CN106636692B - A kind of uranium purification process of ammonium diuranate - Google Patents
A kind of uranium purification process of ammonium diuranate Download PDFInfo
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- CN106636692B CN106636692B CN201611234719.7A CN201611234719A CN106636692B CN 106636692 B CN106636692 B CN 106636692B CN 201611234719 A CN201611234719 A CN 201611234719A CN 106636692 B CN106636692 B CN 106636692B
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- uranium
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- organic phase
- ammonium diuranate
- bearing organic
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0286—Obtaining thorium, uranium, or other actinides obtaining uranium refining, melting, remelting, working up uranium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/381—Phosphines, e.g. compounds with the formula PRnH3-n, with n = 0-3
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
- C22B60/026—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries liquid-liquid extraction with or without dissolution in organic solvents
Abstract
The invention belongs to the dissolution purification process technology fields of ammonium diuranate in uranium purifying conversion process, specifically include the dissolution of ammonium diuranate, the technologies such as uranyl nitrate solution abstraction purification processing.Include the following steps：(1) it dissolves, qualified uranyl nitrate solution is prepared for abstraction purification；(2) it extracts, makes to extract stoste and extractant mixes mass transfer in pulse extraction column, the uranium carrier band in material is entered in extractant, uranium-bearing organic phase is obtained；(3) it washs, so that uranium-bearing organic phase and detergent is sufficiently mixed mass transfer in pulse column scrubber, the impurity element in uranium-bearing organic phase is relaundered into water phase, further increase the purity of uranium, the uranium-bearing organic phase after being purified；(4) it is stripped, purified uranium-bearing organic phase and detergent is made to be sufficiently mixed mass transfer in pulse column scrubber, uranium is stripped again and is entered in water phase, uranyl nitrate solution after purification is obtained；Uranyl nitrate solution after purification prepares uranium oxide by way of denitration is concentrated again.
Description
Technical field
The invention belongs to the dissolution purification process technology fields of ammonium diuranate in uranium purifying conversion process, specifically include
The dissolution of ammonium diuranate, the technologies such as uranyl nitrate solution abstraction purification processing.
Background technique
Presently disclosed uranium purifying conversion building of production line project construction line uses front end wet process purification technique, dense with uranium ore
Contracting object (U3O8) it is raw material, uranyl nitrate solution is obtained through dissolution, abstraction purification.Uranyl nitrate solution after being concentrated by evaporation, leads to again
It crosses denitration and obtains UO3, UO3It is restored after hydration improves activity again and UO is made2。UO2Again through works such as hydrofluorination, fluorination, condensation liquefactions
The UF for meeting natural hex technical conditions is made in sequence6Product.Once raw material sources, chemical form and its impurity form and contain
Amount varies widely, the production line and its can auxiliary facility meet safety in production, continuous and steady operation requirement waits to confirm.
When uranium purifies conversion Design of Production Line, with U3O8Front end wet process purifying process is used for raw material production, utilizes HNO3
Solution dissolution prepares uranyl nitrate solution, recycles TBP big to uranium saturated capacity, is having close under saturation conditions to impurity element
The characteristics of higher detergent power, is finally completed the purification purification of uranium.
For ammonium diuranate during the wet technique refinement of uranium, there are two types of selections：First is that by the way of high-temperature calcination, cracking system
Standby triuranium octoxide out, then by dissolution purifying process, prepare the qualified uranyl nitrate solution of purification；Second is that directly will weight uranium
Sour ammonium dissolution, carries out purifying purification, but can generate a large amount of waste liquor of ammonium containing nitric acid.
To reduce technique change as far as possible, the purifying conversion production line raw tissue production using ammonium diuranate material as uranium
When, using the method directly dissolved, the adaptability and process conditions and control parameter of existing equipment are required to explore and test
Card.
In uranium purifying conversion process, raw material that existing equipment form separate sources, chemical form and its impurity is fitted
Answering property is directly related to the processing buying selectional restriction of uranium purifying conversion raw material.In order to further widen uranium purifying conversion process pair
The limitation of raw material needs to develop a kind of ammonium diuranate purification treating method, to realize the uranium refinement purifying of ammonium diuranate.
Summary of the invention
The technical problem to be solved by the present invention is to propose a kind of process for refining and purifying of ammonium diuranate material, weight uranium is realized
The impurity and purification target of uranium in sour ammonium.
