CN106745278B - A method of detergent and ammonium diuranate for ammonium diuranate remove fluorine - Google Patents
A method of detergent and ammonium diuranate for ammonium diuranate remove fluorine Download PDFInfo
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- CN106745278B CN106745278B CN201611060134.8A CN201611060134A CN106745278B CN 106745278 B CN106745278 B CN 106745278B CN 201611060134 A CN201611060134 A CN 201611060134A CN 106745278 B CN106745278 B CN 106745278B
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- fluorine
- ammonium diuranate
- detergent
- ammonium
- diuranate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G43/00—Compounds of uranium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of method that detergent for ammonium diuranate and ammonium diuranate remove fluorine, in detergent provided by the invention, contain and UO2 2+Ion component with stronger mating capability can effectively wash out the fluorine ion in ADU, can be by UO2F2The fluorine of the mass fraction about 5% contained in the ADU of material system preparation is reduced to 0.7%, in this way, using this detergent in nuclear fuel manufacturing process, after handling intermediate product ammonium diuranate, fluorine be can be effectively reduced to preparing the corrosion-damaged of fuel engineering equipment, meanwhile fluorine content is also less in the nuclear fuel finally obtained, can effectively avoid or mitigate fuel element cladding inner surface oxidation film caused by fluorine subtracting blunt situation；The invention discloses a kind of methods that ammonium diuranate removes fluorine can effectively realize above-mentioned purpose using this method simultaneously, meanwhile, this method goes fluorine technique compared to existing nuclear fuel, also have the advantages that it is easy to operate, be easily achieved.
Description
Technical field
The present invention relates to nuclear material manufacturing technology fields, more particularly to a kind of detergent for ammonium diuranate and weight uranium
The method that sour ammonium removes fluorine.
Background technique
Preparing nuclear fuel (UO2Pellet fuel, high burnup UO2Ball-type fuel etc.) during, ammonium diuranate (ADU) is weight
The intermediate product wanted.It is prepared in intermediate product and nuclear fuel in nuclear fuel it is desirable to control F content in reduced levels.Reason
Be: on the one hand, F is a kind of highly corrosive agents, in ADU the F of too high levels to prepare fuel engineering equipment have it is stronger corrosion-damaged；
On the other hand, in nuclear fuel F may cause fuel element cladding inner surface oxidation film subtract it is blunt, to the hydrogen embrittlement of involucrum play luring and
Facilitation reduces safe operation and the phase in longevity of nuclear fuel.In UO2Have strictly in pellet fuel preparation process to residual fluorine content
It is required that: presurized water reactor UO2Fluorine content requirement≤100ug/gU of powder, heavy water reactor UO2Fluorine content requirement≤30ug/gU of powder,
Fluorine content requirement≤25ug/gU of mox fuel bead.
By UO2F2Contain the F of about 5% mass fraction in the ADU of material system preparation.F is made with physisorption and chemistry
With in conjunction with ADU, mainly with UO2F2.3NH4F form exists.Therefore, F content how is effectively reduced in ADU to nuclear fuel (UO2
Pellet fuel and UO2Ball-type fuel) production process and performance be of great significance.
Summary of the invention
For in above-mentioned nuclear fuel manufacturing process, fluorine has stronger corrosion-damaged, Yi Jihe to fuel engineering equipment is prepared
In use, fluorine may cause fuel element cladding inner surface oxidation film and subtracts blunt fuel, play luring to the hydrogen embrittlement of involucrum
And facilitation, safe operation and the phase in longevity of nuclear fuel are reduced, F content how is effectively reduced in ADU to nuclear fuel production process
And performance the problem of being of great significance, the present invention provides a kind of detergent for ammonium diuranate and ammonium diuranate to remove fluorine
Method.
To solve the above problems, a kind of side for removing fluorine for the detergent and ammonium diuranate of ammonium diuranate provided by the invention
Method is achieved the goal by following technical essential: a kind of detergent for ammonium diuranate, includes in the ingredient of the detergent
Ammonium carbonate and hydrogen peroxide.
