomolybdate is the inorganic matter of stable structure, it is extremely difficult to Basis material forms the compound-split material of stable structure by strong effect power, and recycling stability is inadequate, makes in circulation With that can have different degrees of molten damage in the process, some composite materials preparation process is complicated.
About rubidium caesium in FLOTATION SEPARATION solution, Ma Fuqiu etc. uses potassium ferrocyanide and has investigated pair as precipitation reagent The precipitate flotation of caesium in radioactive liquid waste radiates waste liquid for the solid of the caesium containing rubidium or liquid resource mine, and system is simple, Separating difficulty is small, but the rubidium caesium sediment that potassium ferrocyanide is formed simultaneously is difficult to cycling and reutilization;Furthermore existing floatation is all It is the extraction separation that rubidium caesium in radioactive liquid waste is difficult to for solid mineral.
Summary of the invention
The main purpose of the present invention is to provide the precipitate flotation separation systems of rubidium, caesium in a kind of aqueous solution, existing to overcome There is the deficiency in technology.
Another object of the present invention, which also resides in, provides the precipitate flotation separation system in FLOTATION SEPARATION rubidium ion, cesium ion In application.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides the precipitate flotation separation systems of rubidium, caesium in a kind of aqueous solution comprising:
Precipitating reagent includes at least phosphomolybdate;And
Collecting agent and foaming agent include at least cationic surfactant.
The embodiment of the invention also provides the precipitate flotation separation systems of rubidium, caesium in the aqueous solution in FLOTATION SEPARATION rubidium Application in ion and/or cesium ion.
The embodiment of the invention also provides the flotation separation methods of rubidium, cesium ion in a kind of aqueous solution comprising:
Will precipitating reagent, collecting agent and foaming agent be added the aqueous solution containing rubidium ion and/or cesium ion in reaction make rubidium from Son and/or cesium ion precipitating, wherein the precipitating reagent includes at least phosphomolybdate, the collecting agent and foaming agent include at least sun Ionic surface active agent;
The precipitating solid content collecting reaction and obtaining is handled by FLOTATION SEPARATION.
In some preferred embodiments, the flotation separation method specifically includes:
Precipitating reagent is added in the aqueous solution containing rubidium ion and/or cesium ion and be reacted, precipitating solid content is generated, obtains the One intermediate system;
The backward first intermediate system in collecting agent and foaming agent is added, and be uniformly mixed, obtain the second intermediate system;
FLOTATION SEPARATION processing is carried out to the described second intermediate system using floatation separator, collects the precipitating solid Object.
Compared with prior art, beneficial effects of the present invention at least that:
1) present invention is provided a kind of using phosphomolybdate as the precipitate flotation of precipitating reagent by precipitating-floatation process combination System can be used for the removal of rubidium, cesium ion in the separation and Extraction or radiation waste liquid of rubidium caesium resource, can overcome in use process negative The problems such as molten damage of load type ammonium phosphomolybdate adsorbent or complicated material preparation;
2) present invention provides first precipitating, the process of FLOTATION SEPARATION again, and compared with extraction, the scope of application is wide, organic reagent Dosage is low, and extraction is only applicable to separation and Extraction rubidium, caesium under alkaline condition;Compared with direct simple precipitation method, it is separated by solid-liquid separation speed Rate is fast, it is more thorough to be separated by solid-liquid separation;Compared with load type adsorbing agent absorption method, method is easily enlarged scale.
3) phosphomolybdate of rubidium caesium is easier to cycling and reutilization in the present invention, more excellent in terms of the separation and Extraction of rubidium caesium resource Gesture.
Detailed description of the invention
Fig. 1 be rubidium in a kind of aqueous solution in an of the invention exemplary embodiments, cesium ion flotation separation method flow chart.
Fig. 2 a is the pictorial diagram of CsCl and ammonium phosphomolybdate mixed solution before flotation in an exemplary embodiments of the invention.
Fig. 2 b is the pictorial diagram of RbCl and ammonium phosphomolybdate mixed solution before flotation in an exemplary embodiments of the invention.