In order to realize the purpose, the technical solution adopted by the present invention is that：
A kind of uranium purification process of ammonium diuranate, includes the following steps：
(1) it dissolves
Material is that uranium content is 70-75wt%, is mingled with the ammonium diuranate of uranium-bearing material；
Material is added in the nitric acid solution of 5~10mol/L of acidity by star-shaped feeding machine and is dissolved；
Using the collective effect of mechanical stirring and the empty stirring of pressure, uranyl nitrate solution is prepared into ammonium diuranate dissolution；
Insoluble impurities little particle aggregation in solution is set to be easy to implement separation of solid and liquid by being aged operation；
The solution after ageing is separated with solid impurity by centrifuge separation operation；
The uranium concentration of uranyl nitrate solution is controlled in 400~450g/L by condiment operation, controlling pH is in 0.8mol/
L~3mol/L；
By above-mentioned steps, qualified uranyl nitrate solution is prepared for abstraction purification；
(2) it extracts
1 is pressed in pulse extraction column：0.5~6 stream is than being added extraction stoste and extractant；Wherein, extraction stoste is that step (1) obtains
The uranyl nitrate solution arrived, extractant are tributyl phosphate-diluents；
Make to extract stoste and extractant is sufficiently mixed mass transfer in pulse extraction column, the uranium carrier band in material is entered into extractant
In, obtain uranium-bearing organic phase；
(3) it washs
8~20 are pressed in pulse column scrubber：1 stream is than being added uranium-bearing organic phase and detergent obtained in step 2；Wherein,
Detergent is the nitric acid solution of 0.3~1mol/L；
Uranium-bearing organic phase and detergent is set to be sufficiently mixed mass transfer in pulse column scrubber, by the impurity member in uranium-bearing organic phase
Element is relaundered into water phase, further increases the purity of uranium, the uranium-bearing organic phase after being purified；
(4) it is stripped
Purified uranium-bearing organic phase and stripping agent are pressed 1：1~3 stream is than being added in pulse re-extraction column；Wherein, stripping agent
For deionized water；
So that purified uranium-bearing organic phase and detergent is sufficiently mixed mass transfer in pulse column scrubber, uranium is stripped again into
Enter in water phase, obtains uranyl nitrate solution after purification；
Uranyl nitrate solution after purification prepares uranium oxide by way of denitration is concentrated again.
Further, a kind of uranium purification process of ammonium diuranate as described above, in step (1), solution temperature 40-
100 DEG C, dissolution time 3-6h.
Further, a kind of uranium purification process of ammonium diuranate as described above, in step (1), digestion time is 4~
10h。
Further, a kind of uranium purification process of ammonium diuranate as described above, in step (2), in extractant, tricresyl phosphate
The volume fraction of butyl ester is 20~30%, and diluent is hydrotreated kerosene.
Further, a kind of uranium purification process of ammonium diuranate as described above, in step (2), pulse extraction column internal control
20~30r/min of pulse frequency processed, 0.02~0.08MPa of pulse.
Further, a kind of uranium purification process of ammonium diuranate as described above, in step (3), pulse column scrubber internal control
20~30r/min of pulse frequency processed, 0.02~0.08MPa of pulse.
Further, a kind of uranium purification process of ammonium diuranate as described above, in step (4), the control of pulse re-extraction column
20~30r/min of pulse frequency, 0.02~0.08MPa of pulse.
The beneficial effect of technical solution of the present invention is：By providing a kind of polishing purification processing technique of ammonium diuranate,
Not only ammonium diuranate can be handled by front end wet process purification technique, expand wet process purifying to the scope of application of raw material, meanwhile, also
It can use pulse extraction column, by the process of extraction, washing and back extraction, impurity elements other in ammonium diuranate removed, it is real
The polishing purification of existing uranium.Finally, by the process route, the engineering application for the purifying of practical ammonium diuranate wet process provides one
Fixed technological operation foundation.
Detailed description of the invention
Fig. 1 is Uranium in Waste Water processing technique process flow diagram.
Specific embodiment
Technical solution of the present invention is described in detail in the following with reference to the drawings and specific embodiments.
By dissolving the analysis of reaction principle to ammonium diuranate and triuranium octoxide, main difference is that ammonium diuranate nitre
Acid dissolution produces ammonium nitrate, and there is no the generations of gas, and the dissolution of triuranium octoxide nitric acid is along with oxides of nitrogen gas
It generates, does not have the introducing of other impurities；This patent proposes following skill as shown in Figure 1 according to the difference of its dissolution reaction
Art scheme：
A kind of uranium purification process of ammonium diuranate, includes the following steps：
(1) it dissolves
Material is that uranium content is 70-75wt%, is mingled with the ammonium diuranate of uranium-bearing material；
Material is added in the nitric acid solution of 5~10mol/L of acidity by star-shaped feeding machine and is dissolved；Solution temperature is
40-100 DEG C, dissolution time 3-6h.
Using the collective effect of mechanical stirring and the empty stirring of pressure, uranyl nitrate solution is prepared into ammonium diuranate dissolution；
Insoluble impurities little particle aggregation in solution is set to be easy to implement separation of solid and liquid by being aged operation；Digestion time is 4
~10h.
