CN106409372A - Dissolving method for uranium tetrafluoride - Google Patents
Dissolving method for uranium tetrafluoride Download PDFInfo
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- CN106409372A CN106409372A CN201510486616.9A CN201510486616A CN106409372A CN 106409372 A CN106409372 A CN 106409372A CN 201510486616 A CN201510486616 A CN 201510486616A CN 106409372 A CN106409372 A CN 106409372A
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- MZFRHHGRNOIMLW-UHFFFAOYSA-J uranium(4+);tetrafluoride Chemical compound F[U](F)(F)F MZFRHHGRNOIMLW-UHFFFAOYSA-J 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 59
- 238000004090 dissolution Methods 0.000 claims abstract description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- 238000011978 dissolution method Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- HNVCXDAVEHOIBP-UHFFFAOYSA-N 2-[(5-bromopyridin-2-yl)diazenyl]-5-(diethylamino)phenol Chemical compound OC1=CC(N(CC)CC)=CC=C1N=NC1=CC=C(Br)C=N1 HNVCXDAVEHOIBP-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
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- Removal Of Specific Substances (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种四氟化铀的溶解方法，该溶解方法包括如下步骤：(1)将四氟化铀和双氧水反应5分钟以上，所述四氟化铀和所述双氧水中的H2O2的摩尔比大于等于1:1；(2)加入氨水反应5分钟以上，所述氨水中的NH3·H2O与所述双氧水中的H2O2的摩尔比大于等于2:3；(3)加入硝酸，加热至120℃以上，反应即可；所述硝酸中的HNO3与所述双氧水中的H2O2的摩尔比大于等于1.3:1。本发明的溶解方法能够使四氟化铀溶解最大化，且溶样时间短，充分提高了四氟化铀的使用率，降低了四氟化铀的使用浪费。The invention discloses a method for dissolving uranium tetrafluoride. The dissolving method comprises the following steps: (1) reacting uranium tetrafluoride and hydrogen peroxide for more than 5 minutes ; The molar ratio of O 2 is greater than or equal to 1:1; (2) add ammonia water and react for more than 5 minutes, and the molar ratio of NH 3 ·H 2 O in the ammonia water to H 2 O 2 in the hydrogen peroxide is greater than or equal to 2:3 (3) Add nitric acid, heat to above 120°C, and react; the molar ratio of HNO 3 in the nitric acid to H 2 O 2 in the hydrogen peroxide is greater than or equal to 1.3:1. The dissolution method of the invention can maximize the dissolution of uranium tetrafluoride, and the sample dissolution time is short, which fully improves the utilization rate of uranium tetrafluoride and reduces the use waste of uranium tetrafluoride.
Description
技术领域technical field
本发明涉及一种四氟化铀的溶解方法。The invention relates to a method for dissolving uranium tetrafluoride.
背景技术Background technique
为了将四氟化铀(UF4)从乏燃料中分离出来，经进一步处理加工后返回到反应堆再次利用，达到燃料循环使用的目的，在核燃料后处理流程水法段，需要研究如何提高UF4在水溶液中的溶解率，以实现UF4的有效分离、回收和利用。已有的溶解UF4的方法是使用双氧水与硝酸体系，但采用此方法溶解UF4时为保证UF4中的U4+可以完全被氧化为UO2 2+通常会加入过量的双氧水，然而过量的双氧水又会与氧化生成的UO2 2+离子反应生成UO4，造成UF4的溶解效率不高，导致UF4的使用浪费。因此，如何提高UF4的溶解效率和使用率已成为本领域面临的重要课题。In order to separate uranium tetrafluoride (UF 4 ) from spent fuel, return it to the reactor for reuse after further processing, and achieve the purpose of fuel recycling, in the water section of the nuclear fuel reprocessing process, it is necessary to study how to increase UF 4 Dissolution rate in aqueous solution to achieve effective separation, recovery and utilization of UF4 . The existing method of dissolving UF 4 is to use hydrogen peroxide and nitric acid system, but when dissolving UF 4 by this method, in order to ensure that U 4+ in UF 4 can be completely oxidized to UO 2 2+ , an excess of hydrogen peroxide is usually added, but the excess The hydrogen peroxide will react with the UO 2 2+ ions generated by oxidation to form UO 4 , resulting in low dissolution efficiency of UF 4 , resulting in wasted use of UF 4 . Therefore, how to improve the dissolution efficiency and utilization rate of UF 4 has become an important issue in this field.
