CN105845188B - A kind of method of adsorbing separation strontium - Google Patents
A kind of method of adsorbing separation strontium Download PDFInfo
- Publication number
- CN105845188B CN105845188B CN201610177218.3A CN201610177218A CN105845188B CN 105845188 B CN105845188 B CN 105845188B CN 201610177218 A CN201610177218 A CN 201610177218A CN 105845188 B CN105845188 B CN 105845188B
- Authority
- CN
- China
- Prior art keywords
- strontium
- adsorbent
- adsorbing separation
- chromatographic column
- nitrate solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
Abstract
The invention discloses a kind of method of adsorbing separation strontium, comprise the following steps：Nitrate solution containing various metals ion is by being filled with the chromatographic column of adsorbent, elements strontium is adsorbed by adsorbent, chromatographic column after absorption is eluted, respectively obtains elements strontium, the adsorbent is made up of compound loaded as shown in structure formula (I) on carrier；Contain Sr (II) and other metal ions in the nitrate solution, other metal ions are at least one of Li (I), Na (I), K (I), Rb (I), Ba (II), Ce (III), Pd (II), Ca (II), Mg (II).The method of adsorbing separation strontium of the present invention, separated under the conditions of faintly acid (close to neutrality), mild condition, selectivity is good, and separating rate is fast, simple to operate, easy to spread.
Description
Technical field
The present invention relates to element sepatation technical field, and in particular to a kind of method of adsorbing separation strontium.
Background technology
Being widely used in for nuclear energy also brings huge health threat while bringing various convenient to the mankind, using
A large amount of radioactive wastes are often produced during nuclear energy, these waste degradation times length, easily cause serious environment
Pollution, how safely and effectively to handle these radioactive wastes and have become the key factor for restricting nuclear energy sustainable development.
Low-activity waste liquid is the important component of radioactive waste, and the method for conventional processing low radioactive waste liquid has absorption
Method, ion-exchange and membrane separation process, the number of devices involved by these methods is numerous, and treatment process steps are complicated；Due to place
When managing low radioactive waste liquid, waste liquid when a kind of equipment or structures often by can all cause radioactive pollution, therefore set in processing procedure
Standby number is more, and processing step is more complicated, caused by pollute more serious, therefore should try one's best and reduce number of devices, shorten and handle work
Skill flow.
Heating element strontium in low-activity waste liquid be present, it is necessary to be separated, in addition, at desalinization and salt lake saline
Reason field, also face the separation problem of elements strontium.
The content of the invention
The invention provides a kind of method of adsorbing separation strontium, succinct efficient, selectivity is good, and separating rate is fast.
A kind of method of adsorbing separation strontium, comprises the following steps：Nitrate solution containing various metals ion is by filling out
Chromatographic column equipped with adsorbent, elements strontium are adsorbed by adsorbent, and the chromatographic column after absorption is eluted, respectively obtains element
Strontium, the adsorbent are made up of compound loaded as shown in structure formula (I) on carrier：
Contain Sr (II) and other metal ions in the nitrate solution, other metal ions are Li (I), Na (I), K
(I), at least one of Rb (I), Ba (II), Ce (III), Pd (II), Ca (II), Mg (II).
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 compound be prepared by a certain percentage.
Preferably, the carrier is the macro-pore SiO of coated polymer2。
The macro-pore SiO of the coated polymer2For silicon substrate-styrene-divinylbenzene polymer (SiO2- P), it is a kind of
Novel inorganic/organic support material, SiO is disclosed in United States Patent (USP) US68439212- styrene-divinylbenzene polymer,
SiO2- P is a kind of organic high polymer complex carrier of particle containing porous silicon dioxide carrier, and its preparation method is as follows：
(1) by the SiO of macropore2Washed, filtered with concentrated nitric acid, deionized water is washed till neutrality, repetition more than 10 times, drying.