In the present solution, ammonium carbonate is as buffer, for preventing ammonium diuranate from dissolving；Hydrogen oxide and UO2 2-Ion complex energy
Power is strong, may replace the F ion in ammonium diuranate, reaches the technical effect of washing defluorinate.I.e. present solution provides a kind of solute packets
The solution of ammonium carbonate and hydrogen peroxide is included as detergent, is contained in the detergent and UO2 2-Ion with stronger mating capability
Ingredient can effectively remove the fluorine ion in ADU, pass with certain mode of washing washing ADU filter cake to reduce fluorine content in ADU
The mass fraction of fluorine is 3% or so in ADU after the ADU of system goes fluorine mode to remove fluorine, and the quality of fluorine is divided in ADU after the washing of this detergent
Number can be reduced to 0.7% or hereinafter, this buffer provides technical guarantee for the optimization of nuclear fuel preparation process.
As the further technical solution of the above detergent:
The detergent is mixed by sal volatile and hydrogen peroxide solution, and sal volatile and hydrogen peroxide solution
Volume ratio ratio is 1.5~3, and the mass percent concentration of sal volatile is 8%~10%, the quality percentage of hydrogen peroxide solution
Specific concentration is 3%~5%.In the present solution, hydrogen peroxide solution is the aqueous solution of hydrogen peroxide, to ammonium carbonate in detergent and mistake
The restriction of the amount of hydrogen oxide, the detergent that may make this case to provide can in the case where guaranteeing wash environment that ammonium diuranate is stabilized,
Obtain higher washing defluorinate ability.
As preferred proportion mode, the volume ratio ratio of sal volatile and hydrogen peroxide solution is 2.It is mentioned using this programme
The detergent of confession may make that fluorine content mass fraction is reduced to 0.3% in washed rear ammonium diuranate through once washing.
Meanwhile the invention also discloses a kind of method that ammonium diuranate removes fluorine, this method using it is provided above any one
Detergent scheme is washed for carrying out fluorine to ammonium diuranate, the following steps carried out including sequence:
S1, ammonium diuranate is mixed with the detergent, so that ammonium diuranate is scattered in the detergent, is mixed
Object A；
S2, the mixture A is filtered, the filter cake being obtained by filtration is to remove the ammonium diuranate after fluorine.
The above method that this case provides is easy to operate, can effectively wash out the fluorine ion in ADU.Fluorine contains in ADU after washing
Amount can be reduced to 0.7%.
As the further technical solution of above method:
In step sl, the temperature of the detergent is 45 DEG C to 50 DEG C.To the restriction of detergent temperature in this case, it is intended to
One kind is provided in the case where guaranteeing removal efficiency of flouride, a kind of mode that fluorine technique is more easily implemented is provided: by verifying,
The operation temperature of detergent is limited to 45 DEG C to 50 DEG C, the mass fraction for obtaining fluorine in filter cake after washing may make to drop to
0.4% or less；After detergent temperature is higher than 50 DEG C,
Wash temperature influences fluorine content in ammonium diuranate after washing little.
It further include repeating filtration step S3 to promote removal efficiency of flouride, the filtration step S3 that repeats is that will filter last time
The filter cake arrived is mixed with the detergent again, and obtained mixture is for re-filtering.By washing twice, gained filter
The mass fraction of fluorine can drop to 0.2% in cake,
As the specific implementation of step S1, after is container is added in ammonium diuranate by the implementation of above step S1,
The container then is added in the cleaning solution, is well-dispersed in ammonium diuranate in cleaning solution by stirring.The method passes through
Simple stirring, that is, aloow ammonium diuranate to be well-dispersed in detergent.
In order to improve filter efficiency, while ammonium diuranate moisture content is reduced as far as possible, the step S2 uses vacuum filter
It is filtered.
In order to remove the mother liquor for having higher fluorine content in ammonium diuranate as far as possible by filter type, to improve washing fluorine removal effect
Fruit, the moisture content of the ammonium diuranate raw material before going fluorine to wash is not higher than 45%.
The invention has the following advantages:
In detergent provided by the invention, contain and UO2 2+Ion component with stronger mating capability can be washed effectively
Fluorine ion in ADU out, can be by UO2F2The fluorine of the mass fraction about 5% contained in the ADU of material system preparation is reduced to
0.7% and hereinafter, in this way, using this detergent in nuclear fuel manufacturing process, after handling intermediate product ammonium diuranate,
Fluorine be can be effectively reduced to preparing the corrosion-damaged of fuel engineering equipment, meanwhile, in the nuclear fuel finally obtained fluorine content also compared with
Less, it can effectively avoid or mitigate fuel element cladding inner surface oxidation film caused by fluorine to subtract blunt situation；The present invention is public simultaneously
A kind of method that ammonium diuranate removes fluorine has been opened, using this method, can effectively realize above-mentioned purpose, meanwhile, this method is compared
Go fluorine technique in existing nuclear fuel, also have the advantages that it is easy to operate, be easily achieved.
