CN103736472A - Gel sphere-type cesium-ion adsorbing agent, preparation method and application thereof - Google Patents
Gel sphere-type cesium-ion adsorbing agent, preparation method and application thereof Download PDFInfo
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- CN103736472A CN103736472A CN201410015386.3A CN201410015386A CN103736472A CN 103736472 A CN103736472 A CN 103736472A CN 201410015386 A CN201410015386 A CN 201410015386A CN 103736472 A CN103736472 A CN 103736472A
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Abstract
The invention relates to a technology for selective separation of metal ions and particularly discloses a gel sphere-type cesium-ion adsorbing agent which is rubidium silicotungstate-calcium alginate gel microspheres. The invention also discloses a preparation method of the adsorbing agent, and an application thereof for separating and extracting cesium from a solution system containing cesium ions. The gel sphere-type cesium-ion adsorbing agent disclosed by the invention has the advantages that the adsorption capacity is high, and the selectivity is good; the radiation resistance and the heat stability are good and the mechanical strength is high; the gel sphere-type cesium-ion adsorbing agent exists in the form of microsphere particles, so that the solid-liquid separation is convenient; the preparation method is simple and convenient, and the production cost is low; the gel sphere-type cesium-ion adsorbing agent can be used for separating and extracting cesium by an adsorbing method and removing radioactive cesium ions and has no secondary pollution.
Description
Technical field
The present invention relates to metalloform-selective isolation technics, specifically openly gel ball-type cesium ion adsorbent, its preparation method and application.
Background technology
Caesium (Cs) is arranged in the first main group period 6 of the periodic table of elements, and it is active metal, is also the rare alkaline metal of high degree of dispersion, expensive.Caesium has very strong chemism and excellent photoelectric effect performance, in medical treatment, electronic device manufacture, the various fields such as catalyze and synthesize and all play an important role.At occurring in nature, caesium mainly exists with ore and two kinds of forms of bittern.
China's caesium aboundresources, the caesium resource existing with solid-state ore deposit forms such as pollucites is mainly distributed in the ground such as Xinjiang, Jiangxi, Sichuan; The Cs existing with bittern form is extensively distributed in Qinghai, Deng Di salt lake, Tibet, GEOTHERMAL WATER, water of oil-gas field.The element symbiosis such as caesium and lithium, sodium, potassium, rubidium, magnesium, calcium, physics, the chemical property of these Coexisting Elements are close, to separation and Extraction, bring certain difficulty.
The separation and Extraction of caesium mainly contains the precipitation method, extraction, absorption method.The precipitation method are only applicable to the system that caesium content is higher, when the content of nuclear waste and Cesium in Bittern Water is lower, process poorly with separated effect by the precipitation method, and precipitation process is more complicated.Solvent extraction is also applicable to the system that caesium content is higher, and the method is high to equipment requirement, technological process more complicated, and organic reagent used also can produce and pollute environment.Absorption method is suitable for separation and Extraction caesium from the lower system of caesium content, has the advantages such as easy and simple to handle, flow process is short, effective, the rate of recovery is high.
Adopt absorption method to process containing caesium system and relate generally to two kinds of situations: (1) using caesium as Resource Access out, is used; (2) caesium is processed as pollutant.For the previous case, should consider absorption, consider again the regeneration of desorption and adsorbent; For latter event, more concerns absorption, and wish that adsorbent is difficult for regeneration, like this by after radiocesium absorption, caesium is difficult for running off, and is difficult for causing secondary pollution, is convenient to the follow-up processing such as bury.
CN200810147723.9 discloses the processing method of the micro-contaminated soil of a kind of radiocesium.Adopt bar screen, two plate sieve and spiral screen to sieve the micro-contaminated soil of radiocesium, sift out thicker grogs, then by subtracting the micro-contaminated soil of radiocesium after appearance and have a liking for the active bacterium liquid of the ferrous Thiobacillus of acid oxidase and mix in microorganism dissolution reactor, with the radiocesium in the micro-contaminated soil of dissolution to liquid phase; Containing radiocesium solution, transfer to microbial adsorption precipitation reactor, by regulating pH value, utilize sulfate reducing bacteria activity bacterium liquid that the radiocesium of transferring in liquid phase is precipitated.Utilize the method can remove efficiently, quickly the radiocesium in micro-contaminated soil.
