CN103451428B - Ruthenium purifying technology in plutonium purification cycle of Purex process - Google Patents
Ruthenium purifying technology in plutonium purification cycle of Purex process Download PDFInfo
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- 238000000746 purification Methods 0.000 title claims abstract description 39
- 229910052778 Plutonium Inorganic materials 0.000 title claims abstract description 38
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 title claims abstract description 38
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000003350 kerosene Substances 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 239000003599 detergent Substances 0.000 abstract description 8
- 238000012958 reprocessing Methods 0.000 abstract description 5
- 239000003758 nuclear fuel Substances 0.000 abstract description 2
- 229910052770 Uranium Inorganic materials 0.000 description 14
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 14
- 238000005202 decontamination Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 239000012074 organic phase Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003588 decontaminative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012527 feed solution Substances 0.000 description 2
- 230000004992 fission Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明属于核燃料后处理技术领域，公开了Purex流程钚纯化循环中钌的净化工艺，该工艺是在2A槽中加入萃取剂2AX和洗涤剂2AS将2AF料液中的少量钌元素除去，所用的萃取剂2AX的组成为30%TBP/煤油，洗涤剂2AS为c(HNO3)=0.5~1.5mol/L的水溶液，流比2AF:2AX=3.5~6，萃取计数为8~10级，洗涤级数大于6级。该工艺能进一步净化钌，提高Purex流程最终钚产品的质量。
The invention belongs to the technical field of nuclear fuel reprocessing, and discloses a purification process for ruthenium in the plutonium purification cycle of the Purex process. The process is to add an extractant 2AX and a detergent 2AS in the 2A tank to remove a small amount of ruthenium in the 2AF feed liquid. The composition of the extractant 2AX is 30%TBP/kerosene, the detergent 2AS is c(HNO 3 )=0.5~1.5mol/L aqueous solution, the flow ratio is 2AF:2AX=3.5~6, the extraction count is 8~10, and the washing The number of stages is greater than 6. The process further purifies the ruthenium and improves the quality of the final plutonium product of the Purex process.
Description
技术领域 technical field
本发明属于核燃料后处理技术领域，具体涉及Purex流程钚纯化循环中钌的净化工艺。 The invention belongs to the technical field of nuclear fuel reprocessing, and in particular relates to a purification process for ruthenium in the plutonium purification cycle of the Purex process.
背景技术 Background technique
Purex流程包括共去污分离循环、钚纯化循环和铀净化循环。共去污分离循环的主要目的之一是要实现铀、钚与裂变元素间最大限度的分离，铀净化循环和钚纯化循环是为了得到高纯度的铀、钚产品。钌为后处理中要去除的裂变产物之一，为强γ放射性核素，其在铀、钚产品中的量直接决定着后处理操作的人员防护标准，因此钌的含量是铀、钚产品的一个重要检测项目。 The Purex process includes a co-decontamination separation cycle, a plutonium purification cycle and a uranium purification cycle. One of the main purposes of the decontamination and separation cycle is to achieve the maximum separation between uranium, plutonium and fissile elements, and the uranium purification cycle and plutonium purification cycle are to obtain high-purity uranium and plutonium products. Ruthenium is one of the fission products to be removed in reprocessing. It is a strong γ-radioactive nuclide. Its amount in uranium and plutonium products directly determines the personnel protection standards for reprocessing operations. An important test item.
在共去污分离循环中通过加入萃取剂，使铀、钚进入有机相，钌等裂变元素进入萃余液，但是仍然有少量钌以其萃取形态进入钚纯化循环。钚纯化循环的主要任务是对共去污分离循环得到的含裂片和铀的钚粗产品液进行纯化和浓缩，以获得合格的钚产品液，并满足后续工艺的要求，其工艺简图如图1。钌在钚纯化循环中与共去污分离循环中的净化有两点重要的不同：（1）在动力堆乏燃料后处理共去污分离循环中钌浓度为0.22g/gPu，远高于钚纯化循环中的钌浓度22.5μg/gPu，浓度相差约10000倍；（2）共去污循环中有机相铀、钚饱和度较高为75%，利于钌的净化，而钚纯化循环中有机相铀、钚饱和度较低为15%左右，不利于钌的净化。因此，对钚纯化循环中微量钌行为和走向的研究具有重要意义。国内外公开文献中未见有关钚纯化循环中钌的净化的报道。 In the co-decontamination separation cycle, by adding extractant, uranium and plutonium enter the organic phase, and fissile elements such as ruthenium enter the raffinate, but a small amount of ruthenium enters the plutonium purification cycle in its extracted form. The main task of the plutonium purification cycle is to purify and concentrate the crude plutonium product liquid containing fragments and uranium obtained from the co-decontamination and separation cycle, so as to obtain qualified plutonium product liquid and meet the requirements of subsequent processes. The process diagram is shown in the figure 1. There are two important differences between the purification of ruthenium in the plutonium purification cycle and the co-decontamination and separation cycle: (1) The concentration of ruthenium in the power reactor spent fuel reprocessing co-decontamination and separation cycle is 0.22g/gPu, which is much higher than that of plutonium purification The concentration of ruthenium in the cycle is 22.5 μg/gPu, and the concentration difference is about 10,000 times; (2) The organic phase uranium and plutonium saturation in the common decontamination cycle is 75%, which is conducive to the purification of ruthenium, while the organic phase uranium in the plutonium purification cycle , The plutonium saturation is as low as about 15%, which is not conducive to the purification of ruthenium. Therefore, it is of great significance to study the behavior and trend of trace ruthenium in plutonium purification cycle. There is no report on the purification of ruthenium in the plutonium purification cycle in the open literature at home and abroad.