发明内容Contents of the invention
本发明所要解决的技术问题在于克服现有的四氟化铀溶解效率不高以及使用率不高的缺陷，提供一种四氟化铀的溶解方法。本发明的溶解方法能够使UF4溶解最大化，且溶样时间短，充分提高了UF4的使用率，降低了UF4的使用浪费。The technical problem to be solved by the present invention is to overcome the existing defects of low dissolving efficiency and low utilization rate of uranium tetrafluoride, and provide a method for dissolving uranium tetrafluoride. The dissolution method of the present invention can maximize the dissolution of UF 4 , and the sample dissolution time is short, which fully improves the utilization rate of UF 4 and reduces the waste of UF 4 in use.
本发明提供了一种四氟化铀的溶解方法，其包括如下步骤：The invention provides a method for dissolving uranium tetrafluoride, which comprises the steps of:
(1)将四氟化铀和双氧水反应5分钟以上，所述四氟化铀和所述双氧水中的H2O2的摩尔比大于等于1:1；(1) reacting uranium tetrafluoride and hydrogen peroxide for more than 5 minutes, the molar ratio of the uranium tetrafluoride and the H2O2 in the hydrogen peroxide is greater than or equal to 1:1;
(2)加入氨水反应5分钟以上，所述氨水中的NH3·H2O与所述双氧水中的H2O2的摩尔比大于等于2:3；(2) add ammonia water and react for more than 5 minutes, the molar ratio of NH 3 ·H 2 O in the ammonia water to H 2 O 2 in the hydrogen peroxide is greater than or equal to 2:3;
(3)加入硝酸，加热至120℃以上，反应即可；所述硝酸中的HNO3与所述双氧水中的H2O2的摩尔比大于等于1.3:1。(3) Add nitric acid, heat to above 120°C, and react; the molar ratio of HNO 3 in the nitric acid to H 2 O 2 in the hydrogen peroxide is greater than or equal to 1.3:1.
步骤(1)中，所述反应可在室温下进行，所述反应时间不少于5分钟可避免因反应不充分而导致杂质的产生。In step (1), the reaction can be carried out at room temperature, and the reaction time is not less than 5 minutes to avoid the generation of impurities due to insufficient reaction.
步骤(1)中，所述双氧水的浓度较佳地为10～40wt％。In step (1), the concentration of the hydrogen peroxide is preferably 10-40 wt%.
步骤(1)中，所述四氟化铀和所述双氧水中的H2O2的摩尔比较佳地大于等于2.4:1。In step (1), the molar ratio between the uranium tetrafluoride and the H 2 O 2 in the hydrogen peroxide is preferably greater than or equal to 2.4:1.
步骤(2)中，所述氨水的浓度较佳地为25～30wt％。In step (2), the concentration of the ammonia water is preferably 25-30 wt%.
步骤(2)中，所述氨水中的NH3·H2O与所述双氧水中的H2O2的摩尔比较佳地大于等于1.1:1。In step (2), the molar ratio of NH 3 ·H 2 O in the ammonia water to H 2 O 2 in the hydrogen peroxide solution is preferably greater than or equal to 1.1:1.
步骤(2)中，所述反应可在室温下进行。In step (2), the reaction can be carried out at room temperature.
步骤(3)中，在所述加入硝酸前，较佳地还进行加热处理，以除去过量的氨水，防止生成(NH4)2UO2(NO3)4。In step (3), before adding nitric acid, heat treatment is preferably performed to remove excess ammonia water and prevent the formation of (NH 4 ) 2 UO 2 (NO 3 ) 4 .
步骤(3)中，所述硝酸的浓度较佳地为50～69wt％。In step (3), the concentration of the nitric acid is preferably 50-69 wt%.
步骤(3)中，所述加热较佳地为敞口加热，以除去反应中产生的氢氟酸，以免反应逆行。所述反应的时间较佳地为至四氟化铀完全溶解所需的时间。In step (3), the heating is preferably open heating, so as to remove the hydrofluoric acid generated during the reaction, so as to prevent the reaction from going backwards. The reaction time is preferably the time required for the complete dissolution of uranium tetrafluoride.
步骤(3)中，所述反应结束后，较佳地还进行如下处理：将所得样品冷却至室温，然后加入去离子水溶解定容。In step (3), after the reaction is completed, the following treatment is preferably carried out: cooling the obtained sample to room temperature, and then adding deionized water to dissolve to a constant volume.
本发明中，所述室温指的是室内环境温度，一般为20～30℃。In the present invention, the room temperature refers to the indoor ambient temperature, which is generally 20-30°C.
