CN101323906A - Method for separating heating element Sr and metal element Ba from high-level waste - Google Patents
Method for separating heating element Sr and metal element Ba from high-level waste Download PDFInfo
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- CN101323906A CN101323906A CNA2008101201712A CN200810120171A CN101323906A CN 101323906 A CN101323906 A CN 101323906A CN A2008101201712 A CNA2008101201712 A CN A2008101201712A CN 200810120171 A CN200810120171 A CN 200810120171A CN 101323906 A CN101323906 A CN 101323906A
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Abstract
The invention discloses a method for separating a heating element of Sr and a metallic element of Ba from high-level wastes, comprising the following steps: (1) the concentration of nitric acid in a nitrate solution containing the heating element of Sr and the metallic element of Ba is adjusted to 0.5 to 4 mol/L; (2) after adjusting the concentration of nitric acid, the nitrate solution flows through a chromatographic column filled with a sorbent; the heating element of Sr is adsorbed by the filled sorbent while the metallic element of Ba flows out; (3) chromatographic column adsorbing the heating element of Sr is washed by deionized water and the heating element of Sr is washed out in a form of nitrate. The method of the invention has the advantages of good separation effect, strong preferential adsorption of the sorbent and being capable of separating the heating element of Sr and the metallic element of Ba from the high-level wastes thoroughly.
Description
Technical field
The present invention relates to separating of heating element Sr and metallic element Ba in aftertreatment field, the especially high-level waste of nuclear industry high-level waste.
Background technology
As the high-level waste (HLLW) that spent fuel (SF) aftertreatment produces, processing that it is safe and disposal are one of nuclear fuel cycle technology key link.According to national nuclear power development policies, rational and effective is utilized limited nuclear resource, is guaranteed security, nuclear non-proliferation, environmental compatibility, economy and be its basic principle by the effective treatment and disposal HLLW of spent fuel post-processing technology.
Contain heating element, the inferior actinide elements sliver products (FP) such as (MA) of long lifetime (millions of years) in the spent fuel, the present situation of aftertreatment is: except Separation and Recovery useful metal U and Pu, 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 extracting and separating flow processs that this purpose develops (having used the TRUEX flow process of CMPO and DIAMEX flow process that France has used ammoniac compounds etc. such as the U.S.), even but few to the Separation and Recovery of heating element Cs and Sr.
Cs the earliest and Sr Separation Research are from U.S. France and Japan.With regard to its isolation technique, mainly contain absorption method and solvent extration.Present Cs absorption method research mainly concentrates on inorganic adsorbent aspects such as silico-aluminate, titanate and the insoluble hexacyanoferrate.Yet, for reducing in the strongly acidic solution because of H
+Competitive adsorption and the serious Cs absorption that hinders, neutralization, denitration are essential as pre-treatment, cause processing costs and secondary refuse significantly to increase, and its slow adsorption rate, are difficult to reach effective separation of Cs.
The Cs of Separation and Recovery and Sr 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.In addition, Separation and Recovery Sr from HLLW can make vitrification body quantity significantly reduce; Spent fuel cooling period significantly shortens; Bear the viewpoint of reduction, utilization of resources from economy raising, the ecotope of HLLW treatment and disposal, meaning of crucial importance is also arranged, significant contribution is arranged constructing innovative nuclear fuel cycle system.
Document number is to disclose a kind of high-level waste treatment process among the U.S.'s patent of invention of US6843921B2 and the English Patent GB3290474 of the same clan, and high-level waste is made salpeter solution, also contains the HNO of 3 mol in the solution
3, this solution is isolated time actinide elements after chromatographic column is separated.Chinese patent application CN101143273 discloses a kind of method from high-level waste separating heating element Cs and Sr, in the nitrate solution of the high-level waste of isolating time actinide elements, add concentrated nitric acid and adjust concentration of nitric acid, this solution is isolated Cs and Sr successively through twice chromatographic column fractionation by adsorption.But in this method, heating element Sr and metallic element Ba are by chromatographic column selective adsorption simultaneously, and in the solution of chromatographic column after deionized water drip washing, Sr and Ba element are present in this nitrate solution simultaneously, and metallic element barium also must carry out further separating treatment.
Summary of the invention
The invention provides the separating heating element Sr from high-level waste of a kind of good separating effect, environmental protection and the method for metallic element Ba.
A kind of from high-level waste the method for separating heating element Sr and metallic element Ba, may further comprise the steps:
(1) concentration of nitric acid that will contain in the nitrate solution of heating element Sr and metallic element Ba transfers to 0.5～4 mol;
Can adjust with concentrated nitric acid when adjusting concentration of nitric acid.
