CN102935355A - Adsorbent for separating heating element Cs and preparation method and application thereof - Google Patents
Adsorbent for separating heating element Cs and preparation method and application thereof Download PDFInfo
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- CN102935355A CN102935355A CN2012104373223A CN201210437322A CN102935355A CN 102935355 A CN102935355 A CN 102935355A CN 2012104373223 A CN2012104373223 A CN 2012104373223A CN 201210437322 A CN201210437322 A CN 201210437322A CN 102935355 A CN102935355 A CN 102935355A
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Abstract
The invention discloses an adsorbent for separating a heating element Cs. The adsorbent is made of macropore SiO2 loaded on coated polymer through calix dicrown ether, the mass of the SiO2 of the coated polymer is 0.5-40 times of that of the calix dicrown ether, the calix dicrown ether has a structural general formula (I), and the SiO2 of the coated polymer is SiO2-styrol-divinyl benzene polymer. The invention further provides a preparation method and application of the adsorbent. The preparation method is simple, heating element Cs separation effect is good, and the adsorbent for separating the heating element Cs and the preparation method are environment-friendly.
Description
Technical field
The present invention relates to the post processing field of nuclear industry high-level waste, relate in particular to adsorbent of a kind of separating heating element Cs and its preparation method and application.
Background technology
As the high-level waste (HLLW) that spentnuclear fuel (SF) post processing produces, its safe processing is one of key link of nuclear fuel cycle technology with disposing.
Contain heating element, the Fission products (FP) such as Minor actinides (MA) of long-life (millions of years) in the spentnuclear fuel, the present situation of post processing is: reclaim useful metal U and Pu except separating, a part of Np and similar all FP elements have all entered among the HLLW.For long-life MA, separation/transmuting technology has been proposed and for reaching some extract and separate flow processs that this purpose develops (such as the U.S. with the TRUEX flow process of using CMPO and France with the DIAMEX flow process of using ammoniac compounds etc.), even but the separation of heating element Cs is reclaimed theoretical few with technical research.
Cs among the HLLW is high heating element, and the half-life of its main nucleic Cs-137 is 30 years, because of the physical chemistry instability that its heat generation may cause, is considered to affect one of the most dangerous harmful element of HLLW glass solidification safe disposal; Another main nucleic Cs-135 has and reaches 2 * 10
6The half-life in year, earth ecological environment security is caused long-term burden, require it is carried out effective separation and safe disposal for this reason.In addition, the Cs that separate to reclaim both can be used as line source and also can be used as thermal source and be used effectively in medical treatment ﹠ health health care system.This is so that separate to reclaim Cs from HLLW, cause following favourable technology essential factor: glass solidified body quantity significantly reduces; SF cooling period significantly shortens; Process economy raising, the ecological environment disposed from HLLW and bear the viewpoint of reduction, utilization of resources, meaning of crucial importance is also arranged, to constructing innovative nuclear fuel cycle system significant contribution is arranged.
Cs Separation Research the earliest is from U.S. France and Japan.With regard to its isolation technics, mainly contain absorption method and solvent extraction.Present Cs absorption method research mainly concentrates on the inorganic adsorbent aspects such as alumino-silicate, titanate and the insoluble iron cyanide.Yet, be reducing the Cs absorption that hinders because the H+ competitive Adsorption is serious in the strongly acidic solution, neutralization, denitration are essential as pre-treatment, cause disposal cost and secondary refuse significantly to increase, and its slow rate of adsorption, are difficult to reach the effective separation of Cs.
The isolation technics of Cs among the HLLW, at present main research work concentrates on the liquid liquid solvent extraction method, representational flow process has CSSX (or CSEX) (the Caustic-Side Solvent Extraction) flow process of U.S. ORNL and INL, the extractant of use be BOBCalixC6 (Calix[4] BisC6-bis-(tert-octylbenzo-crown-6).For eliminating extractant at hydrocarbon diluent
The third phase that occurs among the L, (1-(2 for alcohol acids molecular modification agent Cs-7SB, 2,3,3-tetrafluoropropoxy)-3-(4-sec-butylphenoxy)-2-propanol, Chinese name 1-(2,2,3, the 3-tetrafluoro is for propoxyl group)-3-(the 4-second month in a season-butyl phenoxy)-2-propyl alcohol) or Cs-3 (1-(1,1,2,2-tetrafluoroethoxyl)-3-[4-(tert-octyl) phenoxyl]-2-propanol, Chinese name 1-(1,1,2, the 2-tetrafluoro is for propoxyl group)-3-[4-(uncle-octyl group) phenoxy group]-the 2-propyl alcohol) and TOA (tri-n-octylamine, Chinese name three n-octylamine) be added to
In the L extraction system.
