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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- dissolving method
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Abstract
The invention discloses a dissolving method for uranium tetrafluoride. The dissolving method comprises the following steps: (1) subjecting uranium tetrafluoride and hydrogen peroxide to a reaction for 5 minutes or more, wherein the mole ratio of uranium tetrafluoride to H2O2 in hydrogen peroxide is greater than or equal to 1: 1; (2) adding ammonia water into the reaction solution, and carrying out a reaction of 5 minutes or more, wherein the mole ratio of NH3.H2O in the ammonia water to H2O2 in hydrogen peroxide is greater than or equal to 2: 3; and (3) adding nitric acid into the reaction solution, heating the reaction solution to the temperature of 120 DEG C or above, and carrying out a reaction, thereby dissolving uranium tetrafluoride, wherein the mole ratio of HNO3 in nitric acid to H2O2 in hydrogen peroxide is greater than or equal to 1.3: 1. According to the dissolving method disclosed by the invention, the uranium tetrafluoride can be dissolved to the maximum, and the dissolving time is short, so that the utilization ratio of uranium tetrafluoride is increased thoroughly, and the waste of use of uranium tetrafluoride is lowered.
Description
Technical field
The present invention relates to a kind of dissolving method of green salt.
Background technology
In order to by green salt (UF4) separate from spentnuclear fuel, return after processing after further treatment
Return to reactor to reuse, reach the purpose of fuel recycle use, in nuclear fuel reprocessing flow process water law
Section, needs how research improves UF4Dissolution rate in aqueous, to realize UF4Efficiently separate,
Reclaim and utilize.Existing dissolving U F4Method be using hydrogen peroxide and nitric acid system, but adopt this side
Method dissolving U F4When for ensure UF4In U4+UO can be oxidized to completely2 2+Excess would generally be added
Hydrogen peroxide, but the hydrogen peroxide of excess again can with oxidation generate UO2 2+Ionic reaction generates UO4,
Cause UF4Dissolved efficiency not high, lead to UF4Using waste.Therefore, how to improve UF4Molten
Solution efficiency and utilization rate have become the important topic that this area faces.
Content of the invention
The technical problem to be solved be to overcome existing green salt dissolved efficiency not high with
And the defect that utilization rate is not high, a kind of dissolving method of green salt is provided.The dissolving method energy of the present invention
Enough make UF4Dissolving maximizes, and the molten sample time is short, substantially increases UF4Utilization rate, reduce
UF4Using waste.
The invention provides a kind of dissolving method of green salt, it comprises the steps：
(1) green salt and hydrogen peroxide are reacted more than 5 minutes, described green salt and described dioxygen
H in water2O2Mol ratio be more than or equal to 1:1；
(2) ammonia is added to react more than 5 minutes, the NH in described ammonia3·H2O and described hydrogen peroxide
In H2O2Mol ratio be more than or equal to 2:3；
(3) add nitric acid, be heated to more than 120 DEG C, react；HNO in described nitric acid3
With the H in described hydrogen peroxide2O2Mol ratio be more than or equal to 1.3:1.
In step (1), described reaction can be carried out at room temperature, and the described response time is no less than 5 minutes
Can avoid because reacting generation that is insufficient and leading to impurity.
In step (1), the concentration of described hydrogen peroxide is preferably 10～40wt%.
H in step (1), in described green salt and described hydrogen peroxide2O2Mol ratio preferably big
In equal to 2.4:1.
In step (2), the concentration of described ammonia is preferably 25～30wt%.
NH in step (2), in described ammonia3·H2H in O and described hydrogen peroxide2O2Mole
Than preferably more than or equal to 1.1:1.
In step (2), described reaction can be carried out at room temperature.
In step (3), before described addition nitric acid, preferably also carry out heat treated, to remove
The ammonia of amount, prevents from generating (NH4)2UO2(NO3)4.
In step (3), the concentration of described nitric acid is preferably 50～69wt%.
In step (3), described heating is preferably heating in the open, with the hydrogen fluorine producing in dereaction
Acid, in order to avoid reaction is driven in the wrong direction.The time of described reaction preferably to green salt be completely dissolved required when
Between.
In step (3), after described reaction terminates, preferably also it is handled as follows：By gained sample
It is cooled to room temperature, be subsequently adding deionized water dissolving constant volume.
In the present invention, described room temperature refers to indoor environment temperature, generally 20～30 DEG C.
On the basis of meeting common sense in the field, above-mentioned each optimum condition, can combination in any, obtain final product this
Bright each preferred embodiments.
Agents useful for same of the present invention and raw material are all commercially available.
The positive effect of the present invention is：
The dissolving method of the present invention selects hydrogen peroxide, ammonia and nitric acid as solvent so that green salt
Dissolving maximizes, and the molten sample time is short, substantially increases the utilization rate of green salt, reduces using wave
Take.
Specific embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention to
Among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, according to normal
Rule method and condition, or select according to catalogue.
In following embodiments, green salt used and solvent are all commercially available.
Embodiment 1
A kind of dissolving method of green salt, it comprises the steps：Weigh the green salt of 120mg,
It is added thereto to the hydrogen peroxide that 1.7mL concentration is 30wt%, room temperature reaction 5 minutes successively；Add 3.4mL
Concentration is the ammonia of 30wt%, room temperature reaction 5 minutes；Add the nitric acid that 2.2mL concentration is 68wt%,
It is heated to 120～130 DEG C, except the Fluohydric acid. of generation in dereaction, be cooled to room temperature, the sample to after cooling
In plus deionized water dissolving be settled to 10mL.The molten sample time of whole green salt is in 25～30min.