在符合本领域常识的基础上，上述各优选条件，可任意组合，即得本发明各较佳实例。On the basis of conforming to common knowledge in the field, the above-mentioned preferred conditions can be combined arbitrarily to obtain preferred examples of the present invention.
本发明所用试剂和原料均市售可得。The reagents and raw materials used in the present invention are all commercially available.
本发明的积极进步效果在于：The positive progress effect of the present invention is:
本发明的溶解方法选用双氧水、氨水和硝酸作为溶剂，使得四氟化铀的溶解最大化，且溶样时间短，充分提高了四氟化铀的使用率，降低了使用浪费。The dissolution method of the invention uses hydrogen peroxide, ammonia water and nitric acid as solvents to maximize the dissolution of uranium tetrafluoride, and the sample dissolution time is short, which fully improves the utilization rate of uranium tetrafluoride and reduces use waste.
具体实施方式detailed description
下面通过实施例的方式进一步说明本发明，但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法，按照常规方法和条件，或按照商品说明书选择。The present invention is further illustrated below by means of examples, but the present invention is not limited to the scope of the examples. For the experimental methods that do not specify specific conditions in the following examples, select according to conventional methods and conditions, or according to the product instructions.
下述实施例中，所用四氟化铀和溶剂均市售可得。In the following examples, the uranium tetrafluoride and solvents used are commercially available.
实施例1Example 1
一种四氟化铀的溶解方法，其包括如下步骤：称取120mg的四氟化铀，依次向其中加入1.7mL浓度为30wt％的双氧水，室温反应5分钟；加入3.4mL浓度为30wt％的氨水，室温反应5分钟；加入2.2mL浓度为68wt％的硝酸，加热至120～130℃，除去反应中生成的氢氟酸，冷却至室温，向冷却后样品中加去离子水溶解定容至10mL。整个四氟化铀的溶样时间在25～30min。A method for dissolving uranium tetrafluoride, comprising the steps of: weighing 120 mg of uranium tetrafluoride, sequentially adding 1.7 mL of hydrogen peroxide with a concentration of 30 wt %, and reacting at room temperature for 5 minutes; adding 3.4 mL of hydrogen peroxide with a concentration of 30 wt % Ammonia, react at room temperature for 5 minutes; add 2.2mL of nitric acid with a concentration of 68wt%, heat to 120-130°C, remove hydrofluoric acid generated in the reaction, cool to room temperature, add deionized water to the cooled sample to dissolve and dilute to 10mL. The sample dissolution time of the whole UF4 is 25-30min.
实施例2Example 2
一种四氟化铀的溶解方法，其包括如下步骤：称取100mg的四氟化铀，依次向其中加入4.3mL浓度为10wt％的双氧水，室温反应10分钟；加入8.6mL浓度为30wt％的氨水，室温反应5分钟；加入5.6mL浓度为69wt％的硝酸，加热至120～130℃，除去反应中生成的氢氟酸，冷却至室温，向冷却后样品中加去离子水溶解定容至10mL。整个四氟化铀的溶样时间在25～30min。A method for dissolving uranium tetrafluoride, comprising the steps of: weighing 100 mg of uranium tetrafluoride, sequentially adding 4.3 mL of hydrogen peroxide with a concentration of 10 wt %, and reacting at room temperature for 10 minutes; adding 8.6 mL of hydrogen peroxide with a concentration of 30 wt % Ammonia, react at room temperature for 5 minutes; add 5.6mL of nitric acid with a concentration of 69wt%, heat to 120-130°C, remove hydrofluoric acid generated in the reaction, cool to room temperature, add deionized water to the cooled sample to dissolve and dilute to 10mL. The sample dissolution time of the whole UF4 is 25-30min.
实施例3Example 3
一种四氟化铀的溶解方法，其包括如下步骤：称取150mg的四氟化铀，依次向其中加入1.6mL浓度为40wt％的双氧水，室温反应10分钟；加入3.9mL浓度为25wt％的氨水，室温反应10分钟；加入2.8mL浓度为50wt％的硝酸，加热至120～130℃，除去反应中生成的氢氟酸，冷却至室温，向冷却后样品中加去离子水溶解定容至10mL。整个四氟化铀的溶样时间在25～30min。A method for dissolving uranium tetrafluoride, comprising the steps of: weighing 150 mg of uranium tetrafluoride, sequentially adding 1.6 mL of hydrogen peroxide with a concentration of 40 wt %, and reacting at room temperature for 10 minutes; adding 3.9 mL of hydrogen peroxide with a concentration of 25 wt % Ammonia water, react at room temperature for 10 minutes; add 2.8mL of 50wt% nitric acid, heat to 120-130°C, remove hydrofluoric acid generated in the reaction, cool to room temperature, add deionized water to the cooled sample to dissolve and dilute to 10mL. The sample dissolution time of the whole UF4 is 25-30min.