Fig. 2 c be in an of the invention exemplary embodiments reaction time be after twenty minutes that precipitating reagent ammonium phosphomolybdate rubs with cesium chloride Pictorial diagram after the flotation that your ratio is 3:1 (yellow is float product, and colourless is flotation bottom liquid).
Fig. 2 d be in an of the invention exemplary embodiments reaction time be after twenty minutes that precipitating reagent ammonium phosphomolybdate rubs with rubidium chloride Pictorial diagram after the flotation that your ratio is 3:1 (yellow is float product, and colourless is flotation bottom liquid).
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose of the invention Technical solution.The technical solution, its implementation process and principle etc. will be further explained as follows.
The precipitate flotation separation system of rubidium, caesium in a kind of aqueous solution that the one aspect of the embodiment of the present invention provides, packet It includes:
Precipitating reagent includes at least phosphomolybdate;And
Collecting agent and foaming agent include at least cationic surfactant.
In some embodiments, the precipitate flotation separation system further includes stabilizer.
Further, the stabilizer includes No. 2 oil, but not limited to this.
In some embodiments, the phosphomolybdate is preferably ammonium phosphomolybdate, phosphomolybdic acid potassium etc., but not limited to this.
Further, the collecting agent and foaming agent include hexadecyltrimethylammonium chloride, cetyl trimethyl bromine Change in ammonium, dodecyl trimethyl ammonium bromide, octadecyltrimethylammonium chloride, Dodecyl Dimethyl Amine acetate etc. Any one or two or more combinations, but not limited to this, and preferably hexadecyltrimethylammonium chloride and/or cetyl Trimethylammonium bromide.
The precipitate flotation separation system of rubidium, caesium is in floating in the aqueous solution that the other side of the embodiment of the present invention provides Application in choosing separation rubidium ion and/or cesium ion.
The other side of the embodiment of the present invention also provides the flotation separation method of rubidium, cesium ion in a kind of aqueous solution, Include:
Will precipitating reagent, collecting agent and foaming agent be added the aqueous solution containing rubidium ion and/or cesium ion in reaction make rubidium from Son and/or cesium ion precipitating, wherein the precipitating reagent includes at least phosphomolybdate, the collecting agent and foaming agent include at least sun Ionic surface active agent;
The precipitating solid content collecting reaction and obtaining is handled by FLOTATION SEPARATION.
In some preferred embodiments, the flotation separation method specifically includes:
Precipitating reagent is added in the aqueous solution containing rubidium ion and/or cesium ion and be reacted, precipitating solid content is generated, obtains the One intermediate system;
The backward first intermediate system in collecting agent and foaming agent is added, and be uniformly mixed, obtain the second intermediate system;
FLOTATION SEPARATION processing is carried out to the described second intermediate system using floatation separator, collects the precipitating solid Object.
In some preferred embodiments, the flotation separation method further include: to described containing rubidium ion and/or cesium ion Aqueous solution or the first intermediate system in be added stabilizer, the stabilizer includes No. 2 oil.
Specifically, the flotation separation method of rubidium ion and/or cesium ion is (can be with phosphomolybdate in the aqueous solution Ammonium phosphomolybdate or phosphomolybdic acid potassium) be precipitating reagent, the cationic surfactants such as hexadecyltrimethylammonium chloride be collecting agent and Foaming agent, No. 2 oil are stabilizer, carry out the precipitate flotation of rubidium caesium.Ammonium salt solution is regenerative agent.
In some more specifically embodiments, precipitate flotation operating process be can be found in shown in Fig. 1, first by precipitating reagent phosphorus molybdenum Sour ammonium be added to containing rubidium, cesium ion solution in, precipitating completely after, add collecting agent hexadecyltrimethylammonium chloride and Stabilizer, being passed through air and carrying out FLOTATION SEPARATION (can also carry out precipitating reagent and flotation agent while being added in solution precipitating to float Choosing).Gained isolate is regenerated with ammonium salt solution after flotation, can be recycled.
Further, the time of the reaction is 0.1~12h.
