CN105845188A - Method for adsorption separation of strontium - Google Patents
Method for adsorption separation of strontium Download PDFInfo
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- CN105845188A CN105845188A CN201610177218.3A CN201610177218A CN105845188A CN 105845188 A CN105845188 A CN 105845188A CN 201610177218 A CN201610177218 A CN 201610177218A CN 105845188 A CN105845188 A CN 105845188A
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- strontium
- nitrate solution
- adsorbing separation
- adsorbent
- chromatographic column
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for adsorption separation of strontium. The method comprises the following steps: passing nitrate solution containing a variety of metal ions through a chromatographic column filled with an adsorbent to ensure that the element strontium is adsorbed by the adsorbent, and performing elution on the chromatographic column after adsorption to obtain the element strontium respectively, wherein the adsorbent is prepared by loading a compound shown by a structural formula (I) on a carrier; and the nitrate solution contains Sr (II) and other metal ions, and the other metal ions are at least one of Li (I), Na (I), K (I), Rb (I), Ba (II), Ce (III), Pd (II), Ca (II), and Mg (II). According to the method for adsorption separation of strontium, disclosed by the invention, separation is performed under a weakly acidic (nearly neutral) condition, the condition is mild, the selectivity is good, the separation speed is high, and the operation is simple, so that the method is easy to popularize.
Description
Technical field
The present invention relates to element sepatation technical field, a kind of method being specifically related to adsorbing separation strontium.
Background technology
Being widely used in bring to the mankind of nuclear energy various simultaneously also brings huge health easily
Threaten, during using nuclear energy, often produce a large amount of radioactive waste, these waste degradations
Time is long, easily causes serious environmental pollution, the most safely and effectively processes these radioactivity and discards
Thing has become as the key factor of restriction nuclear energy sustainable development.
Low-activity waste liquid is the important component part of radioactive waste, conventional process low radioactive waste liquid
Method has absorption method, ion exchange and membrane separation process, and the number of devices involved by these methods is numerous,
Treatment process steps is complicated；During owing to processing low radioactive waste liquid, waste liquid is often through a kind of equipment or structures
Shi Douhui causes radioactive pollution, and therefore in processing procedure, number of devices is the most, and processing step is the most complicated,
The pollution caused is the most serious, therefore should reduce number of devices as far as possible, shortens processing technological flow.
Low-activity waste liquid exists heating element strontium, needs to separate, it addition, in desalinization
And salt lake saline process field, also face the separation problem of elements strontium.
Summary of the invention
A kind of method that the invention provides adsorbing separation strontium, the most efficiently, selectivity is good, separates speed
Degree is fast.
A kind of method of adsorbing separation strontium, comprises the steps: the nitrate containing many kinds of metal ions
Solution is by being filled with the chromatographic column of adsorbent, and elements strontium is adsorbed by adsorbent, to the chromatograph after absorption
Post carries out eluting, respectively obtains elements strontium, and described adsorbent is by the chemical combination as shown in structure formula (I)
Thing is supported on carrier and makes:
Containing Sr (II) and other metal ions in described nitrate solution, other metal ions be Li (I),
In Na (I), K (I), Rb (I), Ba (II), Ce (III), Pd (II), Ca (II), Mg (II) at least one
Kind.
Adsorbent in the present invention is by the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons (English name р-tert
-butysulfonycalix [4] arene, as shown in structure formula (I)) and carrier carry out multiple by a certain percentage
Conjunction prepares.
As preferably, described carrier is the macro-pore SiO of coating polymer2。
The macro-pore SiO of described coating polymer2For silica-based-styrene-divinylbenzene polymer
(SiO2-P), it is a class novel inorganic/organic support material, disclosed in United States Patent (USP) US6843921
SiO2-styrene-divinylbenzene polymer, SiO2-P is a kind of containing porous silicon dioxide carrier
Organic high polymer complex carrier of grain, its preparation method is as follows:
(1) by the SiO of macropore2It is washed till neutrality with concentrated nitric acid washing, sucking filtration, deionized water, repeats
More than 10 times, it is dried.
(2) vacuum under the conditions of having argon shield, with glyceryl trichloride and m-dimethylbenzene as solvent,
To macro-pore SiO2The m/p-formyl styrene of middle addition 48.7g, the m/p-divinylbenzene of 8.9g,
72.2g dioctyl faces phthalic acid ester, 54.0g benzoin methyl acid sodium, 0.56g α, α-idol bis-isobutyronitrile
And 0.57g1,1 '-even hexanamine-1-nitrile, room temperature it is gradually heated to 90 DEG C, and keeps 13 hours, it
After, progressively it is cooled to room temperature.
(3) respectively with acetone and methanol washing, the above-mentioned product of sucking filtration, repeat more than 10 times, be dried.