The Calix-bis-crown Calix[4 of Commissariat A L'Energie Atomique (CEA) exploitation] arene-R14 (1,3-[(2,4-diethyl-heptylethoxy) oxy]-2,4-crown-6-Calix[4] arene) see structural formula (III), the Selective Separation performance to Cs in the CCCEX extraction procedure is excellent.
Calix[4 is selected in control] the suitable vestibule size of arene-R14, can be at HNO
3Selective Separation Cs in the solution.Its main deficiency is that the solubility of these large ring organic compounds in the hydrocarbon diluent commonly used such as n-dodecane and kerosene is very low, must use some very special strong toxicity diluents such as nitrobenzene, tetrapropyl hydrogen, nitrobenzophenone Octyl Ether, even so, its saturated concentration also only has 0.001-0.1M; For the third phase that suppresses to occur, also must add a large amount of organic phase adjusting agents, such as Methyl Octyl-2-amide dimethyl butyrate, Cs-7SB, Cs-3 and Cs-4 (2,3-(uncle 4--Octylphenoxy)-propyl alcohol) etc. are so that separation process must be used large capacity multistage extraction equipment, produce a large amount of liquid wastes and reluctant second-order activity debirs in the post processing flow process, the solvent that occurs thus chemistry instability causes the worry to the post processing circulation safe.
Summary of the invention
The invention provides adsorbent of a kind of separating heating element Cs and its preparation method and application, the preparation method is simple, and is effective for separating of heating element Cs, and environmentally friendly.
A kind of adsorbent of separating heating element Cs is loaded on the macro-pore SiO of coating polymer by Calix-bis-crown
2And make;
The macro-pore SiO of coating polymer
2Quality be 0.5～40 times of quality of Calix-bis-crown;
Described Calix-bis-crown has general structure (I)
In the general structure (I), R is C
1～C
20Alkylidene, alkylene oxide group, the halo alkylidene of optional replacement; In the alkylidene that replaces, alkylene oxide group, halo alkylidene, has at least following substituting group a: C
1～C
8Haloalkyl, C
1～C
18Alkoxyl;
N is 1～10 integer;
The macro-pore SiO of described coating polymer
2Be SiO
2-styrene-divinylbenzene polymer.
As preferably, the macro-pore SiO of coating polymer
2Quality be 2～10 times of quality of Calix-bis-crown.
As preferably, in the described Calix-bis-crown general structure (I), R is C
1～C
4Alkylidene or alkylene oxide group.Further preferred R is ethylidene.
As preferably, n is 4～6 integer.As preferably, described Calix-bis-crown is 1,3-calix[4] arene-25,26,27,28-bis-(crown-6) (1,3-Calix[4] BisC6), have structural formula (II)
The macro-pore SiO of described coating polymer
2Be SiO
2-styrene-divinylbenzene polymer (SiO
2-P), be a class novel inorganic/organic carrier, the macro-pore SiO of coating polymer is disclosed in the US Patent No. 6843921
2, SiO
2-P is a kind of organic high polymer complex carrier that contains the porous silica carrier granular, and its preparation method is:
(1) with the SiO of macropore
2Be washed till neutrality with red fuming nitric acid (RFNA) washing, suction filtration, deionized water, repeat drying more than 10 times.
(2) vacuum and having under the argon shield condition is solvent with 1,2,3-trichloropropane and m-dimethylbenzene, to macro-pore SiO
2The m/p-formyl styrene of middle adding 48.7g, 8.9g the m/p-divinylbenzene, 72.2g dioctyl faces phthalic acid ester, 54.0g benzoin methyl acid sodium, 0.56g α, α-even bis-isobutyronitrile and 0.57g 1,1 '-even dicyclohexyl amine-1-nitrile, progressively be heated to 90 ℃ by room temperature, and kept 13 hours, afterwards, progressively be cooled to room temperature.