Further, the precipitating reagent phosphomolybdate can be arbitrary size, preferably ammonium phosphomolybdate, it is also possible to phosphomolybdic acid Potassium substitution.Rubidium in precipitating reagent and aqueous solution, cesium ion molar ratio be 1:3~3:1.
Further, cationic surfactant is used as collecting agent and foaming agent simultaneously, the collecting agent and foaming agent with The mass volume ratio of aqueous solution is 0.01g/L~0.1g/L, and flotation can be carried out by being added to be greater than 5 minutes in solution after precipitating.
Further, the collecting agent and foaming agent include hexadecyltrimethylammonium chloride, cetyl trimethyl bromine Change in ammonium, dodecyl trimethyl ammonium bromide, octadecyltrimethylammonium chloride, Dodecyl Dimethyl Amine acetate etc. Any one or two or more combinations, but not limited to this, and preferably hexadecyltrimethylammonium chloride and/or cetyl Trimethylammonium bromide.
Further, the flotation separation method includes: to be added among described first by the collecting agent and foaming agent 5min or more is stirred after system, then carries out the FLOTATION SEPARATION processing.
Further, the mass volume ratio of the stabilizer and aqueous solution is 0~0.1g/L.
Further, the aqueous solution includes radioactive liquid waste, but not limited to this.
In some preferred embodiments, the flotation separation method further include: with regenerative agent to FLOTATION SEPARATION rubidium caesium after Float product carry out regeneration treatment.
Further, the regenerative agent includes ammonium salt solution, preferably ammonium chloride, ammonium nitrate solution etc., particularly preferably For ammonium chloride solution.
Further, the concentration of the ammonium salt solution is in 1mol/L or more.
Further, the flotation system after FLOTATION SEPARATION rubidium caesium can be directly entered subsequent cycle after ammonium salt regenerates, and carry out Precipitate flotation.The phosphomolybdate of rubidium caesium is easier to cycling and reutilization in the present invention, more excellent in terms of the separation and Extraction of rubidium caesium resource Gesture.
In conclusion the present invention is provided a kind of using phosphomolybdate as the heavy of precipitating reagent by precipitating-floatation process combination Shallow lake flotation system can be used for the removal of rubidium, cesium ion in the separation and Extraction or radiation waste liquid of rubidium caesium resource, can be in use process The problems such as overcoming the molten damage of support type ammonium phosphomolybdate adsorbent or complicated material preparation.
Below by specific embodiments and drawings, the invention will be further described, but it is above-mentioned to should not be construed the present invention Subject area is only limitted to following embodiments.Without departing from the idea case in the present invention described above, according to the common skill in this field Art knowledge and customary means make various replacements and change, should all include within the scope of the present invention.In the following example The test method of actual conditions is not specified, usually according to normal condition.
Embodiment 1
First to 500mL Cs+Ammonium phosphomolybdate 0.5mmol is added in the CsCl solution of 1mmol/L, is stirred to react 60 minutes Afterwards, hexadecyltrimethylammonium chloride 0.01g, No. 2 oil 0.1mL is added to be placed in flotation cell after stirring 30 minutes and carry out flotation Flotation froth is collected in separation, carries out Cs in flotation substrate+Concentration (calculates to obtain removal rate 95%).
After 2h being sufficiently stirred in the ammonium chloride of the foam addition 100mL 2mol/L of flotation collecting in regenerative process, air-blowing FLOTATION SEPARATION, flotation froth are the flotation system after regeneration, can be used for rubidium, caesium in next step FLOTATION SEPARATION solution.Flotation tail washings For the mixed solution of cesium chloride and ammonium chloride.
Embodiment 2
First to 500mL Rb+Ammonium phosphomolybdate 0.5mmol is added in the RbCl solution of 1mmol/L, is stirred to react 40 minutes Afterwards, hexadecyltrimethylammonium chloride 0.01g, No. 2 oil 0.1mL is added to be placed in flotation cell after stirring 30 minutes and carry out flotation Flotation froth is collected in separation, carries out Rb in flotation substrate+Concentration (calculates to obtain removal rate 93%).