Embodiment 2
A kind of dissolving method of green salt, it comprises the steps：Weigh the green salt of 100mg,
It is added thereto to the hydrogen peroxide that 4.3mL concentration is 10wt%, room temperature reaction 10 minutes successively；Add
8.6mL concentration is the ammonia of 30wt%, room temperature reaction 5 minutes；5.6mL concentration is added to be 69wt%'s
Nitric acid, is heated to 120～130 DEG C, except the Fluohydric acid. of generation in dereaction, is cooled to room temperature, to cooling
Add deionized water dissolving afterwards in sample and be settled to 10mL.The molten sample time of whole green salt exists
25～30min.
Embodiment 3
A kind of dissolving method of green salt, it comprises the steps：Weigh the green salt of 150mg,
It is added thereto to the hydrogen peroxide that 1.6mL concentration is 40wt%, room temperature reaction 10 minutes successively；Add
3.9mL concentration is the ammonia of 25wt%, room temperature reaction 10 minutes；Addition 2.8mL concentration is 50wt%
Nitric acid, be heated to 120～130 DEG C, except the Fluohydric acid. generating in dereaction, be cooled to room temperature, Xiang Leng
But add deionized water dissolving in sample after and be settled to 10mL.The molten sample time of whole green salt exists
25～30min.
Comparative example 1
A kind of dissolving method of green salt, it comprises the steps：Weigh the green salt of 118mg,
It is added thereto to the hydrogen peroxide that 1.5mL concentration is 40wt%, room temperature reaction 10 minutes successively；Add
1.5mL concentration is the ammonia of 25wt%, room temperature reaction 10 minutes；Add 1.5mL concentrated nitric acid, heating
To 100 DEG C, it is cooled to room temperature, wherein can be clearly visible the green salt solid not being completely dissolved, to
Add deionized water dissolving in sample after cooling and be settled to 10mL.Entirely the molten sample time reaches 45 points to this comparative example
Clock, and still have fraction green salt solid not to be completely dissolved.
Effect example 1
Using 2- (5- Bromo-2-pyridylazo) -5- diethylamino phenol (5-Br-PADAP) ultraviolet spectrophotometry
The U concentration of green salt in analysis embodiment 1 and comparative example 1, according to computing formula dissolution rate=reality
Concentration value/theoretical concentration value calculates UF4Dissolution rate, wherein, UF4Actual concentrations value is to be divided according to ultraviolet
The volume of multiple and constant volume that the U concentration that analysis method obtains combines dilution obtains.It is computed, embodiment
1 UF4Dissolution rate is more than 97%, the UF of comparative example 14Dissolution rate is only 80%.As can be seen here, originally
The dissolving method of invention significantly improves UF4Dissolution rate in aqueous.
Claims (10)
1. a kind of dissolving method of green salt is it is characterised in that it comprises the steps：
(1) green salt and hydrogen peroxide are reacted more than 5 minutes, described green salt and described dioxygen
H in water2O2Mol ratio be more than or equal to 1:1；
(2) ammonia is added to react more than 5 minutes, the NH in described ammonia3·H2O and described hydrogen peroxide
In H2O2Mol ratio be more than or equal to 2:3；
(3) add nitric acid, be heated to more than 120 DEG C, react；HNO in described nitric acid3
With the H in described hydrogen peroxide2O2Mol ratio be more than or equal to 1.3:1.
2. dissolving method as claimed in claim 1 is it is characterised in that in step (1), described anti-
Should carry out at room temperature；
And/or, in step (2), described reaction is carried out at room temperature.
3. dissolving method as claimed in claim 1 is it is characterised in that in step (1), described double
The concentration of oxygen water is 10～40wt%.
4. dissolving method as claimed in claim 1 is it is characterised in that in step (1), and described four
H in uranium fluoride and described hydrogen peroxide2O2Mol ratio be more than or equal to 2.4:1.
5. dissolving method as claimed in claim 1 is it is characterised in that in step (2), described ammonia
The concentration of water is 25～30wt%.
6. dissolving method as claimed in claim 1 is it is characterised in that in step (2), described ammonia
NH in water3·H2H in O and described hydrogen peroxide2O2Mol ratio be more than or equal to 1.1:1.
7. dissolving method as claimed in claim 1 is it is characterised in that in step (3), described
Before adding nitric acid, also carry out heat treated.
8. dissolving method as claimed in claim 1 is it is characterised in that in step (3), described nitre
The concentration of acid is 50～69wt%.
9. dissolving method as claimed in claim 1 is it is characterised in that in step (3), described plus
Heat is heating in the open；
And/or, the time of described reaction is to be completely dissolved the required time to green salt.
10. dissolving method as claimed in claim 1 is it is characterised in that in step (3), described
After reaction terminates, also it is handled as follows：Gained sample is cooled to room temperature, is subsequently adding deionized water
Dissolving constant volume.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
-
2015
- 2015-08-10 CN CN201510486616.9A patent/CN106409372B/en active Active
Non-Patent Citations (6)
| Title |
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| C.A.LAUE .ET 1L: "Dissolution of metallic and its alloys", 《JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY》 * |
| F.BUNUS .ET AL: "chemical analysisi of UF4 obtained in a wet process", 《JOURNAL OF RADIOANALYTICAL CHEMISRY》 * |
| 吴王锁 等: "离子交换法分离/分光光度法测定四氟化铀中的微量钍", 《原子能科学技术》 * |
| 吴王锁 等: "萃取分离--化学光谱法测定UF4中18中微量杂质元素", 《原子能科学技术》 * |
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| 郑小北 等: "载体盐组成对UF4溶解行为的研究", 《中国核学会会议论文集》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN106409372B (en) | 2019-05-07 |
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