(3) use respectively acetone and methanol wash, the above-mentioned product of suction filtration, repeat drying more than 10 times.
The present invention also provides a kind of preparation method of adsorbent of described separating heating element Cs, and Calix-bis-crown is dissolved in the carrene, mixes, and adds the macro-pore SiO of coating polymer again
2Stir vacuum drying.
More owing to initial stage carrene content when dry, the load of vavuum pump when alleviating the later stage vacuum drying, can be first under normal pressure, stir about 45 ℃, make the carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The present invention also provides the method for described adsorbent separating heating element Cs as follows:
Comprise the steps:
(1) adds red fuming nitric acid (RFNA) in the nitrate solution of high-level waste concentration of nitric acid is adjusted into 0.4～6 mol/L;
(2) nitrate solution that will adjust the high-level waste behind the concentration of nitric acid contacts with described adsorbent, makes heating element Cs be adsorbed agent absorption.
As preferably, add red fuming nitric acid (RFNA) in the nitrate solution of high-level waste in the step (1) concentration of nitric acid is adjusted into 2～3 mol/L.
The concentration of described nitric acid has certain impact for the result of separating heating element Cs, and is further preferred, adds red fuming nitric acid (RFNA) in the nitrate solution of high-level waste in the step (1) concentration of nitric acid is adjusted into 2 mol/L.
As preferably, the metal ion total concentration is 4.0 * 10 in the nitrate solution described in the step (1)
-3～6.0 * 10
-3Mol/L.
The concentration of metal ion is also influential for utilizing chromatogram to carry out the separating resulting of heating element Cs, and the excessive concentration of metal ion might surpass the separating power of adsorbent, can not realize the fully separation of Cs; The concentration of metal ion is excessively low, then reduces separative efficiency.
Further preferred, the metal ion total concentration is 5.0 * 10 in the nitrate solution described in the step (1)
-3～6.0 * 10
-3Mol/L.
The inventive method at room temperature operates and gets final product.
Based on the excellent extraction ability of Calix-bis-crown to Cs, the present invention utilizes Calix-bis-crown to load on the macro-pore SiO of coating polymer
2(SiO
2-P) synthesized the silica-based Supramolecular Recognition adsorbent 1 of novel macropore, 3-Calix[4] BisC6/SiO
2-P.
The silica-based Supramolecular Recognition material Calix-bis-crown of the large ring of adsorbent employing of the present invention is good to the recognition capability of Cs, adsorption capacity is high, and the rate of recovery is high, can realize that high selectivity is separated recovery Cs from HLLW.
If separately Calix-bis-crown is loaded on SiO
2On-the P, because Calix-bis-crown is water-soluble bad, be difficult to load on SiO
2On-the P, must be aided with other auxiliary agents.
Adsorbent of the present invention and need not use the diluent with property to dilute or dissolve in adsorption process does not need to add other organic compounds, has both overcome the deficiency of solvent extraction, has kept again its loading capacity than high; Calix-bis-crown loads on the SiO of granularity 40-60 μ m
2-P carrier is compared with existing adsorbent, and ion diffusion, Adsorption and desorption speed all are significantly increased,, be that having of can expecting filled a part security, economy, high efficiency separation and recovery technology flow process.This is significant to realizing processing safely and effectively disposal HLLW.
Description of drawings
Fig. 1 is that the adsorbent that utilizes the present invention to prepare separates the distribution coefficient of heating element Cs in the high-level waste with the graph of a relation of variation time of contact;
Fig. 2 is that the adsorbent that utilizes the present invention to prepare separates the distribution coefficient of heating element Cs in the high-level waste with the graph of a relation of nitrate concentration variation.