After 2h being sufficiently stirred in the ammonium nitrate of the foam addition 100mL 3mol/L of flotation collecting in regenerative process, air-blowing FLOTATION SEPARATION, flotation froth are the flotation system after regeneration, can be used for rubidium, caesium in next step FLOTATION SEPARATION solution.Flotation tail washings For the mixed solution of rubidium chloride and ammonium nitrate.
Embodiment 3
First to 500mL Cs+Ammonium phosphomolybdate 1.0mmol is added in the CsCl solution of 1mmol/L, is stirred to react 30 minutes Afterwards, hexadecyltrimethylammonium chloride 0.015g, No. 2 oil 0.1mL is added to be placed in flotation cell and floated after stirring 30 minutes Choosing separation, collects flotation froth, carries out Cs in flotation substrate+Concentration (calculates to obtain removal rate 96%).
Regeneration step and embodiment 1 are almost the same.
Embodiment 4
First to 500mL Rb+Ammonium phosphomolybdate 1.0mmol is added in the RbCl solution of 1mmol/L, is stirred to react 20 minutes Afterwards, hexadecyltrimethylammonium chloride 0.015g, No. 2 oil 0.1mL is added to be placed in flotation cell and floated after stirring 30 minutes Choosing separation, collects flotation froth, carries out Rb in flotation substrate+Concentration (calculates to obtain removal rate 95%).
Regeneration step and embodiment 2 are almost the same.
Embodiment 5
First to 500mL Cs+Ammonium phosphomolybdate 0.25mmol is added in the CsCl solution of 1mmol/L, is stirred to react 6 minutes Afterwards, hexadecyltrimethylammonium chloride 0.015g is added to be placed in flotation cell after stirring 80 minutes and carry out FLOTATION SEPARATION, collects Flotation froth carries out Cs in flotation substrate+Concentration (calculates to obtain removal rate 96%).
Regeneration step and embodiment 1 are almost the same.
Embodiment 6
First to 500mLRb+Ammonium phosphomolybdate 0.25mmol is added in the RbCl solution of 1mmol/L, is stirred to react 10 minutes Afterwards, hexadecyltrimethylammonium chloride 0.005g is added, stirring after sixty minutes, is placed in flotation cell and carries out FLOTATION SEPARATION, collects Flotation froth carries out Rb in flotation substrate+Concentration (calculates to obtain removal rate 98%).
Regeneration step and embodiment 2 are almost the same.
Embodiment 7
First to 500mL Cs+Ammonium phosphomolybdate 0.5mmol is added in the CsCl solution of 3mmol/L, after being stirred to react 12h, Hexadecyltrimethylammonium chloride 0.05g, No. 2 oil 0.02g is added to be placed in flotation cell after stirring 90 minutes and carry out flotation point From collection flotation froth carries out Cs in flotation substrate+Concentration (calculates to obtain removal rate 93%).
Regeneration step and embodiment 1 are almost the same.
Embodiment 8
First to 500mLRb+Ammonium phosphomolybdate 0.5mmol is added in the RbCl solution of 3mmol/L, after being stirred to react 10h, adds Enter hexadecyltrimethylammonium chloride 0.04g, No. 2 oil 003g to be placed in flotation cell after stirring 100 minutes and carry out FLOTATION SEPARATION, Flotation froth is collected, Rb in flotation substrate is carried out+Concentration (calculates to obtain removal rate 92%).
Regeneration step and embodiment 2 are almost the same.
Embodiment 9
First to 500mL Cs+Ammonium phosphomolybdate 1.5mmol is added in the CsCl solution of 1mmol/L, is stirred to react 20 minutes Afterwards, hexadecyltrimethylammonium chloride 0.015g, No. 2 oil 0.02g is added to be placed in flotation cell and floated after stirring 30 minutes Choosing separation, collects flotation froth, carries out Cs in flotation substrate+Concentration (calculates to obtain removal rate 95%).
Regeneration step and embodiment 1 are almost the same.