对比例1Comparative example 1
一种四氟化铀的溶解方法，其包括如下步骤：称取118mg的四氟化铀，依次向其中加入1.5mL浓度为40wt％的双氧水，室温反应10分钟；加入1.5mL浓度为25wt％的氨水，室温反应10分钟；加入1.5mL浓硝酸，加热至100℃，冷却至室温，其中可明显看到有未完全溶解的四氟化铀固体，向冷却后样品中加去离子水溶解定容至10mL。该对比例整个溶样时间达45分钟，且仍有小部分四氟化铀固体未完全溶解。A method for dissolving uranium tetrafluoride, comprising the steps of: weighing 118 mg of uranium tetrafluoride, adding 1.5 mL of hydrogen peroxide with a concentration of 40 wt % therein, and reacting at room temperature for 10 minutes; adding 1.5 mL of hydrogen peroxide with a concentration of 25 wt % Ammonia water, react at room temperature for 10 minutes; add 1.5mL of concentrated nitric acid, heat to 100°C, cool to room temperature, there is obviously incompletely dissolved uranium tetrafluoride solid, add deionized water to the cooled sample to dissolve to volume to 10mL. In this comparative example, the entire sample dissolution time is 45 minutes, and there is still a small part of uranium tetrafluoride solid that is not completely dissolved.
效果实施例1Effect Example 1
采用2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)紫外分光光度法分析实施例1和对比例1中四氟化铀的U浓度，根据计算公式溶解率＝实际浓度值/理论浓度值计算UF4的溶解率，其中，UF4实际浓度值是根据紫外分析方法得到的U浓度结合稀释的倍数以及定容的体积得到。经计算，实施例1的UF4溶解率大于97％，对比例1的UF4溶解率仅为80％。由此可见，本发明的溶解方法显著提高了UF4在水溶液中的溶解率。Adopt 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) ultraviolet spectrophotometry to analyze the U concentration of uranium tetrafluoride in embodiment 1 and comparative example 1, according to Calculation formula Dissolution rate = actual concentration value/theoretical concentration value to calculate the dissolution rate of UF 4 , wherein the actual concentration value of UF 4 is obtained from the U concentration obtained by the ultraviolet analysis method combined with the dilution multiple and the constant volume. It is calculated that the UF4 dissolution rate of Example 1 is greater than 97%, and the UF4 dissolution rate of Comparative Example 1 is only 80%. It can be seen that the dissolution method of the present invention significantly improves the dissolution rate of UF in aqueous solution .
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| CN112176393A (en) * | 2020-09-28 | 2021-01-05 | 中核四川环保工程有限责任公司 | Electrochemical decontamination electrolyte and preparation method and application thereof |
| CN112710776A (en) * | 2020-11-26 | 2021-04-27 | 中核北方核燃料元件有限公司 | Oxidation-reduction titration detection method for uranium content in uranium tetrachloride |
| CN116354314A (en) * | 2021-12-27 | 2023-06-30 | 核工业北京化工冶金研究院 | Method for improving nitric acid solubility of uranium peroxide product |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109637686A (en) * | 2018-12-27 | 2019-04-16 | 中核四0四有限公司 | A kind of purifying treatment method for green salt fluorination tail gas leacheate |
| CN109637686B (en) * | 2018-12-27 | 2023-03-17 | 中核四0四有限公司 | Purification treatment method for uranium tetrafluoride fluorinated tail gas leacheate |
| CN112176393A (en) * | 2020-09-28 | 2021-01-05 | 中核四川环保工程有限责任公司 | Electrochemical decontamination electrolyte and preparation method and application thereof |
| CN112176393B (en) * | 2020-09-28 | 2021-09-21 | 中核四川环保工程有限责任公司 | Electrochemical decontamination electrolyte and preparation method and application thereof |
| US11342092B2 (en) | 2020-09-28 | 2022-05-24 | China Nuclear Sichuan Environmental Protection Engineering Co., Ltd. | Electrolyte for electrochemical decontamination and preparation method and application thereof |
| CN112710776A (en) * | 2020-11-26 | 2021-04-27 | 中核北方核燃料元件有限公司 | Oxidation-reduction titration detection method for uranium content in uranium tetrachloride |
| CN116354314A (en) * | 2021-12-27 | 2023-06-30 | 核工业北京化工冶金研究院 | Method for improving nitric acid solubility of uranium peroxide product |
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