发明内容 Contents of the invention
（一） 发明目的(1) Purpose of the invention
根据现有技术所存在的问题，本发明提供了一种能在钚纯化循环中净化钌的工艺，该工艺能进一步净化钌，在钚收率大于99.9%的前提下，钌的净化系数大于1000，提高了Purex流程最终钚产品的质量。 According to the existing problems in the prior art, the present invention provides a process capable of purifying ruthenium in the plutonium purification cycle, which can further purify ruthenium. Under the premise that the plutonium yield is greater than 99.9%, the purification coefficient of ruthenium is greater than 1000 , improving the quality of the final plutonium product of the Purex process.
（二） 技术方案(2) Technical solutions
为了解决上述问题，本发明是通过以下技术方案实现的：在2A槽中加入萃取剂2AX和洗涤剂2AS将2AF料液中的少量钌元素除去，关键在于，所用的萃取剂2AX的组成为30%TBP/煤油，洗涤剂2AS为c(HNO3)=0.5~1.5mol/L的水溶液，流比2AF:2AX=3.5~6，萃取级数为8~10级，洗涤级数大于6级。 In order to solve the above problems, the present invention is achieved through the following technical solutions: add extractant 2AX and detergent 2AS in the 2A tank to remove a small amount of ruthenium in the 2AF feed liquid, the key is that the used extractant 2AX has a composition of 30 %TBP/kerosene, the detergent 2AS is an aqueous solution of c(HNO 3 )=0.5~1.5mol/L, the flow ratio 2AF:2AX=3.5~6, the extraction stage is 8~10, and the washing stage is greater than 6 stages.
（三） 有益效果(3) Beneficial effects
本发明提供的Purex流程钚纯化循环中钌的净化工艺，首次提出在钚纯化循环中进行微量钌的净化，其有益效果为：（1）在钚纯化循环中净化微量钌能进一步降低钌含量，提高钚产品纯度，降低操作人员的防护水平。（2）钚收率高、钌净化系数大。提出流比2AF:2AX=3.5~6，萃取级数为8~10级，洗涤级数大于6级的工艺条件，在钚收率大于99.9%的前提下，钌的净化系数大于1000。 The purification process of ruthenium in the plutonium purification cycle of the Purex process provided by the present invention proposes for the first time the purification of trace ruthenium in the plutonium purification cycle, and its beneficial effects are: (1) purifying trace ruthenium in the plutonium purification cycle can further reduce the ruthenium content, Improve the purity of plutonium products and reduce the protection level of operators. (2) The yield of plutonium is high and the purification coefficient of ruthenium is large. The process conditions of flow ratio 2AF:2AX=3.5~6, extraction stages of 8~10, and washing stages of more than 6 are proposed. On the premise that the plutonium yield is greater than 99.9%, the purification factor of ruthenium is greater than 1000.
附图说明 Description of drawings
图1. 钚纯化循环工艺简图 Figure 1. Schematic diagram of plutonium purification cycle process
实施方式Implementation
下面结合说明书附图和具体实施方式对本发明作进一步阐述。 The present invention will be further elaborated below in conjunction with the accompanying drawings and specific embodiments.
实施例1Example 1
在温度为20℃条件下，在2A槽中加入萃取剂2AX和洗涤剂2AS将2AF料液中的少量铀及钌等裂变元素除去，关键在于，所用的萃取剂2AX为30%TBP/煤油，洗涤剂2AS为c(HNO3)=0.5mol/L的水溶液，流比2AF:2AX:2AS=3.5:1:0.45，所用2AF料液的组成为：c(Pu4+)=6.8g/L，c(UO2 2+)=0.74g/L，c(HNO3)=3.5mol/L，c(Ru)=0.3108mg/L的水溶液，选用的萃取级数为8级，洗涤级数为6级，有机相与水相相比为2:1。 At a temperature of 20°C, add extractant 2AX and detergent 2AS to the 2A tank to remove a small amount of fission elements such as uranium and ruthenium in the 2AF feed liquid. The key point is that the extractant 2AX used is 30%TBP/kerosene, The detergent 2AS is an aqueous solution of c(HNO 3 )=0.5mol/L, the flow ratio is 2AF:2AX:2AS=3.5:1:0.45, and the composition of the 2AF feed liquid used is: c(Pu 4+ )=6.8g/L , c(UO 2 2+ )=0.74g/L, c(HNO 3 )=3.5mol/L, c(Ru)=0.3108mg/L aqueous solution, the selected extraction stage is 8, and the washing stage is Level 6, the ratio of organic phase to aqueous phase is 2:1.
