CN110194494A - A method of uranium is recycled by fluorization agent fluorination volatilization of Nitrogen trifluoride - Google Patents
A method of uranium is recycled by fluorization agent fluorination volatilization of Nitrogen trifluoride Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G56/00—Compounds of transuranic elements
- C01G56/004—Compounds of plutonium
- C01G56/006—Halides
Abstract
The present invention provides a kind of methods for recycling uranium as fluorization agent fluorination volatilization using Nitrogen trifluoride, it is the following steps are included: (1) removes the air and water in reactor, the fused salt of compound of the reactor equipped with uranium-bearing, perhaps the compound of the mixture of uranium-bearing simple substance or one or more uranium；The content of uranium element is 0.01%~30% in the fused salt of the compound of uranium-bearing；The mixture of uranium-bearing simple substance is the mixture of uranium simple substance and fission products and/or metal alloy；(2) segmentally heating reactor, first stage are heated to 200 DEG C~250 DEG C by room temperature, keep the temperature for the first time；Second stage is heated to 500 DEG C~750 DEG C by the temperature at the end of the first stage；Second of heat preservation；It is passed through the mixed gas of Nitrogen trifluoride and inert gas, is reacted；Recycle reaction product；Nitrogen trifluoride volume fraction is 5%~50% in the mixed gas.Equipment safety, stable longtime running may be implemented in method of the invention.
Description
Technical field
The present invention relates to a kind of methods for recycling uranium as fluorization agent fluorination volatilization using Nitrogen trifluoride.
Background technique
Without using water as solvent in spentnuclear fuel dry method last handling process, main separating step carries out at high temperature.
In addition, the process of spentnuclear fuel dry method post-processing has many advantages, such as that radiation resistance, low critical risk, radioactive waste are few, suitable treatment
High burnup, short cooling phase spentnuclear fuel.Fluorination volatilization technology is important dry method post-processing technology, by being reacted as follows by lower valency
Uranium fluorination is high-valence state fluoride UF6:
UF4(d)+F2(g)→UF6(g)
Utilize UF6Low boiling point, the volatile separation and recycling that uranium may be implemented, be usually used in natural uranium conversion, uranium combustion
The fields such as recycling of uranium in the purifying and concentration of material and MOX or uranium-bearing hardware.
Molten salt reactor is to melt nuclear fuel to be used as one of the liquid fluorinated salt of coolant fluid fueled reactor.Molten salt reactor
The concept attention new by scientific circles in last century end and the beginning of this century, be chosen as 6 of forth generation reactor candidate heap-type it
One.The big advantage of the one of molten salt reactor is the closed loop mode work of thorium base nuclear fuel and uranium base nuclear fuel utilization.Mode closed loop (follow by enclosed
Ring) it is also known as nuclear fuel recycling, it is to prepare and used into heap again by spentnuclear fuel (used nuclear fuel), nuclear fuel, it is real
Nuclear fuel cycle process is now repeated several times.The separation and recycling of molten salt reactor center fuel uranium are to realize molten salt reactor nuclear fuel cycle
It is crucial.And fluorination volatilization technology can be achieved to the recycling of molten salt system uranium, realize the nuclear fuel cycle of molten salt reactor.
Although the fluorination volatilization technique of uranium has, process is short, equipment is few, easy to operate, reaction speed is fast, separative efficiency
Height, side reaction is few, separation selectivity is good, product purity and decontamination factor are high, is easily achieved many advantages, such as continuous operation, but
It is that prior art needs to use fluorine gas as fluorization agent, fluorine gas is a kind of extremely strong gas of oxidisability, is corroded to process equipment tight
Weight, the especially fluorination reaction under liquid molten salt system, high temperature and fused salt environment make equipment corrosion aggravation.In addition, fluorine gas city
Field price is higher, and safety is poor in production, transport, storage and use, and exists to the health of operator and threaten.