The specific embodiment
The preparation of embodiment 1 adsorbent
100 grams are had 1 of structural formula (II), a 3-Calix[4] BisC6 is dissolved in the 1000mL carrene, mixes; The macro-pore SiO that adds 300 gram coating polymer
2(SiO
2-P) stir and make carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The preparation of embodiment 2 adsorbents
100 grams are had 1 of structural formula (II), a 3-Calix[4] BisC6 is dissolved in the 1500mL carrene, mixes; The macro-pore SiO that adds 600 gram coating polymer
2(SiO
2-P) stir and make carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The preparation of embodiment 3 adsorbents
100 grams are had 1 of structural formula (II), a 3-Calix[4] BisC6 is dissolved in the 3000mL carrene, mixes; The macro-pore SiO that adds 1500 gram coating polymer
2(SiO
2-P) stir and make carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The preparation of embodiment 4 adsorbents
100 grams are had 1 of structural formula (II), a 3-Calix[4] BisC6 is dissolved in the 4500mL carrene, mixes; The macro-pore SiO that adds 2000 gram coating polymer
2(SiO
2-P) stir and make carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The separation of heating element Cs in embodiment 5 high-level wastes (HLLW)
High-level waste and nitric acid are mixed and made into nitrate solution, HNO in the nitrate solution
3Concentration is 2.0 mol/L, and the metal ion total concentration is 5.0 * 10 in the nitrate solution
-3Mol/L.
With the mixing that in container, contacts of the nitrate solution of adjusting the high-level waste behind the concentration of nitric acid and the adsorbent of embodiment 1 preparation, for the raising adsorption effect can be aided with concussion, Cs is adsorbed on the adsorbent.
Adsorbent of the present invention has good selective to Cs, so can separate with Cs absorption and with other metallic elements, have good separating effect.The separating effect spectrogram is seen Fig. 1, and can realize the fully separation of Cs when being 60min time of contact.
The separation of heating element Cs in embodiment 6～12 high-level wastes (HLLW)
High-level waste and nitric acid are mixed and made into nitrate solution, HNO in the nitrate solution
3Concentration be followed successively by 0.5 mol/L, 1.0 mol/L, 2.0 mol/L, 3.0 mol/L, 4.0 mol/L, 5.0 mol/L, 6.0 mol/L, the metal ion total concentration is 5.0 * 10 in the nitrate solution
-3Mol/L;
With mixings that in container, contact of the above nitrate solution of respectively adjusting the high-level waste behind the concentration of nitric acid and the adsorbent of embodiment 1 preparation, for the raising adsorption effect can be aided with concussion, Cs is adsorbed on the adsorbent.Time of contact, as shown in Figure 2, different nitrate concentrations was larger on the separating effect impact when being 180min, and when nitrate concentration was 2.0 mol/L, the effect of separating heating element Cs was best.
Claims (8)
1. the adsorbent of a separating heating element Cs is characterized in that, is loaded on the macro-pore SiO of coating polymer by Calix-bis-crown
2And make;
The macro-pore SiO of coating polymer
2Quality be 0.5～40 times of quality of Calix-bis-crown;
Described Calix-bis-crown has general structure (I)
In the general structure (I), R is C
1～C
20Alkylidene, alkylene oxide group, the halo alkylidene of optional replacement; In the alkylidene that replaces, alkylene oxide group, halo alkylidene, has at least following substituting group a: C
1～C
8Haloalkyl, C
1～C
18Alkoxyl;
N is 1～10 integer;
The macro-pore SiO of described coating polymer
2Be SiO
2-styrene-divinylbenzene polymer.
2. the adsorbent of separating heating element Cs as claimed in claim 1 is characterized in that, the macro-pore SiO of coating polymer
2Quality be 2～10 times of quality of Calix-bis-crown.
3. the adsorbent of separating heating element Cs as claimed in claim 1 is characterized in that, in the described Calix-bis-crown general structure (I), R is C
1～C
4Alkylidene or alkylene oxide group.
4. the adsorbent of separating heating element Cs as claimed in claim 1 is characterized in that, n is 4～6 integer.
5. such as the adsorbent of the arbitrary described separating heating element Cs of claim 1～4, it is characterized in that, described Calix-bis-crown has structural formula (II)
6. such as the preparation method of the adsorbent of the arbitrary described separating heating element Cs of claim 1～5, it is characterized in that, Calix-bis-crown is dissolved in the carrene, mix, add again the macro-pore SiO of coating polymer
2Stir vacuum drying.