The described nitrate solution that contains heating element Sr and metallic element Ba can from but be not limited only to the nitrate solution that contains heating element Sr and metallic element Ba that obtains among the comfortable Chinese patent application CN101143273.
(2) nitrate solution that will adjust behind the nitrate concentration flows through the chromatographic column that is filled with sorbent material, and heating element Sr is filled with the chromatographic column absorption of sorbent material, and metallic element Ba (with the form of nitrate) flows out chromatographic column.
(3) be adsorbed with the chromatographic column of Sr element with deionized water drip washing, the Sr element washes out with the form of nitrate.
In order to strengthen separating effect, between step (2) and (3), be the pre-drip washing chromatographic column of nitric acid of 1～2 mol with volumetric molar concentration, the Ba element is leached out fully.
Test shows that the chromatographic column that is filled with sorbent material only has the selection adsorptive power at heating element Sr.The nitrate solution that contains heating element Sr and metallic element Ba separates through the chromatographic column selective adsorption, and heating element Sr is separated with metallic element Ba.
In the chromatographic column adsorbents adsorb saturated after, can wash by water, heating element Sr can be got off to finish living again of chromatographic column with the form drip washing of nitrate.
Described sorbent material raw material consists of the macro-pore SiO that loads on the lining polymkeric substance
2On suc as formula the N shown in (I), N, N`, N`-four octyl groups-3-oxygen penta-1,5-diamide (TOOD), the lining polymkeric substance macro-pore SiO
2Quality be 1～20 times of quality of TOOD, preferred 5～15 times.
The macro-pore SiO of described lining polymkeric substance
2Preferred SiO
2-vinylbenzene-divinyl benzene polymers.
Described sorbent material prepares by the following method:
TOOD is dissolved in the methylene dichloride, adds the macro-pore SiO of lining polymkeric substance then
2Stir, obtain sorbent material after the vacuum-drying.
Before vacuum-drying, because initial stage methylene dichloride content is more, the load of vacuum pump when alleviating later stage vacuum-drying, can under normal pressure, stir about 45 ℃ earlier, make methylene dichloride volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45-50 ℃ of following vacuum-drying 24h.
The macro-pore SiO of described lining polymkeric substance
2(SiO
2-P) be a class novel inorganic/organic carrier, the macro-pore SiO of lining polymkeric substance is disclosed in the U.S. Pat 6843921
2(SiO
2-P), SiO
2-P is a kind of organic high polymers complex carrier that contains the porous silica carrier granule, and its preparation method is:
(1) with the SiO of macropore
2Be washed till neutrality with concentrated nitric acid washing, suction filtration, deionized water, repeat 10 surplus time, drying.
(2) vacuum and having under the argon shield condition is a solvent with glyceryl trichloride and m-dimethylbenzene, to macro-pore SiO
2The middle m/p-formyloxy vinylbenzene that adds 48.7g, 8.9g the m/p-Vinylstyrene, 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 acetone and methanol wash, the above-mentioned product of suction filtration respectively, repeat 10 surplus time, drying.
The inventive method good separating effect, sorbent material select adsorptivity strong, can more completely heating element Sr in the high-level waste and metallic element Ba be separated.
Description of drawings
Fig. 1 is the inventive method schematic flow sheet;
Fig. 2 is for after utilizing sorbent material of the present invention and being filled into chromatography column, utilizes liquid chromatography to carry out the spectrogram that separates of heating element Cs and Sr in the high-level waste (HLLW);
X-coordinate: the quality of expression effluent;
Ordinate zou (left side): concentration of metal ions in the expression effluent;
Ordinate zou (right side): expression pH value.
Embodiment
100 gram TOOD are dissolved in the 500mL methylene dichloride, mix; The macro-pore SiO that adds 200 gram lining polymkeric substance
2(SiO
2-P) stir and make methylene dichloride volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of following vacuum-drying 24h.
100 gram TOOD are dissolved in the 2000mL methylene dichloride, mix; The macro-pore SiO that adds 1000 gram lining polymkeric substance
2(SiO
2-P) stir and make methylene dichloride volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of following vacuum-drying 24h.
100 gram TOOD are dissolved in the 3000mL methylene dichloride, mix; The macro-pore SiO that adds 1500 gram lining polymkeric substance
2(SiO
2-P) stir and make methylene dichloride volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of following vacuum-drying 24h.
Heating element Sr and Summoning element B a's separates in the high-level waste
The sorbent material of embodiment 1 preparation is filled in the chromatographic column chromatographic column adopting Glass tubing, 1 centimetre of internal diameter, 1.2 centimetres of external diameters, 30 centimetres of height.
Flow rate of mobile phase generally is 1.0 ml/min.