Detailed description of the invention
Fig. 1 is the process flow chart for one specific embodiment of method that a kind of ammonium diuranate of the present invention removes fluorine.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, but structure of the invention be not limited only to it is following
Embodiment.
Embodiment 1:
A kind of detergent for ammonium diuranate includes ammonium carbonate and hydrogen peroxide in the ingredient of the detergent.
In the present solution, ammonium carbonate is as buffer, for preventing ammonium diuranate from dissolving；Hydrogen oxide and UO2 2-Ion complex energy
Power is strong, may replace the F ion in ammonium diuranate, reaches the technical effect of washing defluorinate.I.e. present solution provides a kind of solute packets
The solution of ammonium carbonate and hydrogen peroxide is included as detergent, is contained in the detergent and UO2 2-Ion with stronger mating capability
Ingredient can effectively remove the fluorine ion in ADU, pass with certain mode of washing washing ADU filter cake to reduce fluorine content in ADU
The mass fraction of fluorine is 3% or so in ADU after the ADU of system goes fluorine mode to remove fluorine, and the quality of fluorine is divided in ADU after the washing of this detergent
Number can be reduced to 0.7% or hereinafter, this buffer provides technical guarantee for the optimization of nuclear fuel preparation process.
Embodiment 2:
The present embodiment is further qualified on the basis of embodiment 1: the detergent is by sal volatile and hydrogen peroxide
Solution mixes, and the volume ratio ratio of sal volatile and hydrogen peroxide solution is 1.5~3, the quality hundred of sal volatile
Dividing specific concentration is 8%~10%, and the mass percent concentration of hydrogen peroxide solution is 3%~5%.In the present solution, hydrogen peroxide solution
The as aqueous solution of hydrogen peroxide, the restriction to the amount of ammonium carbonate in detergent and hydrogen peroxide may make washing for this case offer
Higher washing defluorinate ability can be obtained in the case where guaranteeing wash environment that ammonium diuranate is stabilized by washing agent.
As preferred proportion mode, the volume ratio ratio of sal volatile and hydrogen peroxide solution is 2.It is mentioned using this programme
The detergent of confession may make that fluorine content mass fraction is reduced to 0.3% in washed rear ammonium diuranate through once washing.
Embodiment 3:
As shown in Figure 1, present embodiments providing a kind of method that middle enuatrol removes fluorine: meanwhile, the invention also discloses one
The method that kind ammonium diuranate removes fluorine, this method use any one detergent scheme provided above, for carrying out to ammonium diuranate
Fluorine is gone to wash, the following steps carried out including sequence:
S1, ammonium diuranate is mixed with the detergent, so that ammonium diuranate is scattered in the detergent, is mixed
Object A；
S2, the mixture A is filtered, the filter cake being obtained by filtration is to remove the ammonium diuranate after fluorine.
The above method that this case provides is easy to operate, can effectively wash out the fluorine ion in ADU.Fluorine contains in ADU after washing
Amount can be reduced to 0.7%.
Embodiment 4:
The present embodiment is further qualified on the basis of embodiment 3: in step sl, in step sl, the washing
The temperature of agent is 45 DEG C to 50 DEG C.To the restriction of detergent temperature in this case, it is desirable to provide a kind of in the feelings for guaranteeing removal efficiency of flouride
Under condition, a kind of mode that fluorine technique is more easily implemented is provided: by verifying, the operation temperature of detergent being limited to 45
DEG C to 50 DEG C, the mass fraction for obtaining fluorine in filter cake after washing may make to drop to 0.4% or less；It is higher than 50 in detergent temperature
After DEG C, wash temperature influences fluorine content in ammonium diuranate after washing little.
It further include repeating filtration step S3 to promote removal efficiency of flouride, the filtration step S3 that repeats is that will filter last time
The filter cake arrived is mixed with the detergent again, and obtained mixture is for re-filtering.By washing twice, gained filter
The mass fraction of fluorine can drop to 0.2% in cake,
As the specific implementation of step S1, after is container is added in ammonium diuranate by the implementation of above step S1,
The container then is added in the cleaning solution, is well-dispersed in ammonium diuranate in cleaning solution by stirring.The method passes through
Simple stirring, that is, aloow ammonium diuranate to be well-dispersed in detergent.