The solution after ageing is separated with solid impurity by centrifuge separation operation；
The uranium concentration of uranyl nitrate solution is controlled in 400~450g/L by condiment operation, controlling pH is in 0.8mol/
L~3mol/L；
By above-mentioned steps, qualified uranyl nitrate solution is prepared for abstraction purification；
(2) it extracts
1 is pressed in pulse extraction column：0.5~6 stream is than being added extraction stoste and extractant；Wherein, extraction stoste is that step (1) obtains
The uranyl nitrate solution arrived, extractant are tributyl phosphate-diluents；In extractant, the volume fraction of tributyl phosphate is 20
~30%, diluent is hydrotreated kerosene.
20~30r/min of pulse frequency, 0.02~0.08MPa of pulse are controlled in pulse extraction column, make to extract stoste and
Extractant is sufficiently mixed mass transfer in pulse extraction column, and the uranium carrier band in material is entered in extractant, uranium-bearing organic phase is obtained；
(3) it washs
8~20 are pressed in pulse column scrubber：1 stream is than being added uranium-bearing organic phase and detergent obtained in step 2；Wherein,
Detergent is the nitric acid solution of 0.3~1mol/L；
20~30r/min of pulse frequency is controlled in pulse column scrubber, 0.02~0.08MPa of pulse keeps uranium-bearing organic
Mutually and detergent is sufficiently mixed mass transfer in pulse column scrubber, and the impurity element in uranium-bearing organic phase is relaundered into water phase
In, the purity of uranium is further increased, the uranium-bearing organic phase after being purified；
(4) it is stripped
Purified uranium-bearing organic phase and stripping agent are pressed 1：1~3 stream is than being added in pulse re-extraction column；Wherein, stripping agent
For deionized water；
Pulse re-extraction column controls 20~30r/min of pulse frequency, and 0.02~0.08MPa of pulse makes purified contain
Uranium organic phase and detergent are sufficiently mixed mass transfer in pulse column scrubber, and uranium is stripped again and is entered in water phase, is obtained after purification
Uranyl nitrate solution；
Uranyl nitrate solution after purification prepares uranium oxide by way of denitration is concentrated again.
It is operated by the dissolution purification process of above-mentioned ammonium diuranate, obtains the optimised process behaviour of ammonium diuranate wet process purifying
Make parameter, demonstrate the feasibility of the novel process technology path, provides a kind of efficient stable for the processing of ammonium diuranate
Technology path.
Claims (8)
1. a kind of uranium purification process of ammonium diuranate, which is characterized in that include the following steps：
(1) it dissolves
Material is that uranium content is 70-75wt%, is mingled with the ammonium diuranate of uranium-bearing material；
Material is added in the nitric acid solution of 5~10mol/L of acidity by star-shaped feeding machine and is dissolved；
Using the collective effect of mechanical stirring and the empty stirring of pressure, uranyl nitrate solution is prepared into ammonium diuranate dissolution；
Insoluble impurities little particle aggregation in solution is set to be easy to implement separation of solid and liquid by being aged operation；
The solution after ageing is separated with solid impurity by centrifuge separation operation；
By condiment operation by the control of the uranium concentration of uranyl nitrate solution in 400~450g/L, controlling pH 0.8mol/L~
3mol/L；
By above-mentioned steps, qualified uranyl nitrate solution is prepared for abstraction purification；
(2) it extracts
1 is pressed in pulse extraction column：0.5~6 stream is than being added extraction stoste and extractant；Wherein, extraction stoste is that step (1) obtains
Uranyl nitrate solution, extractant are tributyl phosphate-diluents；
Make to extract stoste and extractant be sufficiently mixed mass transfer in pulse extraction column, the uranium carrier band in material is entered in extractant,
Obtain uranium-bearing organic phase；
(3) it washs
8~20 are pressed in pulse column scrubber：1 stream is than being added uranium-bearing organic phase and detergent obtained in step 2；Wherein, it washs
Agent is the nitric acid solution of 0.3~1mol/L；
Uranium-bearing organic phase and detergent is set to be sufficiently mixed mass transfer in pulse column scrubber, by the impurity element weight in uranium-bearing organic phase
New washing enters in water phase, further increases the purity of uranium, the uranium-bearing organic phase after being purified；
(4) it is stripped
Purified uranium-bearing organic phase and stripping agent are pressed 1：1~3 stream is than being added in pulse re-extraction column；Wherein, stripping agent is to go
Ionized water；
So that purified uranium-bearing organic phase and detergent is sufficiently mixed mass transfer in pulse column scrubber, uranium is stripped again and enters water
Xiang Zhong obtains uranyl nitrate solution after purification；
Uranyl nitrate solution after purification prepares uranium oxide by way of denitration is concentrated again.