CN201110179500.2 provides a kind of preparation method of magnetic caesium selective absorbent.By Ni (NO
3)
2solution slowly adds K
4fe (CN)
6-CH
3cOOH solution, solution drips follow-up continuous reaction a period of time completely, after reaction finishes, quiescent settling, the supernatant that inclines, last, filtration, washing precipitation, dry constant weight for 110 ℃.Synthetic adsorbent be pure inorganic material higher to the distribution coefficient of Cs, selectively good, exchange velocity is fast, large, the anti-irradiation of this adsorbent exchange capacity and thermal stability are good and have a good hydrolytic stability, can carry out column operation, can also carry out Magnetic Isolation, be applicable to various low processing of putting containing Cs waste water.
CN201210301959.X discloses the preparation method of another magnetic caesium selective absorbent.First to Ni powder and K
4fe (CN)
63H
2in the mixture of O, add deionized water, make K
4fe (CN)
63H
2o dissolves completely, then gained dissolved matter is placed under water bath with thermostatic control, dropwise add wherein HCl solution, continuous stirring reaction a period of time, by gained reactant at room temperature static ageing a period of time, treat that crystalline structure growth is complete, next the precipitation generating with deionized water washing, until cleaning solution is water white transparency, and pH value substantially constant till, finally being deposited under constant temperature after washing is dried to constant weight, obtains ferrocyanide nickel potassium-nickel adsorbent.Adopt this sorbent treatment can obtain good volume reduction ratio and decontamination factor containing caesium waste liquid.
CN201210241779.7(relates to the caesium adsorbent of preparing with potassium ferrocyanide spherical particles), CN201110179500.2 and US6046131(relate to the caesium adsorbent of preparing with the iron cyanide), US6616860B1(relates to the caesium adsorbent of preparing with heteropolyacid salt), although disclose the preparation method of the caesium adsorbent of different compositions, absorption property also carried out to certain description.But because the composition of actual salt lake bittern, oil field water, GEOTHERMAL WATER system is complicated, micro-cesium ion wherein and multiple other Ordinary ion coexist, and the Ordinary ion coexisting disturbs very large to the adsorbing separation of cesium ion.Based on the disclosed technology of existing patent, can not realize the separated of cesium ion and other ion in the complex systems such as salt lake bittern, oil field water, GEOTHERMAL WATER.
Therefore, also need that a kind of approach is with separation and Extraction cesium ion more effectively, easily.
Summary of the invention
The present invention is intended to overcome the above defect of prior art, provide a kind of can be from the approach of complicated ingredient system separation and Extraction caesium.
One aspect of the present invention provides a kind of gel ball-type cesium ion adsorbent, and described adsorbent is silico-tungstic acid rubidium-calcium alginate gel bead.
In some embodiment, described gel micro-ball can have 1.5 to 2.5mm, for example the particle diameter of 2mm.
In some embodiment, in described gel micro-ball, the amount ratio of silico-tungstic acid rubidium and calcium alginate can be 1:(5-100).
The present invention provides a kind of method of preparing described gel ball-type cesium ion adsorbent on the other hand, comprises step: the S1 mixing sodium alginate hydrosol and silico-tungstic acid rubidium, form colloidal sol mixed liquor; S2 splashes into calcium chloride solution by described colloidal sol mixed liquor, and ageing, separation, obtain gel micro-ball; S3 washs described gel micro-ball to free from admixture ion.
In some embodiment, described silico-tungstic acid rubidium can prepare by following steps: silicon tungsten acid solution is mixed with ribidium salt solution, generate precipitation; Dry described precipitation to remove moisture, obtain silico-tungstic acid rubidium solid.
In some embodiment, the concentration of the described sodium alginate hydrosol can be 2-2.5%(quality), the mass ratio of the described sodium alginate hydrosol and silico-tungstic acid rubidium can be (5-100): 1.
In some embodiment, the concentration of described calcium chloride solution can be 4-5%(quality).
In some embodiment, digestion time can be 12 to 48 hours.
Further aspect of the present invention provides a kind of method from the solution system separation and Extraction caesium that comprises cesium ion, and described method is used described gel ball-type cesium ion adsorbent of the present invention to carry out static state and/or Dynamic Adsorption.
In some embodiment, described solution system can be salt lake bittern, oil field water, GEOTHERMAL WATER, alkali metal ion coexist system, level radioactive nuclear waste.