7. the method for a utilization such as the arbitrary described adsorbent of claim 1～5 separating heating element Cs from high-level waste is characterized in that, comprises the steps:
(1) adds red fuming nitric acid (RFNA) in the nitrate solution of high-level waste concentration of nitric acid is adjusted into 0.4～6 mol/L;
(2) nitrate solution that will adjust the high-level waste behind the concentration of nitric acid contacts with described adsorbent, makes heating element Cs be adsorbed agent absorption.
8. method as claimed in claim 7 is characterized in that, the metal ion total concentration is 5.0 * 10 in the nitrate solution described in the step (1)
-3～6.0 * 10
-3Mol/L.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103157446A (en) * | 2013-03-11 | 2013-06-19 | 浙江大学 | Adsorbent for separating palladium from alkali metals and alkaline-earth metals and its preparation method and use |
| CN105130950A (en) * | 2015-09-17 | 2015-12-09 | 清华大学 | Bisamide-substituted novel calixcrown ether compound as well as synthesis method and application thereof |
| CN105363425A (en) * | 2015-12-03 | 2016-03-02 | 中国科学院青海盐湖研究所 | Magnetic cesium ion adsorbent and preparation method therefor |
| CN105854849A (en) * | 2016-03-24 | 2016-08-17 | 浙江大学 | Method for separating caesium by using solid adsorbent |
| CN106186154A (en) * | 2016-07-25 | 2016-12-07 | 浙江大学 | A kind of method concurrently separating rubidium and caesium from salt lake saline |
| CN108273473A (en) * | 2018-01-19 | 2018-07-13 | 华东交通大学 | A method of detaching caesium using carbon-based calixarenes crown ether hybrid material |
| CN108311108A (en) * | 2018-01-19 | 2018-07-24 | 东华理工大学 | A kind of carbon-based calixarenes crown ether hybrid material and its preparation method and application |
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| CN101093735A (en) * | 2007-04-11 | 2007-12-26 | 浙江大学 | Adsorbent in use for separating heating element Cs, preparation and application |
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2012
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Patent Citations (1)
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|---|---|---|---|---|
| CN101093735A (en) * | 2007-04-11 | 2007-12-26 | 浙江大学 | Adsorbent in use for separating heating element Cs, preparation and application |
Non-Patent Citations (1)
| Title |
|---|
| JONG SEUNG KIM ET AL.: "Calix[4]arenes Bridged with Two Different Crown Ether Loops:Influence of Crown Size on Metal Ion Recognition", 《JOURNAL OF INCLUSION PHENOMENA AND MACROCYCLIC CHEMISTRY》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103157446A (en) * | 2013-03-11 | 2013-06-19 | 浙江大学 | Adsorbent for separating palladium from alkali metals and alkaline-earth metals and its preparation method and use |
| CN103157446B (en) * | 2013-03-11 | 2014-12-03 | 浙江大学 | Adsorbent for separating palladium from alkali metals and alkaline-earth metals and its preparation method and use |
| CN105130950A (en) * | 2015-09-17 | 2015-12-09 | 清华大学 | Bisamide-substituted novel calixcrown ether compound as well as synthesis method and application thereof |
| CN105363425A (en) * | 2015-12-03 | 2016-03-02 | 中国科学院青海盐湖研究所 | Magnetic cesium ion adsorbent and preparation method therefor |
| CN105363425B (en) * | 2015-12-03 | 2017-12-15 | 中国科学院青海盐湖研究所 | Magnetic cesium ion adsorbent and preparation method thereof |
| CN105854849A (en) * | 2016-03-24 | 2016-08-17 | 浙江大学 | Method for separating caesium by using solid adsorbent |
| CN105854849B (en) * | 2016-03-24 | 2018-04-27 | 浙江大学 | A kind of method using solid absorbent separation caesium |
| CN106186154A (en) * | 2016-07-25 | 2016-12-07 | 浙江大学 | A kind of method concurrently separating rubidium and caesium from salt lake saline |
| CN108273473A (en) * | 2018-01-19 | 2018-07-13 | 华东交通大学 | A method of detaching caesium using carbon-based calixarenes crown ether hybrid material |
| CN108311108A (en) * | 2018-01-19 | 2018-07-24 | 东华理工大学 | A kind of carbon-based calixarenes crown ether hybrid material and its preparation method and application |
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Application publication date: 20130220 |