In the present invention, the preparation method of described adsorbent is as follows:
By the compound dissolution as shown in structure formula (I) in dichloromethane, add in gained solution
Enter carrier mix homogeneously, steam through rotation dried, obtain adsorbent.
When rotation is steamed, make major part dichloromethane evaporate into nearly dry state, inhale in capillarity and physics
Under attached effect, compound molecule enters in the space of carrier, and the material of the most dry state exists
It is vacuum dried at 45～55 DEG C at least 24 hours, obtains adsorbent.
As preferably, every g compound dissolution as shown in structure formula (I) is in 130～150mL dichloromethanes
In alkane.The macro-pore SiO of coating polymer2Quality is the compound quality shown in structure formula (I) 8～
10 times.
In order to ensure separating effect, it is preferable that chromatographic column column temperature is 25 ± 5 DEG C.Containing various metals
The nitrate solution of ion flow velocity in the chromatography column is 0.1mL/min～3mL/min.To ensure metal
Ion is fully contacted absorption with the adsorbent in chromatographic column.
In nitrate solution, the concentration of metal ion and the pH value of nitrate solution all can affect separation
Effect, it is preferable that in nitrate solution, the concentration of every metal ion species is 5.0 × 10-4～1.0 × 10-3M。
The pH scope of nitrate solution is 6～7.
In order to strengthen separating effect, use as nitrate solution the aqueous solution of nitric acid of pH value to absorption
Saturated chromatographic column is washed, and is rinsed out by other the most adsorbed metallic elements, then utilizes
Elements strontium is resolved by water with the form drip washing of nitrate, completes the separation of elements strontium, the completeest
Become the regeneration of chromatographic column.
The method of adsorbing separation strontium of the present invention, separates under the conditions of faintly acid (close to neutral),
Mild condition, selectivity is good, and separating rate is fast, simple to operate, it is easy to promote.
Accompanying drawing explanation
Fig. 1 is in the embodiment of the present invention 4～10, and the adsorption isothermequation of elements strontium closes with the change of pH value
System's figure.
Detailed description of the invention
Embodiment 1
0.5g is dissolved in 70.0mL to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons (as shown in structure formula (I))
In dichloromethane, fully dissolve, gained solution adds 4.5gSiO2-P stirs, and makes SiO2-P
Mix homogeneously with to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons, make dichloromethane wave through decompression rotary evaporation
Send out major part and do state to material near, under capillarity and physisorption, make organic molecule
Enter SiO2In-P aperture, the material of the most dry state is vacuum dried 24h at 45 DEG C, obtains
Adsorbent.
Embodiment 2
0.5g is dissolved in 75.0mL to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons (as shown in structure formula (I))
In dichloromethane, fully dissolve, gained solution adds 4.0gSiO2-P stirs, and makes SiO2-P
Mix homogeneously with to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons, make dichloromethane wave through decompression rotary evaporation
Send out major part and do state to material near, under capillarity and physisorption, make organic molecule
Enter SiO2In-P aperture, the material of the most dry state is vacuum dried 24h at 50 DEG C, obtains
Adsorbent.
Embodiment 3
0.5g is dissolved in 80.0mL to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons (as shown in structure formula (I))
In dichloromethane, fully dissolve, gained solution adds 5.0gSiO2-P stirs, and makes SiO2-P
Mix homogeneously with to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons, make dichloromethane wave through decompression rotary evaporation
Send out major part and do state to material near, under capillarity and physisorption, make organic molecule
Enter SiO2In-P aperture, the material of the most dry state is vacuum dried 24h at 55 DEG C, obtains
Adsorbent.
Embodiment 4～10
(1) by alkali metal salt LiNO3、NaNO3、KNO3、RbNO3；Alkali salt Mg (NO3)2、
Ca(NO3)2、Sr(NO3)2、Ba(NO3)2、Ce(NH4)2(NO3)6It is dissolved in salpeter solution, is subsequently adding
Precious metals pd (5%w/w) nitrate solution, is configured to contain the nitric acid of many kinds of metal ions simultaneously
Saline solution.
(2) in nitrate solution, concentrated nitric acid and deionized water are added, the pH of regulation nitrate solution
Being respectively 1,2,3,4,5,6,7, the concentration of every metal ion species is 5.0 × 10-4M。
(3) absorbent filling embodiment 1 prepared is the chromatograph of ID10mm × h300mm to specification
In post, the flow velocity setting flowing phase is 298K as 1mL/min, the temperature of chromatographic column.
(4) nitrate solution that step (2) has adjusted pH passes through the chromatographic column equipped with adsorbent,
Elements strontium is filled the chromatographic column absorption of adsorbent.
(5) aqueous solution of nitric acid (pH of the pH value of aqueous solution of nitric acid and corresponding nitrate solution is utilized
Being worth identical, such as, the pH value of nitrate solution is 1, then the aqueous solution of nitric acid using pH to be 1 is carried out
Washing) chromatographic column being adsorbed with elements strontium is washed, flush out that adsorbent do not adsorbs other
Metallic element.