The spherical cesium ion adsorbent of gel of the present invention is to the radioresistance of cesium ion and Heat stability is good, and mechanical strength is high; For microsphere particle, be convenient to Separation of Solid and Liquid, can carry out column operation; Its preparation method technique is simple, production cost is low; In lithium, sodium, potassium, rubidium, cesium ion competition system and bittern, high to the adsorption capacity of caesium, selectively good; Can be used for absorption method and remove the cesium ion in level radioactive nuclear waste, non-secondary pollution, cesium ion in separation and Extraction alkali metal ion competition system and bittern, and the cesium ion that coexists in system of the separated bittern of dynamic adsorption method, oil field water, GEOTHERMAL WATER and alkali metal ion, unrestricted to the content of cesium ion.
Accompanying drawing explanation
Fig. 1 is according to the photo of gel ball-type cesium ion adsorbent of the present invention.
Fig. 2 is the XRD figure according to silico-tungstic acid rubidium-Ca-alginate gel beads of the present invention.
Fig. 3 is the SEM figure according to silico-tungstic acid rubidium-Ca-alginate gel beads of the present invention.
Fig. 4 illustrates and uses gel ball-type cesium ion adsorbent of the present invention, in competition system during Static Adsorption different ions, and the contrast situation of adsorbance.
Fig. 5 illustrates and uses gel ball-type cesium ion adsorbent of the present invention, in simulation bittern during Static Adsorption different ions, and the contrast situation of adsorbance.
Fig. 6 illustrates and uses gel ball-type cesium ion adsorbent of the present invention, the breakthrough curve of Dynamic Adsorption simulation bittern.
The specific embodiment
Below in conjunction with specific embodiment and accompanying drawing, the present invention is described in further detail.
Gel ball-type cesium ion adsorbent of the present invention is silico-tungstic acid rubidium-calcium alginate gel bead.It is the gel micro-ball being formed by silico-tungstic acid rubidium and calcium alginate.As shown in fig. 1, this gel micro-ball is white spheric granules, has the particle diameter that is about 2mm, and for example particle diameter can be in 1.5 to 2.5mm scope.
This gel ball-type cesium ion adsorbent can prepare by the following method.
First the mixing sodium alginate hydrosol and silico-tungstic acid rubidium, form colloidal sol mixed liquor.Particularly, for example, prepare the sodium alginate hydrosol, its mass fraction can be 2% to 2.5%.Stir a period of time, for example standing to without bubble after 2 to 12 hours, form the sodium alginate hydrosol.This sodium alginate hydrosol is mixed with silico-tungstic acid rubidium pressed powder, to form uniform colloidal sol mixed liquor, wherein the mass ratio of the sodium alginate hydrosol and silico-tungstic acid rubidium pressed powder can be 5:1 to 100:1 again.
Active ingredient silico-tungstic acid rubidium can be prepared as follows: prepare silicon wolframic acid solution and ribidium salt solution, and two kinds of solution are fully mixed to produce precipitation, after removing moisture, oven dry obtains silico-tungstic acid rubidium solid.For example, take 10 to 60g silico-tungstic acid solids and be dissolved in 6 to 40mL water, after filtration, filtrate is fully mixed with 5 to 70mL, 0.5 ribidium salt solution to 5mol/L, produce precipitation, dry 2 to 24 hours to remove moisture in 30 ℃ to 100 ℃, obtain silico-tungstic acid rubidium pressed powder.
Then, this mixture is splashed in calcium chloride water to produce gel, after ageing, Separation of Solid and Liquid, obtains gel micro-ball.The concentration of calcium chloride water used herein can be for example 4-5%(quality); Digestion time can be for example 12 to 48 hours.
Finally, for example, use distilled water, wash described gel micro-ball, to free from admixture ion.
The gel ball-type cesium ion adsorbent obtaining is silico-tungstic acid rubidium-calcium alginate, i.e. RbWSi-Ca (ALG)
2.
Fig. 2 and Fig. 3 illustrate respectively X-ray diffraction (XRD) figure and SEM (SEM) figure that obtains product produced according to the present invention.According to XRD figure, can confirm that product is silico-tungstic acid rubidium-calcium alginate.Visible according to SEM figure, gel micro-ball pattern is even, and silico-tungstic acid rubidium powder is evenly coated by calcium alginate.
Silico-tungstic acid rubidium-calcium alginate gel bead of the present invention, can be used as cesium ion adsorbent, for the complicated ingredient system from comprising cesium ion, by absorption method (Dynamic Adsorption and/or Static Adsorption), separation and Extraction cesium ion.For example, can be applied to from salt lake bittern, oil field water, GEOTHERMAL WATER, the alkali metal ion system that coexists, etc. separation and Extraction cesium ion in system, and for the treatment of level radioactive nuclear waste.