(2) vacuum and have under argon gas protective condition, with 1,2,3- trichloropropane and m- dimethylbenzene for solvent, to macro-pore SiO2
Middle addition 48.7g m/p- formyl styrene, 8.9g m/p- divinylbenzenes, 72.2g dioctyls face phthalic acid ester,
54.0g benzoin methyl acid sodium, 0.56g α, α-even bis-isobutyronitrile and 0.57g1,1 '-even dicyclohexyl amine -1- nitriles, by room temperature progressively
90 DEG C are heated to, and is kept for 13 hours, afterwards, is progressively cooled to room temperature.
(3) washed respectively with acetone and methanol, filter above-mentioned product, repeated more than 10 times, dry.
In the present invention, the preparation method of the adsorbent is as follows：
Compound as shown in structure formula (I) is dissolved in dichloromethane, it is equal that carrier mixing is added in resulting solution
It is even, after revolving is dried, obtain adsorbent.
During revolving, most of dichloromethane is evaporated into closely dry state, under capillarity and physisorption, change
Adduct molecule enters in the space of carrier, and then the material of nearly dry state is dried in vacuo at least 24 hours at 45~55 DEG C,
Obtain adsorbent.
Preferably, it is dissolved in per compounds of the g as shown in structure formula (I) in 130~150mL dichloromethane.It is coated poly-
The macro-pore SiO of compound2Quality be 8~10 times of the compound quality shown in structure formula (I).
In order to ensure separating effect, it is preferable that chromatographic column column temperature is 25 ± 5 DEG C.Nitrate containing various metals ion
The flow velocity of solution in the chromatography column is 0.1mL/min~3mL/min.To ensure that metal ion and the adsorbent in chromatographic column are abundant
Contact-sorption.
In nitrate solution, the concentration of metal ion and the pH value of nitrate solution can influence separating effect, preferably
Ground, in nitrate solution, the concentration per metal ion species is 5.0 × 10-4~1.0 × 10-3M.The pH scopes of nitrate solution are
6~7.
In order to strengthen separating effect, using the aqueous solution of nitric acid of pH value same with nitrate solution to the chromatogram of adsorption saturation
Post is washed, and other metallic elements not being adsorbed are rinsed out, then using water by elements strontium in the form of nitrate
Elution parsing is got off, and completes the separation of elements strontium, while also complete the regeneration of chromatographic column.
The method of adsorbing separation strontium of the present invention, separated under the conditions of faintly acid (close to neutrality), mild condition, selection
Property is good, and separating rate is fast, simple to operate, easy to spread.
Brief description of the drawings
Fig. 1 is in the embodiment of the present invention 4~10, the adsorption isothermequation of elements strontium with pH value variation relation figure.
Embodiment
Embodiment 1
0.5g is dissolved in 70.0mL dichloromethane to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons (as shown in structure formula (I))
In, fully dissolving, 4.5gSiO is added in resulting solution2- P stirs, and makes SiO2- P with to the tert-butyl group-butyl sulphonyl cup
[4] aromatic hydrocarbons is well mixed, and makes dichloromethane volatilization most of to material to nearly dry state, in capillarity through depressurizing rotary evaporation
And organic molecule is set to enter SiO under physisorption2In-P apertures, then the material of nearly dry state is true at 45 DEG C again
Sky dries 24h, obtains adsorbent.
Embodiment 2
0.5g is dissolved in 75.0mL dichloromethane to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons (as shown in structure formula (I))
In, fully dissolving, 4.0gSiO is added in resulting solution2- P stirs, and makes SiO2- P with to the tert-butyl group-butyl sulphonyl cup
[4] aromatic hydrocarbons is well mixed, and makes dichloromethane volatilization most of to material to nearly dry state, in capillarity through depressurizing rotary evaporation
And organic molecule is set to enter SiO under physisorption2In-P apertures, then the material of nearly dry state is true at 50 DEG C again
Sky dries 24h, obtains adsorbent.