Summary of the invention
The technical problem to be solved by the present invention is in order to overcome fluorination volatilization technique in the prior art to make using fluorine gas
For caused by fluorization agent to process equipment seriously corroded, the defect that service life is short, safety is poor, and provide one kind with three
Nitrogen fluoride is the method that fluorization agent fluorination volatilization recycles uranium.Fluorization agent Nitrogen trifluoride used in method provided by the invention has
Chemical toxicity is low, at room temperature the stable advantage of property, and equipment safety, stable longtime running may be implemented.
The present invention solves above-mentioned technical problem by following technical proposals:
The present invention provides a kind of method for recycling uranium as fluorization agent fluorination volatilization using Nitrogen trifluoride, it is characterized in that, it is described
Method the following steps are included:
(1) air and water in reactor, the fused salt or uranium-bearing list of compound of the reactor equipped with uranium-bearing are removed
The compound of the mixture of matter or one or more uranium；The content of uranium element is in the fused salt of the compound of the uranium-bearing
0.01%~30%, the percentage is mass percent；The mixture of the uranium-bearing simple substance is uranium simple substance and fission products
And/or the mixture of metal alloy.
(2) reactor described in segmentally heating, first stage are heated to 200 DEG C~250 DEG C by room temperature, keep the temperature for the first time；The
Two-stage is heated to 500 DEG C~750 DEG C by the temperature at the end of the first stage；Second of heat preservation；Be passed through Nitrogen trifluoride and
The mixed gas of inert gas, is reacted；Recycle reaction product；Institute in the mixed gas of the Nitrogen trifluoride and inert gas
Stating Nitrogen trifluoride volume fraction is 5%~50%.
In the present invention, the compound of the uranium is preferably green salt, uranyl fluoride, orange oxide, triuranium octoxide
With any one in uranium dioxide.
In the present invention, the fission products are the fission products of this field routine；The metal alloy is this field
Conventional metal alloy, such as uranium zircaloy, nickel-base alloy and aluminium alloy etc..
In the present invention, the fused salt of the compound of the uranium-bearing be mixture A or mixture B, the mixture A by fused salt and
A kind of compound composition of uranium, the mixture B are made of the compound of fused salt and two or more uranium；Preferably, the uranium
Compound is green salt or uranyl fluoride.
In the present invention, fused salt described in the fused salt of the compound of the uranium-bearing is preferably the co-melting salt of fluoride.
In the present invention, the content of uranium element is preferably 0.758%~2.27% in the fused salt of the compound of the uranium-bearing.
Further, the co-melting salt of the fluoride can be the co-melting salt of fluoride of this field routine；Preferably KF-ZrF4
Co-melting salt, NaF-ZrF4Co-melting salt and LiF-BeF4Any one in co-melting salt.
Further, the KF-ZrF4KF and ZrF in co-melting salt4Molar ratio be preferably 58:42；The NaF-
ZrF4NaF and ZrF in co-melting salt4Molar ratio be preferably 58:42；The LiF-BeF2LiF and BeF in co-melting salt2Mole
Than being preferably 67:33.
In the present invention, the mode for removing the air and water in the reactor can be the mode of this field routine, preferably
To remove the air and water in the reactor with inert gas.
Inert gas involved in the present invention can be the inert gas of this field routine, such as in helium, neon and argon gas
It is one or more.
In the present invention, when carrying out the reaction, trifluoro described in the mixed gas of the Nitrogen trifluoride and inert gas
The uranium element content that the dosage of change nitrogen is preferably relative in the reactor is excessive in stoichiometric ratio.
The volume fraction of Nitrogen trifluoride described in the mixed gas of the Nitrogen trifluoride and inert gas is preferably 10%
~50%, it is more preferably 20%~50%.The ventilation flow rate of the mixed gas of the Nitrogen trifluoride and inert gas is preferably
0.2L/min~2L/min is more preferably 0.2L/min~1L/min, is most preferably 0.5L/min~1L/min.
In the present invention, the segmentally heating can remove free water.
In the present invention, during the segmentally heating, the time of the first time heat preservation, preferably 2h~3h.
In the present invention, based on being advanced optimized to raw material, when compound of the reactor equipped with uranium or a variety of uranium
When the mixture of compound, the time of second of heat preservation is preferably 2h~3h.When the reactor is equipped with the uranium-bearing
Compound fused salt when, it is complete that the time of second heat preservation is preferably the fused salt kept the temperature to the compound of the uranium-bearing
Melting is more preferably 3h~for 24 hours.
Those skilled in the art are it should be understood that the temperature of the reaction is the temperature of second of heat preservation, as institute
500 DEG C~750 DEG C of temperature for stating second of heat preservation.
In the present invention, when the reactor is equipped with the raw material containing green salt, the reaction equation of the reaction is preferably
3UF4+2NF3→3UF6+N2。
In the present invention, when the reactor is equipped with the raw material containing uranyl fluoride, the reaction equation of the reaction is preferably
UO2F2+NF3→UF6+N2+O2。
In the present invention, when the reactor is equipped with the raw material containing orange oxide, the reaction equation of the reaction is preferably
UO3+2NF3→UF6+N2+O2。
In the present invention, when the reactor is equipped with the raw material containing triuranium octoxide, the reaction equation of the reaction is preferably
For U3O8+6NF3→3UF6+3N2+2O2。
In the present invention, when the reactor is equipped with the raw material containing uranium dioxide, the reaction equation of the reaction is preferably
UO2+2NF3→UF6+N2+O2。
In the present invention, when the reactor is equipped with the raw material of uranium-bearing simple substance, the reaction equation of the reaction is preferably U+
2NF3→UF6+N2。
In the present invention, the mode of the recycling reaction product can be conventional for this field, preferably condensation method or absorption method.
The condensation method is condensed by using condenser, and the condenser can be the condenser of this field routine, preferably more
Grade condenser.
Preferably, the temperature of the condensation is -70 DEG C to -20 DEG C.
More preferably, the condenser is condensed in two stages device；The temperature of the condensation is respectively -40 DEG C and -60 DEG C.
In the present invention, the absorption method is adsorbed by using the absorber with adsorbent；Extremely to the reactor
The gas piping of the absorber is heated, and the temperature of the heating is preferably 70 DEG C~120 DEG C.
Wherein, the absorber can be the absorber of this field routine, preferably multi-stage absorption device.
Further, the temperature of the absorption is preferably 80 DEG C to 150 DEG C.
Further, the absorber is preferably two-stage absorber, and the temperature of the absorption is preferably 100
℃.Wherein, the adsorbent is preferably sodium fluoride.
In the present invention, during the reaction, according to this field routine, can also proceed as follows: the reaction is produced
UF described in object6When concentration is lower than Monitoring lower-cut, stop the reaction.
Further, preferably, stopping the reaction after reaction progress 1h~8h.
In the present invention, the Monitoring lower-cut is preferably 1ppm.The mode of the detection preferably passes through infrared spectroscopy
The exit gas of reactor described in instrument on-line checking.
In the present invention, stop mixing of the reaction preferably by stopping being passed through the Nitrogen trifluoride and inert gas
Gas is realized.
Preferably, the mode for being passed through the mixed gas of the Nitrogen trifluoride and inert gas is continuously to be passed through；
Wherein, time of the mixed gas of the Nitrogen trifluoride and inert gas and the time one reacted continuously are passed through
It causes.
In the present invention, preferably, being blown using inert gas the reactor and pipeline after stopping the reaction
It sweeps；Then the reactor is vacuumized, primary purging, which adds, once to be vacuumized as one cycle；The circulation is 4~8 times,
Preferably 6 times.
When purging, the flow velocity of the inert gas is 0.3L/min~0.8L/min, preferably 0.6L/min.
The time of the purging is preferably 20min~50min, is more preferably 30min.
In the present invention, the room temperature be room temperature well known to those skilled in the art, as 5 DEG C~40 DEG C.
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition, can any combination to get the present invention it is each preferably
Example.
The positive effect of the present invention is that: the present invention provides one kind and passes through fluorination volatilization by fluorization agent of Nitrogen trifluoride
The method that technology recycles uranium from uranium-bearing raw material, this method have the advantages that
1) Nitrogen trifluoride chemical toxicity is low, and property is stablized under room temperature, therefore the safety in production, transport, storage and use
Property is higher；
2) service life of equipment is long, and the oxidisability of Nitrogen trifluoride is lower than fluorine gas at high temperature, weaker to the corrosivity of equipment；
3) the Nitrogen trifluoride market price is lower than fluorine gas, can reduce production cost.
4) segmentally heating is used, the free water in reactor can be removed, reduce the incidence of side reaction.
Detailed description of the invention
Fig. 1 is the process flow diagram of the invention that uranium is recycled by fluorization agent fluorination volatilization of Nitrogen trifluoride.
Fig. 2 is product UF in reactor in embodiment 16Infrared detection map.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
The selection of product specification.
In following embodiments, the technique of uranium is recycled according to process shown in FIG. 1 by fluorization agent fluorination volatilization of Nitrogen trifluoride
Implement.
The recycling of uranium in the molten salt system of the compound of 1 uranium-bearing of embodiment
(1) 3gUF will be contained4KF-ZrF4Total 100g, is placed in reactor, covers reactor cap, replaced with pure argon
Atmosphere in reactor.
(2) heating response device makes temperature, to after 200 DEG C, keep the temperature 2h by room temperature；At the end of heat preservation, set with pure argon
Change atmosphere in reactor.Gas piping is both heated to 100 DEG C；Using condensed in two stages device, condenser temperature is -60 DEG C.Continue
Heating response device makes temperature reach 700 DEG C；Heat preservation 3h is melted by mass flowmenter into reactor until fused salt melts completely
Mixed gas (the NF of Nitrogen trifluoride and argon gas is passed through in villiaumite3Volume fraction be 50%), flow 0.2L/min, using Fu
In leaf infrared spectrometer reactor outlet gas is detected.
(3) UF in 1h post-reactor exit gas6When concentration is lower than infrared detection lower limit, stop being passed through Nitrogen trifluoride at this time
With the mixed gas of argon gas, reaction terminates；Using flow velocity instead is the pure argon of 0.6L/min to reactor and blowing pipeline 30min.
Then system is vacuumized, so circulation is 6 times total.Reactor is opened, fused salt is taken out.
Effect data: through detecting, by the map in Fig. 2 it is known that the main component of product is UF6.It is melted after fluorination
Uranium content is 21ppm, UF in salt4Reactivity is 99.9%.Condenser containing product is weighed, and is calculated as follows
The rate of recovery to uranium is 93%.
Calculating formula:
The recycling of uranium in 2 green salt of embodiment
(1) by 50g UF4It is placed in reactor, covers reactor cap, with atmosphere in pure argon metathesis reactor.
(2) heating response device makes temperature, to after 250 DEG C, keep the temperature 3h by room temperature；It is replaced at the end of heat preservation with pure argon
Atmosphere in reactor.Gas piping is both heated to 100 DEG C；It uses adsorbent for the two-stage absorber recovery product of sodium fluoride, inhales
Adnexa temperature is 100 DEG C.Continue heating response device, temperature is made to reach 500 DEG C；2h is kept the temperature, by mass flowmenter to reactor
Inside it is passed through the mixed gas (NF of Nitrogen trifluoride and argon gas3Volume fraction be that 5%), flow 1L/min is red using Fourier
External spectrum instrument detects reactor outlet gas.
(3) UF in 2h post-reactor exit gas6When concentration is lower than infrared detection lower limit, stop being passed through Nitrogen trifluoride at this time
With the mixed gas of argon gas, reaction terminates, and using flow velocity instead is the pure argon of 0.6L/min to reactor and blowing pipeline 30min.
Then system is vacuumized, so circulation is 6 times total.
Effect data: reactor is opened without raw material remnants, UF4Reactivity is 100%.Absorber containing product is carried out
It weighs, and the rate of recovery for being calculated as follows to obtain uranium is 95%.
Calculating formula:
The recycling of uranium in the molten salt system of the compound of 3 uranium-bearing of embodiment
(1) 20gUF will be contained4NaF-ZrF4Total 1000g, is placed in reactor, covers reactor cap, use pure argon
Atmosphere in metathesis reactor.
(2) heating response device makes temperature, to after 250 DEG C, keep the temperature 3h by room temperature；It is replaced at the end of heat preservation with pure argon
Atmosphere in reactor；Gas piping is both heated to 100 DEG C；Using condensed in two stages, condenser temperature is respectively -40 DEG C and -70 DEG C.
Continue heating response device, temperature is made to reach 750 DEG C；Heat preservation for 24 hours, until fused salt melts completely, by mass flowmenter to reactor
Mixed gas (the NF of Nitrogen trifluoride and argon gas is passed through in middle melting villiaumite3Volume fraction be 10%), flow 2L/min is adopted
Reactor outlet gas is detected with Fourier infrared spectrograph.
(3) UF in 2h post-reactor exit gas6When concentration is lower than infrared detection lower limit, stop being passed through Nitrogen trifluoride at this time
With the mixed gas of argon gas, reaction terminates；Using flow velocity instead is the pure argon of 0.6L/min to reactor and blowing pipeline 30min.
Then system is vacuumized, so circulation is 6 times total.Reactor is opened, fused salt is taken out.
Effect data: through detecting, uranium content is 7ppm, UF in fused salt after fluorination4Reactivity is 99.9%.Product will be contained
Condenser weighed, and according to the calculating formula in embodiment 1 be calculated uranium the rate of recovery be 96%.
The recycling of uranium in 4 urania of embodiment
(1) 10g urania is placed in reactor, covers reactor cap, with atmosphere in pure argon metathesis reactor.
(2) heating response device makes temperature, to after 200 DEG C, keep the temperature 2h by room temperature；It is replaced at the end of heat preservation with pure argon
Atmosphere in reactor.Gas piping is both heated to 100 DEG C；It uses adsorbent for the two-stage absorber recovery product of sodium fluoride, inhales
Adnexa temperature is 100 DEG C.Continue heating response device, temperature is made to reach 600 DEG C；2h is kept the temperature, by mass flowmenter to reactor
Inside it is passed through the mixed gas (NF of Nitrogen trifluoride and argon gas3Volume fraction be 50%), flow 0.5L/min, using Fourier
Infrared spectrometer detects reactor outlet gas.
(3) UF in 2h post-reactor exit gas6When concentration is lower than infrared detection lower limit, stop being passed through Nitrogen trifluoride at this time
With the mixed gas of argon gas, reaction terminates, and using flow velocity instead is the pure argon of 0.6L/min to reactor and blowing pipeline 30min.
Then system is vacuumized, so circulation is 6 times total.
Effect data: reactor is opened without raw material remnants, UF4Reactivity is 100%.Absorber containing product is carried out
It weighs, and is 95% according to the rate of recovery that uranium is calculated in the calculating formula in embodiment 2.
The recycling of uranium in the molten salt system of the compound of 5 uranium-bearing of embodiment
(1) 5g UF will be contained4LiF-BeF4Total 500g, is placed in reactor, covers reactor cap, set with pure argon
Change atmosphere in reactor.
(2) heating response device makes temperature, to after 250 DEG C, keep the temperature 3h by room temperature；It is replaced at the end of heat preservation with pure argon
Atmosphere in reactor；Gas piping is both heated to 100 DEG C；Using condensed in two stages, condenser temperature is respectively -40 DEG C and -60 DEG C.
Continue heating response device, temperature is made to reach 700 DEG C；5h is kept the temperature, until fused salt melts completely, through mass flowmenter into reactor
Mixed gas (the NF of Nitrogen trifluoride and argon gas is passed through in melting villiaumite3Volume fraction be 20%), flow 1L/min, use
Fourier infrared spectrograph detects reactor outlet gas.
(3) UF in 1h post-reactor exit gas6When concentration is lower than infrared detection lower limit, stop being passed through Nitrogen trifluoride at this time
With the mixed gas of argon gas, reaction terminates；Using flow velocity instead is the pure argon of 0.6L/min to reactor and blowing pipeline 30min.
Then system is vacuumized, so circulation is 6 times total.Reactor is opened, fused salt is taken out.
Effect data: through detecting, uranium content is 20ppm, UF in fused salt after fluorination4Reactivity is 99.9%.Production will be contained
The condenser of object is weighed, and is 92% according to the rate of recovery that uranium is calculated in the calculating formula in embodiment 1.
Although specific embodiments of the present invention have been described above, it will be appreciated by those of skill in the art that these
It is merely illustrative of, protection scope of the present invention is defined by the appended claims.Those skilled in the art is not carrying on the back
Under the premise of from the principle and substance of the present invention, many changes and modifications may be made, but these are changed
Protection scope of the present invention is each fallen with modification.
Claims (10)
1. a kind of method for recycling uranium as fluorization agent fluorination volatilization using Nitrogen trifluoride, which is characterized in that the fluorination volatilization recycling
The method of uranium the following steps are included:
(1) air and water in reactor, the fused salt or uranium-bearing simple substance of compound of the reactor equipped with uranium-bearing are removed
The compound of mixture or one or more uranium；The content of uranium element is 0.01% in the fused salt of the compound of the uranium-bearing
~30%, the percentage is mass percent；The mixture of the uranium-bearing simple substance is uranium simple substance and fission products and/or gold
Belong to the mixture of alloy；
(2) reactor described in segmentally heating, first stage are heated to 200 DEG C~250 DEG C by room temperature, keep the temperature for the first time；Second-order
Section is heated to 500 DEG C~750 DEG C by the temperature at the end of the first stage；Second of heat preservation；It is passed through Nitrogen trifluoride and inertia
The mixed gas of gas, is reacted；Recycle reaction product；Three described in the mixed gas of the Nitrogen trifluoride and inert gas
Nitrogen fluoride volume fraction is 5%~50%.
2. the method for fluorination volatilization recycling uranium as described in claim 1, which is characterized in that the compound of the uranium is tetrafluoride
Any one in uranium, uranyl fluoride, orange oxide, triuranium octoxide and uranium dioxide；
And/or the compound fused salt of the uranium-bearing is mixture A or mixture B, the mixture A by fused salt and a kind of uranium
Compound composition, the mixture B are made of the compound of fused salt and two or more uranium；Preferably, the compound of the uranium is
Green salt or uranyl fluoride；
And/or fused salt described in the fused salt of the compound of the uranium-bearing is the co-melting salt of fluoride；
And/or the content of uranium element is 0.758%~2.27% in the fused salt of the compound of the uranium-bearing.
3. the method for fluorination volatilization recycling uranium as claimed in claim 2, which is characterized in that the co-melting salt of fluoride is KF-
ZrF4Co-melting salt, NaF-ZrF4Co-melting salt and LiF-BeF4Any one in co-melting salt；
The KF-ZrF4KF and ZrF in co-melting salt4Molar ratio be preferably 58:42；
The NaF-ZrF4NaF and ZrF in co-melting salt4Molar ratio be preferably 58:42；
The LiF-BeF2LiF and BeF in co-melting salt2Molar ratio be preferably 67:33.
4. the method for fluorination volatilization recycling uranium as described in claim 1, which is characterized in that remove the air in the reactor
Mode with water is the air and water removed in the reactor with inert gas.
5. the method for fluorination volatilization recycling uranium as described in claim 1, which is characterized in that the Nitrogen trifluoride and inert gas
Mixed gas described in the dosage of Nitrogen trifluoride be in stoichiometric ratio relative to the uranium element content in the reactor
It is excessive；
And/or the volume fraction of Nitrogen trifluoride described in the mixed gas of the Nitrogen trifluoride and inert gas be 10%~
50%, preferably 20%~50%；
And/or the ventilation flow rate of the mixed gas of the Nitrogen trifluoride and inert gas is 0.2L/min~2L/min, preferably
It is more preferably 0.5L/min~1L/min for 0.2L/min~1L/min.
6. the method for fluorination volatilization recycling uranium as described in claim 1, which is characterized in that during the segmentally heating,
The time of the first time heat preservation is 2h~3h；
And/or when the mixture of the compound of compound or a variety of uranium of the reactor equipped with uranium, second of heat preservation
Time be 2h~3h.
7. the method for fluorination volatilization recycling uranium as described in claim 1, which is characterized in that when the reactor contains equipped with described
When the fused salt of the compound of uranium, the time of second of heat preservation is that the fused salt of compound of the heat preservation to the uranium-bearing is completely molten
Melt；Preferably, the time of second heat preservation is 3h~for 24 hours.
8. the method for fluorination volatilization recycling uranium as described in claim 1, which is characterized in that the mode of the recycling reaction product
For condensation method；
The condensation method is condensed by using condenser；
Preferably, the condenser is multi-stage condensing device；
Preferably, the temperature of the condensation is -70 DEG C to -20 DEG C；
More preferably, the condenser is condensed in two stages device；
More preferably, the temperature of the condensation is respectively -40 DEG C and -60 DEG C.
9. the method for fluorination volatilization recycling uranium as described in claim 1, which is characterized in that the mode of the recycling reaction product
For absorption method；
The absorption method is adsorbed by using the absorber with adsorbent；
Preferably, the absorber is multi-stage absorption device；
Preferably, the temperature of the absorption is 80 DEG C to 150 DEG C；
Preferably, the adsorbent is sodium fluoride；
More preferably, the absorber is two-stage absorber；
The temperature of the more preferably described absorption is 100 DEG C.
10. the method for fluorination volatilization as described in claim 1 recycling uranium, which is characterized in that during the reaction, also into
The following operation of row: UF in the reaction product6When concentration is lower than Monitoring lower-cut, stop the reaction；
Preferably, stopping the reaction after the reaction carries out 1h~8h；
Preferably, the Monitoring lower-cut is 1ppm；
Preferably, stopping the reaction to realize by the mixed gas for stopping being passed through the Nitrogen trifluoride and inert gas；
Preferably, the mode for being passed through the mixed gas of the Nitrogen trifluoride and inert gas is continuously to be passed through；
Preferably, after stopping the reaction, using inert gas to the reactor and blowing pipeline；Then to described anti-
Device is answered to vacuumize, primary purging, which adds, once to be vacuumized as one cycle；The circulation is 4~8 times, preferably 6 times；
When purging, the flow velocity of the inert gas is 0.3L/min~0.8L/min, preferably 0.6L/min；
The time of the purging is 20min~50min, preferably 30min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111394741A (en) * | 2020-03-25 | 2020-07-10 | 哈尔滨工程大学 | Fluorinated U3O8Or UO3Method for dissolving in chloride molten salt |
| CN111413291A (en) * | 2020-04-09 | 2020-07-14 | 中国科学院上海应用物理研究所 | Infrared spectrum quantitative analysis method of gas fluoride |
| CN112939085A (en) * | 2019-12-10 | 2021-06-11 | 中核北方核燃料元件有限公司 | Method for preparing uranium tetrafluoride through dry fluorination |
| CN113620346A (en) * | 2021-07-20 | 2021-11-09 | 哈尔滨工程大学 | High-temperature fluorinated U3O8Or UO3Method for preparing uranium tetrafluoride |
| CN113881862A (en) * | 2021-09-08 | 2022-01-04 | 中国科学院上海应用物理研究所 | Method for separating uranium and neptunium by fluorination volatilization technology |
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| US11931763B2 (en) | 2019-11-08 | 2024-03-19 | Abilene Christian University | Identifying and quantifying components in a high-melting-point liquid |
| CN112939085A (en) * | 2019-12-10 | 2021-06-11 | 中核北方核燃料元件有限公司 | Method for preparing uranium tetrafluoride through dry fluorination |
| CN111394741A (en) * | 2020-03-25 | 2020-07-10 | 哈尔滨工程大学 | Fluorinated U3O8Or UO3Method for dissolving in chloride molten salt |
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| CN111413291A (en) * | 2020-04-09 | 2020-07-14 | 中国科学院上海应用物理研究所 | Infrared spectrum quantitative analysis method of gas fluoride |
| CN113620346A (en) * | 2021-07-20 | 2021-11-09 | 哈尔滨工程大学 | High-temperature fluorinated U3O8Or UO3Method for preparing uranium tetrafluoride |
| CN113881862A (en) * | 2021-09-08 | 2022-01-04 | 中国科学院上海应用物理研究所 | Method for separating uranium and neptunium by fluorination volatilization technology |
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