Gel ball-type cesium ion adsorbent adsorption capacity of the present invention is high, selectively good, and time of equilibrium adsorption is shorter, and radioresistance and Heat stability is good, mechanical strength are high; This adsorbent is microsphere particle, is convenient to Separation of Solid and Liquid, can carry out column operation, especially can be for by the cesium ion in dynamic adsorption method separation and Extraction salt lake bittern, and easy desorption, can make Dynamic Adsorption post recycle.Its preparation methods steps is few, technique is simple, flow process is short, cost is low, be convenient to suitability for industrialized production.
Gel ball-type cesium ion adsorbent of the present invention is in lithium, sodium, potassium, rubidium, caesium alkali metal ion competition system and bittern, high to the adsorption capacity of caesium, selectively good; Can be used for absorption method and remove the cesium ion in level radioactive nuclear waste, non-secondary pollution; Cesium ion in absorption method separation and Extraction alkali metal ion competition system and bittern; The cesium ion that the separated bittern of dynamic adsorption method, oil field water, GEOTHERMAL WATER and alkali metal ion coexist in system, and unrestricted to the content of cesium ion.
In addition, in adsorbent of the present invention, the tradable cation of adsorbent active ingredient is rubidium ion, and this adsorbent is particularly suitable for adsorbing separation caesium from the mixed solution of rubidium, caesium.
Embodiment
Further set forth by the following examples the present invention, these embodiment are only presented for purposes of illustration, do not limit the scope of the invention.The test method of unreceipted actual conditions in the following example, conventionally according to normal condition.
preparation Example 1
The sodium alginate hydrosol that preparation mass fraction is 2%; The sodium alginate hydrosol be take with silico-tungstic acid rubidium powder mass ratio as 5:1 mixes rear formation colloidal sol mixed liquor; Colloidal sol mixed liquor is splashed in 4% calcium chloride solution, make gel ageing 48 hours, after Separation of Solid and Liquid, obtain gel ball, be washed with distilled water to free from admixture ion.
preparation Example 2
The sodium alginate hydrosol that preparation mass fraction is 2.5%; The sodium alginate hydrosol be take with silico-tungstic acid rubidium powder mass ratio as 100:1 mixes rear formation colloidal sol mixed liquor; Colloidal sol mixed liquor is splashed in 5% calcium chloride solution, make gel ageing 12 hours, after Separation of Solid and Liquid, obtain gel ball, be washed with distilled water to free from admixture ion.
preparation Example 3
The sodium alginate hydrosol that preparation mass fraction is 2.5%; The sodium alginate hydrosol be take with silico-tungstic acid rubidium powder mass ratio as 10:1 mixes rear formation colloidal sol mixed liquor; Colloidal sol mixed liquor is splashed in 5% calcium chloride solution, make gel ageing 20 hours, after Separation of Solid and Liquid, obtain gel ball, and be washed with distilled water to free from admixture ion.
preparation Example 4
The sodium alginate hydrosol that preparation mass fraction is 2.5%; The sodium alginate hydrosol be take with silico-tungstic acid rubidium powder mass ratio as 50:1 mixes rear formation colloidal sol mixed liquor; Colloidal sol mixed liquor is splashed in 5% calcium chloride solution, make gel ageing 24 hours, after Separation of Solid and Liquid, obtain gel ball, be washed with distilled water to free from admixture ion.
application Example 1
In the mixed alkali metal solion of alkali metal ion competition system: 50mL, comprise LiCl, NaCl, KCl, RbCl, the CsCl that concentration is 0.01mol/L.Static Adsorption operation, adsorption temp is room temperature, without regulator solution pH value.
Absorption situation is referring to Fig. 4, and as seen from the figure, in this alkali metal ion competition system, adsorbent does not adsorb Li substantially
+, Na
+, K
+, Rb
+, to cesium ion show good selectively and stronger adsorption capacity.
application Example 2
Analog salt lake bittern water system: 50mL, comprising lithium, sodium, potassium, magnesium, rubidium, caesium plasma.Static Adsorption operation, adsorption temp is room temperature, without regulator solution pH value.
Absorption situation is referring to Fig. 5, and as seen from the figure, adsorbent is to Li
+, Na
+, K
+, Mg
2+, Cs
+all there is absorption.In Static Adsorption simulation bittern during different metal ion, this adsorbent to cesium ion do not show good selectively and stronger adsorption capacity.
application Example 3
Analog salt lake bittern water system: comprising lithium, sodium, potassium, magnesium, rubidium, caesium plasma.Dynamic Adsorption operation, adsorption temp is room temperature, without regulator solution pH value.