In order to improve filter efficiency, while ammonium diuranate moisture content is reduced as far as possible, the step S2 uses vacuum filter
It is filtered.
In order to remove the mother liquor for having higher fluorine content in ammonium diuranate as far as possible by filter type, to improve washing fluorine removal effect
Fruit, the moisture content of the ammonium diuranate raw material before going fluorine to wash is not higher than 45%.
Embodiment 5:
It present embodiments provides a kind of specific ammonium diuranate and goes fluorine scheme, relevant raw materials and process control parameter are such as
Shown in lower.
Raw material:
Ammonium diuranate (ADU), by UO2F2System preparation, moisture content is less than 45%；
Ammonium carbonate analyzes pure specification；
Hydrogen peroxide analyzes pure specification；
Deionized water.
Equipment:
Electronic balance；
Graduated cylinder；
Blender；
Flat-panel filter with vacuum filtration function.
Technique and technological parameter:
The sal volatile 2L that mass percent concentration is 8% is measured, the hydrogen peroxide that mass percent concentration is 3% is measured
Cleaning solution A1 is made in solution 1L after mixing；The ammonium diuranate (ADU) that 500g fluorine mass fraction is 5% is weighed to be put into beaker；It will
Cleaning solution A1 is heated to 45 DEG C, and measuring mass percent concentration is that the A1 after 1L heating is added in beaker, quickly stirs ADU and is allowed to
It is well dispersed in cleaning solution, ADU slurry B1 is obtained after dispersion；B1 is filtered on flat-panel filter, the ADU after being washed
Filter cake C1, through analysis detection, ADU fluorine content is 0.5%；Repeat above operation primary, completion ADU defluorinate washing process, washing
By analysis detection, ADU fluorine content is 0.3%.
Embodiment 6:
It present embodiments provides a kind of specific ammonium diuranate and goes fluorine scheme, contain according to the washing of following related process parameters
The ADU of higher fluorine content.Its relevant raw materials and process control parameter are as follows.
Raw material:
Ammonium diuranate (ADU), by UO2F2System preparation, moisture content is less than 45%；
Ammonium carbonate analyzes pure specification；
Hydrogen peroxide analyzes pure specification；
Deionized water.
Equipment:
Electronic balance；
Graduated cylinder；
Blender；
Flat-panel filter.
Technique and technological parameter:
The sal volatile 2L that mass percent concentration is 9% is measured, the hydrogen peroxide that mass percent concentration is 4% is measured
Cleaning solution A2 is made in solution 1L after mixing；The ammonium diuranate (ADU) that 500g fluorine mass fraction is 5.5% is weighed to be put into beaker；
Cleaning solution A2 is heated to 48 DEG C, measuring mass percent concentration is that the A2 after 1L heating is added in beaker, and quickly stirring ADU makes
Be well dispersed in cleaning solution, ADU slurry B2 is obtained after dispersion；B2 is filtered on flat-panel filter, after being washed
ADU filter cake C2, through analysis detection, ADU fluorine content is 0.3%；Repeat above operation primary, completion ADU defluorinate washing process.It washes
Through analysis detection after washing, ADU fluorine content is 0.2%.
Embodiment 7:
It present embodiments provides a kind of specific ammonium diuranate and goes fluorine scheme, contain according to the washing of following related process parameters
The ADU of higher fluorine content.Its relevant raw materials and process control parameter are as follows.
Raw material:
Ammonium diuranate (ADU), by UO2F2System preparation, moisture content is less than 45%；
Ammonium carbonate is analyzed pure；
Hydrogen peroxide is analyzed pure；
Deionized water.
Equipment:
Electronic balance；
Graduated cylinder；
Blender；
Flat-panel filter.