(1) be that the disclosed flow process of Chinese invention patent application of CN101143273 is made nitrate solution with high-level waste and carried out separating of heating element Cs and Sr according to document number, the chromatographic column of wherein adsorbing Sr adds the nitrate solution that obtains containing Sr and Ba after hydrolysis is analysed, contain in the nitrate solution of Sr and Ba, the concentration of Sr and Ba is 0.5 mol, with concentrated nitric acid the concentration of nitric acid in this nitrate solution is adjusted into 4 mol;
(2) nitrate solution that will adjust the high-level waste behind the concentration of nitric acid is by being filled with the chromatographic column of sorbent material, and heating element Sr is filled with the chromatographic column absorption of sorbent material, and Ba flows out
(3) in the chromatographic column adsorbents adsorb saturated after, separating of Sr and Ba in the regeneration of getting off to finish chromatographic column and the high-level waste resolved heating element Sr by water with the form drip washing of nitrate.
Owing to be the nitrate solution system, described Sr and Ba all refer to ionic forms in the sepn process of the present invention.
Claims (4)
1. the method for separating heating element Sr and metallic element Ba from a high-level waste may further comprise the steps:
(1) concentration of nitric acid that will contain in the nitrate solution of heating element Sr and metallic element Ba transfers to 0.5～4 mol;
(2) nitrate solution that will adjust behind the concentration of nitric acid flows through the chromatographic column that is filled with sorbent material, the adsorbents adsorb that heating element Sr is loaded, and metallic element Ba flows out;
(3) be adsorbed with the chromatographic column of heating element Sr with deionized water drip washing, the Sr element washes out with the form of nitrate;
Described sorbent material is for loading on the macro-pore SiO of lining polymkeric substance
2N, N, N ', N '-four octyl groups-3-oxygen penta-1, the 5-diamide, the lining polymkeric substance macro-pore SiO
2Quality be N, N, N ', N '-four octyl groups-3-oxygen penta-1,1～20 times of the quality of 5-diamide; The macro-pore SiO of described lining polymkeric substance
2Be SiO
2-vinylbenzene-divinyl benzene polymers.
2. the method for claim 1 is characterized in that, is the pre-drip washing chromatographic column of nitric acid of 1～2 mol with volumetric molar concentration earlier in step (3), and the Ba element is leached out fully; Be adsorbed with the chromatographic column of Sr element again with deionized water drip washing, the form of Sr element with nitrate washed out.
3. the method for claim 1 is characterized in that, the macro-pore SiO of lining polymkeric substance in the described sorbent material
2Quality be N, N, N ', N '-four octyl groups-3-oxygen penta-1,5～15 times of the quality of 5-diamide.
4. as claim 1,2 or 3 described methods, it is characterized in that described sorbent material prepares by the following method:
With N, N, N ', N '-four octyl groups-3-oxygen penta-1, the 5-diamide is dissolved in the methylene dichloride, adds the macro-pore SiO of lining polymkeric substance then
2Stir, obtain sorbent material after the vacuum-drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101201712A CN101323906A (en) | 2008-07-31 | 2008-07-31 | Method for separating heating element Sr and metal element Ba from high-level waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101201712A CN101323906A (en) | 2008-07-31 | 2008-07-31 | Method for separating heating element Sr and metal element Ba from high-level waste |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690853B (en) * | 2009-10-19 | 2011-10-19 | 浙江大学 | Method for separating element Pd from high-level radioactive waste |
| CN102614683A (en) * | 2012-04-05 | 2012-08-01 | 浙江大学 | Method for separating element palladium and sub-actinide elements from high-level waste |
| CN105148732A (en) * | 2015-08-12 | 2015-12-16 | 中国原子能科学研究院 | Method for separating short-life nuclide <141>Ba |
| CN109628759A (en) * | 2019-01-14 | 2019-04-16 | 兰州大学 | A method of extraction strontium |
-
2008
- 2008-07-31 CN CNA2008101201712A patent/CN101323906A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690853B (en) * | 2009-10-19 | 2011-10-19 | 浙江大学 | Method for separating element Pd from high-level radioactive waste |
| CN102614683A (en) * | 2012-04-05 | 2012-08-01 | 浙江大学 | Method for separating element palladium and sub-actinide elements from high-level waste |
| CN105148732A (en) * | 2015-08-12 | 2015-12-16 | 中国原子能科学研究院 | Method for separating short-life nuclide <141>Ba |
| CN105148732B (en) * | 2015-08-12 | 2017-11-21 | 中国原子能科学研究院 | One kind separation short-lived nuclide141Ba method |
| CN109628759A (en) * | 2019-01-14 | 2019-04-16 | 兰州大学 | A method of extraction strontium |
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