Absorption situation, referring to Fig. 6, can be found out by breakthrough curve, for simulation bittern system, Li
+, Na
+, K
+, Rb
+, Mg
2+in 20mL left and right, place penetrates, and Cs
+in 500mL left and right, place penetrates, and shows Cs
+in post adsorption process and Li
+, Na
+, K
+, Rb
+, Mg
2+ion obtains good separation.That is,, when Dynamic Adsorption is simulated the cesium ion in bittern, adsorbent of the present invention has shown good separating effect to cesium ion.
The above the specific embodiment of the present invention, does not form limiting the scope of the present invention.Various other corresponding changes and distortion that any technical conceive according to the present invention has been done, all should be included in the protection domain of the claims in the present invention.
Claims (10)
1. a gel ball-type cesium ion adsorbent, is characterized in that, described adsorbent is silico-tungstic acid rubidium-calcium alginate gel bead.
2. adsorbent as claimed in claim 1, wherein, described gel micro-ball has 1.5 to 2.5mm particle diameter.
3. adsorbent as claimed in claim 1, wherein, in described gel micro-ball, the mass ratio of silico-tungstic acid rubidium and calcium alginate is 1:(5-100).
4. the method for the gel ball-type cesium ion adsorbent described in any one in preparation claims 1 to 3, is characterized in that, comprises step:
The S1 mixing sodium alginate hydrosol and silico-tungstic acid rubidium, form colloidal sol mixed liquor;
S2 splashes into calcium chloride solution by described colloidal sol mixed liquor and forms gel, and ageing, separation obtain gel micro-ball;
S3 washs described gel micro-ball to free from admixture ion.
5. method as claimed in claim 4, wherein, described silico-tungstic acid rubidium prepares by following steps:
Silicon tungsten acid solution is mixed with ribidium salt solution, generate precipitation;
Dry described precipitation to remove moisture, obtain silico-tungstic acid rubidium solid.
6. method as claimed in claim 4, wherein,
The concentration of the described sodium alginate hydrosol is 2-2.5%(quality),
The mass ratio of the described sodium alginate hydrosol and silico-tungstic acid rubidium is (5-100): 1.
7. method as claimed in claim 4, wherein, the concentration of described calcium chloride solution is 4-5%(quality).
8. method as claimed in claim 4, wherein, digestion time is 12 to 48 hours.
9. from a method for the solution system separation and Extraction caesium that comprises cesium ion, it is characterized in that, described method is used gel ball-type cesium ion adsorbent as claimed any one in claims 1 to 3 to carry out static state and/or Dynamic Adsorption.
10. method as claimed in claim 9, wherein, described solution system is salt lake bittern, oil field water, GEOTHERMAL WATER, alkali metal ion coexist system, level radioactive nuclear waste.
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| CN106415733A (en) * | 2014-05-28 | 2017-02-15 | Itn纳诺维森股份公司 | Method and system for removing radioactive nuclides from water |
| CN109824068A (en) * | 2019-04-03 | 2019-05-31 | 陕西省膜分离技术研究院有限公司 | Rb is extracted from low concentration brine+And the method for preparing high-purity rubidium salt |
| CN111511451A (en) * | 2015-12-16 | 2020-08-07 | 哈里发科学技术大学 | Calcium alginate adsorbent |
| CN115608330A (en) * | 2022-09-29 | 2023-01-17 | 一重集团大连工程技术有限公司 | Composite microsphere adsorbent for removing radioactive cesium and preparation method thereof |
| CN116159546A (en) * | 2023-02-14 | 2023-05-26 | 干霸干燥剂(深圳)有限公司 | High-moisture-absorption resin desiccant and preparation method thereof |
| CN116283277A (en) * | 2023-02-03 | 2023-06-23 | 清华大学 | Method for loading cesium nitrate on ceramic microspheres |
| CN116371348A (en) * | 2023-04-23 | 2023-07-04 | 燕山大学 | Preparation method and application of cesium fixation material |
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| CN116283277A (en) * | 2023-02-03 | 2023-06-23 | 清华大学 | Method for loading cesium nitrate on ceramic microspheres |
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| CN116371348A (en) * | 2023-04-23 | 2023-07-04 | 燕山大学 | Preparation method and application of cesium fixation material |
| CN116371348B (en) * | 2023-04-23 | 2023-09-26 | 燕山大学 | Preparation method and application of cesium fixation material |
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| CN103736472B (en) | 2016-01-20 |
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