Technique and technological parameter:
The sal volatile 2L that mass percent concentration is 10% is measured, the dioxygen that mass percent concentration is 5% is measured
Cleaning solution A3 is made in aqueous solution 1L after mixing；The ammonium diuranate (ADU) that 500g fluorine mass fraction is 6% is weighed to be put into beaker；
Cleaning solution A3 is heated to 50 DEG C, measuring mass percent concentration is that the A3 after 1L heating is added in beaker, and quickly stirring ADU makes
Be well dispersed in cleaning solution, ADU slurry B3 is obtained after dispersion；B3 is filtered on the flat-panel filter with vacuum, is obtained
ADU filter cake C3 after washing, through analysis detection, ADU fluorine content is 0.25%；It repeats above operation once, completes ADU defluorinate and wash
Wash process.Through analysis detection after washing, ADU fluorine content is 0.15%.
The above content is combine specific preferred embodiment to the further description of the invention made, and it cannot be said that originally
The specific embodiment of invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs,
The other embodiments obtained in the case where not departing from technical solution of the present invention, should be included within the scope of the present invention.
Claims (6)
1. a kind of method that ammonium diuranate removes fluorine, which is characterized in that this method removes ammonium diuranate using following detergent
Fluorine washing: including ammonium carbonate and hydrogen peroxide in the ingredient of the detergent；The detergent is by sal volatile and hydrogen peroxide
Solution mixes, and the volume ratio ratio of sal volatile and hydrogen peroxide solution is 1.5 ~ 3, the quality percentage of sal volatile
Specific concentration is 8% ~ 10%, and the mass percent concentration of hydrogen peroxide solution is 3% ~ 5%；
The method includes the following steps that sequence carries out:
S1, ammonium diuranate is mixed with the detergent, so that ammonium diuranate is scattered in the detergent, obtains mixture A；
S2, the mixture A is filtered, the filter cake being obtained by filtration is to remove the ammonium diuranate after fluorine.
2. the method that a kind of ammonium diuranate according to claim 1 removes fluorine, which is characterized in that in step sl, described to wash
The temperature for washing agent is 45 DEG C to 50 DEG C.
3. the method that a kind of ammonium diuranate according to claim 1 removes fluorine, which is characterized in that further include repeating filtration step
S3, the filtration step S3 that repeats is to mix the filter cake that last time is obtained by filtration with the detergent again, and mix what is obtained
It is for re-filtering to close object.
4. the method that a kind of ammonium diuranate according to claim 1 removes fluorine, which is characterized in that the realization side of above step S1
Formula is that after container is added in ammonium diuranate, the container then is added in the cleaning solution, keeps ammonium diuranate abundant by stirring
It is scattered in cleaning solution.
5. the method that a kind of ammonium diuranate according to claim 1 removes fluorine, which is characterized in that the step S2 uses vacuum
Filter is filtered.
6. the method that a kind of ammonium diuranate as claimed in any of claims 1 to 5 removes fluorine, which is characterized in that remove fluorine
The moisture content of ammonium diuranate raw material before washing is not higher than 45%.
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| US4155982A (en) * | 1974-10-09 | 1979-05-22 | Wyoming Mineral Corporation | In situ carbonate leaching and recovery of uranium from ore deposits |
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| CN101844812A (en) * | 2009-12-15 | 2010-09-29 | 南华大学 | Process for reducing fluorine in biuranate product |
| CN103601245A (en) * | 2013-11-28 | 2014-02-26 | 中核二七二铀业有限责任公司 | Preparation method of diuranate non-metallic element standard substances |
| CN104192912A (en) * | 2014-08-27 | 2014-12-10 | 南华大学 | Diuranate product fluorine reduction technique |
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2016
- 2016-11-25 CN CN201611060134.8A patent/CN106745278B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4155982A (en) * | 1974-10-09 | 1979-05-22 | Wyoming Mineral Corporation | In situ carbonate leaching and recovery of uranium from ore deposits |
| CN101580775A (en) * | 2008-05-17 | 2009-11-18 | 刘庆民 | Preparation method of toilet deodorization and disinfection cleaning solution |
| CN101844812A (en) * | 2009-12-15 | 2010-09-29 | 南华大学 | Process for reducing fluorine in biuranate product |
| CN103601245A (en) * | 2013-11-28 | 2014-02-26 | 中核二七二铀业有限责任公司 | Preparation method of diuranate non-metallic element standard substances |
| CN104192912A (en) * | 2014-08-27 | 2014-12-10 | 南华大学 | Diuranate product fluorine reduction technique |
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| Title |
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| Recovery of uranium from the filtrate of ‘ammonium diuranate’ prepared from uranium hexafluoride;J.A.Seneda等;《Journal of Alloys and Compounds》;20011231;第838-841页 |
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