2. a kind of uranium purification process of ammonium diuranate as described in claim 1, it is characterised in that：In step (1), solution temperature
It is 40-100 DEG C, dissolution time 3-6h.
3. a kind of uranium purification process of ammonium diuranate as described in claim 1, it is characterised in that：In step (1), digestion time
For 4~10h.
4. a kind of uranium purification process of ammonium diuranate as described in claim 1, it is characterised in that：In step (2), extractant
In, the volume fraction of tributyl phosphate is 20~30%, and diluent is hydrotreated kerosene.
5. a kind of uranium purification process of ammonium diuranate as described in claim 1, it is characterised in that：In step (2), pulse extraction
20~30r/min of pulse frequency, 0.02~0.08MPa of pulse are controlled in column.
6. a kind of uranium purification process of ammonium diuranate as described in claim 1, it is characterised in that：In step (3), pulse washing
20~30r/min of pulse frequency, 0.02~0.08MPa of pulse are controlled in column.
7. a kind of uranium purification process of ammonium diuranate as described in claim 1, it is characterised in that：In step (4), pulse back extraction
Column controls 20~30r/min of pulse frequency, 0.02~0.08MPa of pulse.
8. a kind of uranium purification process of ammonium diuranate as described in claim 1, it is characterised in that：In step (1), solution temperature
It is 40-100 DEG C, dissolution time 3-6h；Digestion time is 4~10h；
In step (2), in extractant, the volume fraction of tributyl phosphate is 20~30%, and diluent is hydrotreated kerosene；Pulse extraction
It takes and controls 20~30r/min of pulse frequency, 0.02~0.08MPa of pulse in column；
In step (3), 20~30r/min of pulse frequency, 0.02~0.08MPa of pulse are controlled in pulse column scrubber；
In step (4), pulse re-extraction column controls 20~30r/min of pulse frequency, 0.02~0.08MPa of pulse.
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| CN108165747A (en) * | 2017-12-22 | 2018-06-15 | 中核四0四有限公司 | A kind of abstraction purification method recycled for uranium in fluorination reaction lime-ash |
| CN108441631B (en) * | 2018-01-24 | 2020-03-24 | 中国原子能科学研究院 | Method for recovering uranium from ammonium diuranate precipitation mother liquor |
| CN109036609A (en) * | 2018-07-13 | 2018-12-18 | 清华大学 | It is a kind of spherical shape Nuclear Fuel Element Production Line return product recovery and treatment method |
| CN109518013B (en) * | 2018-11-30 | 2022-02-08 | 中国工程物理研究院材料研究所 | Method for remelting and purifying metal uranium surface by pulse laser and purification layer prepared by method |
| CN109468474A (en) * | 2018-12-27 | 2019-03-15 | 中核四0四有限公司 | A method of for recycling uranium in the waste liquid of-TBP containing nitric acid |
| CN111004920B (en) * | 2019-09-09 | 2021-05-18 | 湖南中核金原新材料有限责任公司 | Method for smelting and separating uranium, thorium and rare earth from monazite excellent slag |
| CN112941317A (en) * | 2019-12-10 | 2021-06-11 | 中核北方核燃料元件有限公司 | Uranium-containing waste liquid purification method |
| CN113023783B (en) * | 2019-12-24 | 2023-04-14 | 中核新能核工业工程有限责任公司 | Method for purifying trace impurities in uranium after stacking |
| CN111349789B (en) * | 2020-04-24 | 2021-08-17 | 核工业北京化工冶金研究院 | Method for purifying caustic sludge leachate uranium with multi-outlet design |
| CN117438123A (en) * | 2023-12-22 | 2024-01-23 | 中国核电工程有限公司 | Method and device for determining uranium extraction zone in extraction column and method for controlling position of uranium extraction zone |
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| CN102127639A (en) * | 2010-12-23 | 2011-07-20 | 核工业北京化工冶金研究院 | Preparation method of high-clarity uranium solution |
| CN102153143A (en) * | 2011-04-15 | 2011-08-17 | 中核北方核燃料元件有限公司 | Technology method and device for preparing ammonium diuranate |
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| US7157061B2 (en) * | 2004-09-24 | 2007-01-02 | Battelle Energy Alliance, Llc | Process for radioisotope recovery and system for implementing same |
| JP6251010B2 (en) * | 2013-11-14 | 2017-12-20 | 株式会社東芝 | Intermediate product storage method and intermediate product manufacturing apparatus |
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| CN102127639A (en) * | 2010-12-23 | 2011-07-20 | 核工业北京化工冶金研究院 | Preparation method of high-clarity uranium solution |
| CN102153143A (en) * | 2011-04-15 | 2011-08-17 | 中核北方核燃料元件有限公司 | Technology method and device for preparing ammonium diuranate |
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