(6) after the adsorbent in chromatographic column is saturated, with water by elements Sr with the form of nitrate
Drip washing resolves, and completes the separation of elements Sr.
The absorption result of embodiment 4～10 as it is shown in figure 1, in Fig. 1 abscissa be pH value, vertical coordinate is for inhaling
Fufen distribution coefficient Kd, unit is cm3/ g, as seen from Figure 1, when the pH of nitrate solution is 6,
The adsorption isothermequation of strontium is 120cm3/g；When the pH of nitrate solution is 7, the absorption distribution of strontium
Coefficient is 140cm3/ g, in the range of pH6～7, elements Sr all has preferable separating effect.
Embodiment 11
Absorbent filling embodiment 2 prepared is in chromatographic column, and remaining operating condition is with implementing
Example 9.
Embodiment 12
Absorbent filling embodiment 3 prepared is in chromatographic column, and remaining operating condition is with implementing
Example 9.
Claims (8)
1. the method for an adsorbing separation strontium, it is characterised in that comprise the steps: containing multiple
The nitrate solution of metal ion is by being filled with the chromatographic column of adsorbent, and elements strontium is adsorbed agent and inhales
Attached, the chromatographic column after absorption is carried out eluting, respectively obtains elements strontium, described adsorbent is by such as structure
Compound loaded shown in formula (I) is made on carrier:
Containing Sr (II) and other metal ions in described nitrate solution, other metal ions be Li (I),
In Na (I), K (I), Rb (I), Ba (II), Ce (III), Pd (II), Ca (II), Mg (II) at least one
Kind.
2. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that described carrier is
The macro-pore SiO of coating polymer2。
3. the method for adsorbing separation strontium as claimed in claim 2, it is characterised in that coating polymer
Macro-pore SiO2Quality is the compound quality shown in structure formula (I) 8～10 times.
4. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that nitrate solution
In, the concentration of every metal ion species is 5.0 × 10-4～1.0 × 10-3M。
5. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that nitrate solution
PH scope be 6～7.
6. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that containing multiple gold
The nitrate solution of genus ion flow velocity in the chromatography column is 0.1mL/min～3mL/min.
7. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that described adsorbent
Preparation method as follows:
By the compound dissolution as shown in structure formula (I) in dichloromethane, add in gained solution
Enter carrier mix homogeneously, steam through rotation dried, obtain adsorbent.
8. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that chromatographic column column temperature
It it is 25 ± 5 DEG C.
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| CN201610177218.3A CN105845188B (en) | 2016-03-24 | 2016-03-24 | A kind of method of adsorbing separation strontium |
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| CN201610177218.3A CN105845188B (en) | 2016-03-24 | 2016-03-24 | A kind of method of adsorbing separation strontium |
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| CN105845188B CN105845188B (en) | 2017-11-17 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629978A (en) * | 2016-12-30 | 2017-05-10 | 北京师范大学 | Adsorption and regeneration integrated reactor system for radioactive wastewater treatment |
| CN106673108A (en) * | 2016-12-26 | 2017-05-17 | 浙江大学 | Method for separating sodium from salt lake |
| CN114999701A (en) * | 2022-05-31 | 2022-09-02 | 中国核动力研究设计院 | Strontium [ 2 ] 90 Sr]-yttrium [ alpha ], [ alpha ] and [ alpha ] or 90 Y]Generator and separation method |
| CN116139834A (en) * | 2021-11-19 | 2023-05-23 | 中核四0四有限公司 | Preparation method of adsorption chromatographic material for strontium in high-level radioactive waste liquid |
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| US20070158271A1 (en) * | 2006-01-12 | 2007-07-12 | Draxis Health Inc. | Systems and Methods for Radioisotope Generation |
| CN101143273A (en) * | 2007-07-06 | 2008-03-19 | 浙江大学 | Method for separating heating element Cs and Sr from high radioactive waste |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673108A (en) * | 2016-12-26 | 2017-05-17 | 浙江大学 | Method for separating sodium from salt lake |
| CN106673108B (en) * | 2016-12-26 | 2019-10-29 | 浙江大学 | A method of separating sodium from salt lake |
| CN106629978A (en) * | 2016-12-30 | 2017-05-10 | 北京师范大学 | Adsorption and regeneration integrated reactor system for radioactive wastewater treatment |
| CN116139834A (en) * | 2021-11-19 | 2023-05-23 | 中核四0四有限公司 | Preparation method of adsorption chromatographic material for strontium in high-level radioactive waste liquid |
| CN114999701A (en) * | 2022-05-31 | 2022-09-02 | 中国核动力研究设计院 | Strontium [ 2 ] 90 Sr]-yttrium [ alpha ], [ alpha ] and [ alpha ] or 90 Y]Generator and separation method |
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| CN105845188B (en) | 2017-11-17 |
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