The pictorial diagram of CsCl and ammonium phosphomolybdate mixed solution can be found in Fig. 2 a, reaction time 20 before flotation in the present embodiment After minute, the pictorial diagram after the flotation that precipitating reagent ammonium phosphomolybdate is 3:1 with cesium chloride molar ratio is as shown in Figure 2 c, wherein yellow (scheming right sample) is float product, and colourless (scheming left sample) is flotation bottom liquid.
Embodiment 10
First to 500mL Rb+Ammonium phosphomolybdate 1.5mmol is added in the RbCl solution of 1mmol/L, is stirred to react 20 minutes Afterwards, hexadecyltrimethylammonium chloride 0.015g, No. 2 oil 0.05g is added to be placed in flotation cell and floated after stirring 30 minutes Choosing separation, collects flotation froth, carries out Rb in flotation substrate+Concentration (calculates to obtain removal rate 94%).
Regeneration step and embodiment 2 are almost the same.
The pictorial diagram of RbCl and ammonium phosphomolybdate mixed solution can be found in Fig. 2 b, reaction time 20 before flotation in the present embodiment After minute, the pictorial diagram after the flotation that precipitating reagent ammonium phosphomolybdate is 3:1 with rubidium chloride molar ratio is as shown in Figure 2 d, wherein yellow (scheming left sample) is float product, and colourless (scheming right sample) is flotation bottom liquid.
Reference examples 1
This reference examples, as precipitation reagent, carries out precipitate flotation to rubidium, caesium in radioactive liquid waste using potassium ferrocyanide, but It is that the rubidium caesium sediment that potassium ferrocyanide is formed is difficult to cycling and reutilization.
By 1-10's as a result, present invention is provided by the combination of precipitating-floatation process with phosphomolybdic acid of the embodiment of the present invention Salt is the precipitate flotation system of precipitating reagent, can be used for the removal of rubidium, cesium ion in the separation and Extraction or radiation waste liquid of rubidium caesium resource, The problems such as molten damage of support type ammonium phosphomolybdate adsorbent or complicated material preparation can be overcome in use process.
Each aspect of the present invention, embodiment, feature and example should be regarded as to be illustrative and is not intended to limit in all respects The system present invention, the scope of the present invention are only defined by tbe claims.Without departing substantially from the spirit and scope of the present invention advocated In the case of, it will be apparent to those skilled in the art that other embodiments, modification and use.
The use of title and chapters and sections is not intended to limit the present invention in case of the present invention;Each chapters and sections can be applied to the present invention Any aspect, embodiment or feature.
Case of the present invention in the whole text in, composition is being described as have, containing or comprising in place of specific component or will Process description is in place of having, containing or comprising particular procedure step, it is contemplated that the composition of teachings of this disclosure is also substantially by institute Narration component composition is made of described component, and the process of teachings of this disclosure is also substantially made of described process steps Or it is made of described process steps group.
Unless otherwise specific statement, otherwise term " include (include, includes, including) ", " have The use of (have, has or having) " is it is generally understood that be open and without limitation.
It should be understood that the order of each step or the order of execution specific action are not particularly significant, as long as teachings of this disclosure is protected Holding can operate.In addition, two or more steps or movement can be carried out simultaneously.
In addition, inventor also refers to previous embodiment, other raw materials for being addressed with this specification, technological operation, work Skill condition is tested, and obtains ideal result.
Although describing the present invention with reference to an illustrative embodiment, those skilled in the art will appreciate that, it is not carrying on the back Various other changes can be made in the case where from spirit and scope of the present invention, are omitted and/or are added and can use substantial equivalents Substitute the element of the embodiment.In addition, many modifications can be made without departing substantially from the scope of the present invention so that specific Situation or material adapt to teachings of the present invention.Therefore, it is not to restrict the invention to herein for executing institute of the invention Specific embodiment is disclosed, and being intended to makes the present invention by all implementations comprising falling within the scope of the appended claims Example.In addition, removing non-specific statement, otherwise any use of term first, second etc. does not indicate any order or importance, but An element and another element are distinguished using term first, second etc..