Embodiment 3
0.5g is dissolved in 80.0mL dichloromethane to the tert-butyl group-butyl sulphonyl cup [4] aromatic hydrocarbons (as shown in structure formula (I))
In, fully dissolving, 5.0gSiO is added in resulting solution2- P stirs, and makes SiO2- P with to the tert-butyl group-butyl sulphonyl cup
[4] aromatic hydrocarbons is well mixed, and makes dichloromethane volatilization most of to material to nearly dry state, in capillarity through depressurizing rotary evaporation
And organic molecule is set to enter SiO under physisorption2In-P apertures, then the material of nearly dry state is true at 55 DEG C again
Sky dries 24h, 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)6Salpeter solution is dissolved in, precious metals pd (5%w/w) nitrate solution is then added, matches somebody with somebody
The nitrate solution simultaneously containing various metals ion is made.
(2) add concentrated nitric acid and deionized water in nitrate solution, the pH for adjusting nitrate solution is respectively 1,2,3,
4th, 5,6,7, the concentration per metal ion species is 5.0 × 10-4M。
(3) in the chromatographic column for being ID10mm × h300mm by absorbent filling prepared by embodiment 1 to specification, setting flowing
The flow velocity of phase is 1mL/min, and the temperature of chromatographic column is 298K.
(4) nitrate solution that step (2) has been adjusted to pH has been filled by the chromatographic column equipped with adsorbent, elements strontium
The chromatographic column absorption of adsorbent.
(5) using aqueous solution of nitric acid (pH value of aqueous solution of nitric acid is identical with the pH value of corresponding nitrate solution, for example,
The pH value of nitrate solution is 1, then uses pH to be washed for 1 aqueous solution of nitric acid) chromatographic column for being adsorbed with elements strontium is entered
Row washing, flushing out adsorbent does not have other metallic elements adsorbed.
(6) after the adsorbent adsorption saturation in chromatographic column, elements Sr is eluted into parsing in the form of nitrate with water and got off,
Complete the separation of elements Sr.
For the absorption result of embodiment 4~10 as shown in figure 1, abscissa is pH value in Fig. 1, ordinate is adsorption isothermequation
Kd, unit 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 adsorption isothermequation of strontium is 140cm3/ g, in the range of pH6~7, elements Sr all has
There is preferable separating effect.
Embodiment 11
The absorbent filling that embodiment 2 is prepared is into chromatographic column, and remaining operating condition is the same as embodiment 9.
Embodiment 12
The absorbent filling that embodiment 3 is prepared is into chromatographic column, and remaining operating condition is the same as embodiment 9.
Claims (8)
- A kind of 1. method of adsorbing separation strontium, it is characterised in that comprise the following steps：Nitrate containing various metals ion is molten Liquid is adsorbed by adsorbent by being filled with the chromatographic column of adsorbent, elements strontium, the chromatographic column after absorption is eluted, obtains member Plain strontium, the adsorbent are made up of compound loaded as shown in structure formula (I) on carrier：Contain Sr (II) and other metal ions in the nitrate solution, other metal ions are Li (I), Na (I), K (I), At least one of Rb (I), Ba (II), Ce (III), Pd (II), Ca (II), Mg (II).
- 2. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that the carrier is the macropore of coated polymer SiO2。
- 3. the method for adsorbing separation strontium as claimed in claim 2, it is characterised in that the macro-pore SiO of coated polymer2Quality For 8~10 times of the compound quality shown in structure formula (I).
- 4. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that in nitrate solution, per metal ion species Concentration be 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 the pH scopes of nitrate solution are 6~7.
- 6. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that the nitrate containing various metals ion is molten The flow velocity of liquid 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 the preparation method of the adsorbent is as follows：Compound as shown in structure formula (I) is dissolved in dichloromethane, carrier is added in resulting solution and is well mixed, is passed through After revolving is dried, adsorbent is obtained.