实验时，先以不含铀和钚料液进行充槽两个小时，然后加入含铀和钚的料液，运行5.0h后，每个2小时取一瞬时样，运行16h后，停槽分析。 During the experiment, the tank was first filled with uranium and plutonium-free feed solution for two hours, and then the feed solution containing uranium and plutonium was added. After running for 5.0 hours, an instant sample was taken every 2 hours. After running for 16 hours, the tank was stopped for analysis .
实验结果：铀的收率大于99.9%，铀的物料衡算为97%，酸的物料衡算为98%，钚的收率为99.95%，Ru的净化系数DFRu=2653，表明实验过程运行良好，实验结果可靠。 Experimental results: the yield of uranium is greater than 99.9%, the mass balance of uranium is 97%, the mass balance of acid is 98%, the yield of plutonium is 99.95%, and the purification factor of Ru DF Ru =2653, indicating that the experimental process runs Good, the experimental results are reliable.
实施例2Example 2
与实施例1所用的步骤相同，不同的是洗涤剂2AS为c(HNO3)=1mol/L的水溶液，选用的流比2AF:2AX:2AS=5:1:0.45，2AF的组成为c(Pu4+)=2.75g/L，c(UO2 2+)=1.2g/L，c(HNO3)=3.5mol/L，c(Ru)=0.054mg/L的水溶液，萃取级数为9级，洗涤级数为8级，温度为30℃，所得实验结果为：钚收率为99.97%，Ru的净化系数DFRu=3590。 The steps used in Example 1 are the same, except that the detergent 2AS is an aqueous solution of c(HNO 3 )=1 mol/L, the selected flow ratio is 2AF:2AX:2AS=5:1:0.45, and the composition of 2AF is c( Pu 4+ )=2.75g/L, c(UO 2 2+ )=1.2g/L, c(HNO 3 )=3.5mol/L, c(Ru)=0.054mg/L aqueous solution, the extraction stage is 9 stages, 8 stages of washing, and a temperature of 30°C. The experimental results obtained are: the plutonium yield is 99.97%, and the Ru purification factor DF Ru =3590.
实施例3Example 3
与实施例1所用的步骤相同，不同的是洗涤剂2AS为c(HNO3)=1.5mol/L的水溶液，选用的流比2AF:2AX:2AS=6:1:0.45，2AF的组成为c(Pu4+)=2.75g/L，c(UO2 2+)=1.2g/L，c(HNO3)=3.5mol/L，c(Ru)=0.054mg/L的水溶液，萃取级数为10级，洗涤级数为10级，温度为30℃，所得实验结果为：钚收率为99.98%，Ru的净化系数DFRu=3120。 The steps used in Example 1 are the same, the difference is that the detergent 2AS is an aqueous solution of c(HNO 3 )=1.5mol/L, the selected flow ratio is 2AF:2AX:2AS=6:1:0.45, and the composition of 2AF is c (Pu 4+ )=2.75g/L, c(UO 2 2+ )=1.2g/L, c(HNO 3 )=3.5mol/L, c(Ru)=0.054mg/L aqueous solution, extraction stages It is grade 10, the number of washing stages is 10, and the temperature is 30°C. The experimental results obtained are: the yield of plutonium is 99.98%, and the purification factor of Ru is DF Ru =3120.
Claims (3)
- The purification process of ruthenium in 1.Purex flow process plutonium purification cycle, this technique is as extraction agent 2AX with 30%TBP/ kerosene, it is characterized in that, this technique in 2A groove, adds extraction agent 2AX and washing composition 2AS by the ruthenium removing in 2AF feed liquid, and washing composition 2AS used is c (HNO 3the aqueous solution of)=1mol/L.
- 2. the purification process of ruthenium in Purex flow plutonium purification cycle according to claim 1, is characterized in that, described 2AF and 2AX stream is than 2AF:2AX=3.5 ~ 6, and extraction progression is 8 ~ 10 grades, and washing progression is greater than 6 grades.
- 3. the purification process of ruthenium in Purex flow plutonium purification cycle according to claim 1, it is characterized in that, the temperature condition of this technique is 20 DEG C ~ 30 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0143749A1 (en) * | 1983-11-29 | 1985-06-05 | GebràDer Sulzer Aktiengesellschaft | Liquid-liquid extraction process of gallium from aqueous basic solutions using an organic extractant |
| US4656011A (en) * | 1984-02-13 | 1987-04-07 | British Nuclear Fuel Plc | Process of treating nuclear fuel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0143749A1 (en) * | 1983-11-29 | 1985-06-05 | GebràDer Sulzer Aktiengesellschaft | Liquid-liquid extraction process of gallium from aqueous basic solutions using an organic extractant |
| US4656011A (en) * | 1984-02-13 | 1987-04-07 | British Nuclear Fuel Plc | Process of treating nuclear fuel |
Non-Patent Citations (1)
| Title |
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| "单甲基肼改善铀纯化循环中钌的净化";张宇等;《原子能科学技术》;20091231;第43卷(第12期);正文第1187页1.2、图1及表2 * |
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