It should be appreciated that above-described is only some embodiments of the present invention, it is noted that for the common of this field For technical staff, under the premise of not departing from concept of the invention, other modification and improvement can also be made, these are all It belongs to the scope of protection of the present invention.

Claims (10)

1. the precipitate flotation separation system of rubidium, caesium in a kind of aqueous solution, characterized by comprising:
Precipitating reagent includes at least phosphomolybdate;And
Collecting agent and foaming agent include at least cationic surfactant.
2. precipitate flotation separation system according to claim 1, it is characterised in that further include stabilizer;Preferably, described Stabilizer includes No. 2 oil;And/or the precipitating reagent includes ammonium phosphomolybdate and/or phosphomolybdic acid potassium;And/or the collecting agent and Foaming agent includes hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, dodecyl trimethyl ammonium bromide, 18 Any one in alkyl trimethyl ammonium chloride, Dodecyl Dimethyl Amine acetate or two or more combinations, preferably Hexadecyltrimethylammonium chloride and/or cetyl trimethylammonium bromide.
3. the precipitate flotation separation system of rubidium in aqueous solution of any of claims 1 or 2, caesium in FLOTATION SEPARATION rubidium ion and/or Application in cesium ion.
4. the flotation separation method of rubidium, cesium ion in a kind of aqueous solution, characterized by comprising:
Will precipitating reagent, collecting agent and foaming agent be added the aqueous solution containing rubidium ion and/or cesium ion in reaction make rubidium ion and/ Or cesium ion precipitating, wherein the precipitating reagent includes at least phosphomolybdate, the collecting agent and foaming agent include at least cation Surfactant;
The precipitating solid content collecting reaction and obtaining is handled by FLOTATION SEPARATION.
5. flotation separation method according to claim 4, it is characterised in that specifically include:
Precipitating reagent is added in the aqueous solution containing rubidium ion and/or cesium ion and is reacted, precipitating solid content is generated, obtains in first Between system;
The backward first intermediate system in collecting agent and foaming agent is added, and be uniformly mixed, obtain the second intermediate system;
FLOTATION SEPARATION processing is carried out to the described second intermediate system using floatation separator, collects the precipitating solid content.
6. flotation separation method according to claim 4 or 5, it is characterised in that further include: to it is described containing rubidium ion and/ Cesium ion aqueous solution or the first intermediate system in be added stabilizer, the stabilizer includes No. 2 oil.
7. flotation separation method according to claim 5, it is characterised in that: the time of the reaction is 0.1~12h;With/ Or, the precipitating reagent includes ammonium phosphomolybdate and/or phosphomolybdic acid potassium;And/or in the precipitating reagent and aqueous solution rubidium ion and/or The molar ratio of cesium ion is 1:3~3:1.
8. flotation separation method according to claim 5, it is characterised in that: the collecting agent and foaming agent include hexadecane Base trimethyl ammonium chloride, cetyl trimethylammonium bromide, dodecyl trimethyl ammonium bromide, octadecyl trimethyl chlorination Any one in ammonium, Dodecyl Dimethyl Amine acetate or two or more combinations, preferably cetyl trimethyl Ammonium chloride and/or cetyl trimethylammonium bromide;And/or the mass volume ratio of the collecting agent and foaming agent and aqueous solution For 0.01g/L~0.1g/L;And/or the flotation separation method includes: that the collecting agent and foaming agent are being added described the 5min or more is stirred after one intermediate system, then carries out the FLOTATION SEPARATION processing.
9. flotation separation method according to claim 6, it is characterised in that: the quality volume of the stabilizer and aqueous solution Than for 0~0.1g/L;And/or the aqueous solution includes radioactive liquid waste.
10. flotation separation method according to claim 4 or 5, it is characterised in that further include: with regenerative agent to flotation point Regeneration treatment is carried out from the float product after rubidium caesium;Preferably, the regenerative agent includes ammonium salt solution, preferably ammonium chloride And/or ammonium nitrate solution, especially preferably ammonium chloride solution;Preferably, the concentration of the ammonium salt solution is in 1mol/L or more.
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