- 8. the method for adsorbing separation strontium as claimed in claim 1, it is characterised in that chromatographic column column temperature is 25 ± 5 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610177218.3A CN105845188B (en) | 2016-03-24 | 2016-03-24 | A kind of method of adsorbing separation strontium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610177218.3A CN105845188B (en) | 2016-03-24 | 2016-03-24 | A kind of method of adsorbing separation strontium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105845188A CN105845188A (en) | 2016-08-10 |
| CN105845188B true CN105845188B (en) | 2017-11-17 |
Family
ID=56583672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610177218.3A Expired - Fee Related CN105845188B (en) | 2016-03-24 | 2016-03-24 | A kind of method of adsorbing separation strontium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105845188B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070158271A1 (en) * | 2006-01-12 | 2007-07-12 | Draxis Health Inc. | Systems and Methods for Radioisotope Generation |
| CN100566789C (en) * | 2007-07-06 | 2009-12-09 | 浙江大学 | A kind of method from high-level waste separating heating element Cs and Sr |
| JP2010002312A (en) * | 2008-06-20 | 2010-01-07 | Ihi Corp | Method and equipment for supplying high level radioactive waste liquid |
| CN101329312B (en) * | 2008-07-31 | 2011-02-16 | 浙江大学 | Chromatographic column |
| CN102614683B (en) * | 2012-04-05 | 2014-01-15 | 浙江大学 | Method for separating element palladium and sub-actinide elements from high-level waste |
-
2016
- 2016-03-24 CN CN201610177218.3A patent/CN105845188B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN105845188A (en) | 2016-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105688855B (en) | Method that is a kind of while separating strontium and caesium | |
| CN101690853B (en) | Method for separating element Pd from high-level radioactive waste | |
| CN105845188B (en) | A kind of method of adsorbing separation strontium | |
| CN106018634B (en) | A kind of nitrate anion type hydrotalcite adsorbent is to the absorption of six kinds of phenoxy carboxylic acid herbicides in water and De contamination method | |
| CN102614683B (en) | Method for separating element palladium and sub-actinide elements from high-level waste | |
| CN105854849B (en) | A kind of method using solid absorbent separation caesium | |
| Momen et al. | High-capacity extraction chromatographic materials based on polysulfone microcapsules for the separation and preconcentration of lanthanides from aqueous solution | |
| Dulanská et al. | The selective separation of Pu isotopes using molecular recognition technology product AnaLig® Pu02 gel and extraction chromatography TRU® resin | |
| CN106824101A (en) | A kind of method of the adsorption uranium from seawater | |
| Viglašová et al. | Column studies for the separation of 99m Tc using activated carbon | |
| Kong et al. | Preparative enrichment and separation of astragalosides from Radix Astragali extracts using macroporous resins | |
| JPH07299304A (en) | Method and device for continuous separation of boron isotope | |
| CN105617982A (en) | Inorganic adsorbent for removing 110mAg in radioactive water and preparing method thereof | |
| CN105195087A (en) | Extra-large-aperture silicon dioxide new material and preparation method thereof | |
| CN106588951B (en) | A kind of porous metal-organic framework compound and its preparation method and application based on zinc | |
| CN110205490B (en) | Method for separating uranium and iron | |
| CN104338510A (en) | Method for removing radioactive iodine from gas cooled reactor | |
| CN105921113A (en) | Adsorbent used for removing phthalic acid in water and preparation method thereof | |
| CN110205494B (en) | Method for adsorbing and separating rubidium and cesium | |
| Chen et al. | Separation of matrine and oxymatrine from extract through cation exchange resin coupled with macroporous absorption resin | |
| Li et al. | Simultaneous purification and separation of syringoside and oleuropein from Syringa oblata Lindl. extract using macroporous resin | |
| CN115445567B (en) | Method for efficiently adsorbing uranium | |
| CN103464095B (en) | Adsorbent having function of removing potassium ions in Chinese herba preparation and application of adsorbent | |
| CN100372781C (en) | Method for enriching and separating yellow substance from seawater | |
| CN107159125A (en) | A kind of method of adsorbing separation uranium and vanadium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20171117 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |