CN110144598A - A kind of preparation method and applications of uranium trichloride - Google Patents
A kind of preparation method and applications of uranium trichloride Download PDFInfo
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- CN110144598A CN110144598A CN201910516998.3A CN201910516998A CN110144598A CN 110144598 A CN110144598 A CN 110144598A CN 201910516998 A CN201910516998 A CN 201910516998A CN 110144598 A CN110144598 A CN 110144598A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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Abstract
The present invention provides a kind of preparation method and applications of uranium trichloride, using uranium or uranium alloy as anode, apply voltage between the anode and cathode, it is electrolysed in 100~300 DEG C of molten chloride, uranium is melted in anode, and uranium trichloride precipitating, filtering are formed in anode region, purifying obtains uranium trichloride.Method proposed by the present invention solves the problems such as uranium trichloride preparation is complicated, at high cost.Direct in-situ produces uranium trichloride in molten salt system, and raw material is easy to get, and does not use strong corrosive gas, whole process is easy to operate, and reaction condition is mild, practical.
Description
Technical field
The present invention relates to nuclear technology fields, and in particular to a kind of preparation method and applications of uranium trichloride.
Background technique
Dry method post-processing technology has a clear superiority for the following advanced nuclear fuel cycle, at present most promising dry method
Post-processing technology is fused-salt electrolytic refining technology.The technology mainly using chloride fuse salt as medium, is adopted under the high temperature conditions
Electrochemically the actinides in spentnuclear fuel is recycled, while realizing the separation with fission product.With radiation resistance, low face
The advantages that boundary's risk, radioactive waste are few.And as important nuclear industry product, uranium trichloride have in dry method post-processing to
Close important role.During electrorefining, in order to maintain the stability of decomposition voltage, need to be added in the electrolyte a large amount of
Uranium trichloride (about 10wt%).The method that tradition prepares uranium trichloride is with high costs, and complicated for operation, seriously corroded.Preparation
The common method of uranium trichloride is usually relatively complex, such as: it is reacted at high temperature using metallic uranium with chlorine and generates uranium tetrachloride,
Then hydrogen reducing is used again；Can also with hydrogen be reacted with metallic uranium generation uranium hydride, then again with hydrogen chloride gas precursor reactant system
It is standby to obtain uranium trichloride.But preparation step is more, and needs to use the raw materials such as toxic chlorine and hydrogen chloride, can corrode and set
It is standby, pollute environment.Furthermore metal chloride such as CdCl also can be used2Preparation is reacted with metallic uranium in high-temperature molten salt medium,
But it can make to contain impurity in product, later separation is complicated, at high cost, it is difficult to isolated pure uranium trichloride.
Summary of the invention
It is in view of the deficiencies in the prior art and insufficient, the present invention provides a kind of preparation method of uranium trichloride and its
Using.
It is an object of that present invention to provide a kind of preparation methods of uranium trichloride, using uranium or uranium alloy as anode, in chlorination
It is electrolysed in aluminium molten salt system, the aluminium chloride molten salt system is AlCl3- NaCl fused salt, AlCl3- LiCl fused salt, AlCl3- KCl is molten
Salt or NaAlCl4-LiAlCl4-KAlCl4Fused salt.This invention simplifies the methods for preparing uranium trichloride, since uranium trichloride is in chlorine
Change and do not melted in aluminium molten salt system, uranium trichloride can be generated in anode region direct in-situ, and in a manner of precipitating and electrolysis
Liquid separates, and can efficiently prepare pure uranium trichloride, and recycle the uranium in uranium alloy, and have operation temperature
Low, corrosivity is small, easy to operate, low for equipment requirements, advantage at low cost.It therefore, can be in aluminium chloride molten salt system more
Simply, more environmentally friendly, more economical prepares pure uranium trichloride.
Some preferred embodiments according to the present invention, the AlCl3AlCl in-NaCl fused salt3It is with NaCl molar ratio
30:70~63:37；
The AlCl3AlCl in-LiCl fused salt3It is 30:70~63:37 with LiCl molar ratio；
The AlCl3AlCl in-KCl fused salt3It is 30:70~63:37 with KCl molar ratio；
The NaAlCl4-LiAlCl4-KAlCl4Fused salt group becomes any molar ratio；
Preferably, the AlCl3The molar ratio of sodium chloride and aluminium chloride is 1:1~1:1.5 in-NaCl fused salt；
The AlCl3The molar ratio of lithium chloride and aluminium chloride is 1:1~1:1.5 in-LiCl fused salt；
The AlCl3The molar ratio of potassium chloride and aluminium chloride is 1:1~1:1.5 in-KCl fused salt；
The NaAlCl4-LiAlCl4-KAlCl4Fused salt becomes 50:30:20 with molar ratio group.
Some preferred embodiments according to the present invention, the aluminium chloride molten salt system temperature are 100~300 DEG C；It is preferred that
, the AlCl3- NaCl temperature of molten salt is 150-170 DEG C；The AlCl3- LiCl temperature of molten salt is 160 DEG C；The AlCl3-
KCl temperature of molten salt is 170 DEG C；The NaAlCl4-LiAlCl4-KAlCl4Temperature of molten salt is 140 DEG C.
Some preferred embodiments according to the present invention, the anode are pure uranium, U-Al alloy, U-Mo Alloy, the conjunction of uranium silicon
Gold or uranium zircaloy；And/or cathode is aluminium, molybdenum, tungsten, copper, nickel or chromium.
Some preferred embodiments according to the present invention, applying voltage between the anode and cathode is 0.2~3.0V, excellent
It is selected as 1.5~2.5V.
Some preferred embodiments according to the present invention, uranium are melted in anode, and form uranium trichloride precipitating in anode region,
Filtering, purifying obtain uranium trichloride；Preferably, the filtering uses metal mesh filter or decantation；And/or the purifying is
It is evaporated in vacuo at 400~500 DEG C.
Some preferred embodiments according to the present invention, the metal mesh are made of metal screen, it is preferred that the metal
Strainer is metal molybdenum strainer, platinum strainer, tungsten strainer or stainless steel filtering net；And/or the mesh of the metal screen is
200~2000 mesh.
Some preferred embodiments according to the present invention, electrolysis carry out under the conditions of anhydrous and oxygen-free；And/or in protection gas
It is carried out under body, it is preferred that the protective gas is selected from one of argon gas, nitrogen and helium or a variety of.
Some preferred embodiments according to the present invention comprising the steps of:
1) molten chloride of chloride containing aluminium is placed in crucible and is heated to 100~300 DEG C of preferably 140~180 DEG C of temperature,
Make its fusing；
2) two electrode systems are electrolysed: under the conditions of anhydrous and oxygen-free, using uranium or uranium alloy as anode；With aluminium, molybdenum, tungsten, copper,
Nickel or chromium apply 0.2~3V preferably tank voltage of 1.5~2.5V, react 1~10 hour, obtain three in anode region as cathode
Uranium chloride precipitating；Alternatively, three-electrode system is electrolysed: under the conditions of anhydrous and oxygen-free, using uranium or uranium alloy as anode, being done with aluminium bar
Reference electrode, using aluminium, molybdenum, tungsten, copper, nickel or chromium as cathode, control working electrode potential in 0.2~2V preferably 0.5~1.5V,
Reaction 1~10 hour obtains uranium trichloride precipitating in anode region；
3) crucible bottom precipitating is obtained by the metal mesh filter of the yellow-green precipitate in crucible or using decantation,
It is evaporated in vacuo at 400~500 DEG C, obtains uranium trichloride.
Second object of the present invention is the separation or system proposed according to the above-mentioned method for preparing uranium trichloride in uranium alloy
It is applied in standby nuclear industry product.
Beneficial effects of the present invention at least that: the present invention propose uranium trichloride preparation method, solve uranium trichloride
Preparation is complicated, problem at high cost, seriously polluted, and realizes the efficient synthesis rate of uranium trichloride by control reaction condition.
The method of the present invention can be directly realized by uranium and be cooperateed in anode region with electrochemical dissolution and chemical precipitation in aluminium chloride molten salt system
Mode prepare uranium trichloride, and anodic dissolution processes only need to control decomposition voltage, and deposited components are single, are easy to mention
It is pure.Other impurities are not introduced, do not use strong corrosive gas, whole process is easy to operate, reaction condition is mild, equipment requirement
It is low, good economy performance, practical.Method of the invention simultaneously controls the dissolution speed in anode of uranium by changing decomposition voltage
Rate can efficiently produce uranium trichloride precipitating, be evaporated in vacuo after filtering, obtain sterling, simple and practical, and prepare tri-chlorination
Uranium it is low in cost.It is of great significance, has a good application prospect for nuclear industry field.
Detailed description of the invention
Fig. 1 is the schematic diagram of 1 electrolytic preparation uranium trichloride of the embodiment of the present invention.
Fig. 2 is that unsegregated uranium trichloride precipitates schematic diagram after the embodiment of the present invention 1 is electrolysed.
Fig. 3 is that obtained uranium trichloride product schematic diagram is evaporated in vacuo in the embodiment of the present invention 1.
Fig. 4 is the XRD characterization figure for the product uranium trichloride that the embodiment of the present invention 1 obtains.
Specific embodiment
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where spirit of that invention and essence, to modifications or substitutions made by the method for the present invention, step or condition, the present invention is belonged to
Range.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art,
Electrochemistry experiment carries out on Autolab PGSTAT302N in embodiment, controls data using the Nova software package of Metrohm
Acquisition and electro-chemical test, products obtained therefrom are measured characterization with X-ray diffractometer (Bruker, D8Advance).Embodiment
In, reagent is commercially available conventional raw material, is purchased from Mike woods company.The preparation of 1 molten salt system of embodiment, firstly, reagent is transferred to
(water and oxygen content are less than 1ppm) saves in glove box.High-pure anhydrous NaCl and AlCl are configured according to molar ratio 1:13(purity
It is all larger than 99.5%), after mixing, is placed in corundum crucible, be warming up to 240 DEG C.It is outstanding with the molybdenum net filtration removal of 1000 mesh
Floating impurity to get.LiCl and AlCl3, KCl and AlCl3And NaAlCl4-LiAlCl4-KAlCl4Preparation method it is identical.
Embodiment 1
By 100g AlCl3- NaCl salt (AlCl3It is 1:1 with NaCl molar ratio) it is placed in alumina crucible, controlled at
170℃；Fig. 1 is electrolysed schematic diagram for it, and high pure metal uranium bar makees anode (purity is not less than 99.9%), and aluminium wire makees cathode (purity
Not less than 99.999%).Control tank voltage is 2.0V, is electrolysed 2h, and Faradaic current probably maintains 0.4A or so.After electrolysis
(electrodeposit is as shown in Figure 2: illustrating that uranium trichloride is easy to separate with electrolyte), with the metal molybdenum strainer mistake of 1000 mesh
Filter obtains yellow-green precipitate.It will be deposited at 500 DEG C and 1h is evaporated in vacuo, obtaining 3.35g atropurpureus solid, (i.e. uranium trichloride produces
Product, as shown in Figure 3), Fig. 4 is that its XRD characterization is uranium trichloride as the result is shown, illustrates to be prepared by this method pure
Uranium trichloride.The rate of recovery that this method prepares uranium trichloride is 98%.
Embodiment 2
The present embodiment provides a kind of method for preparing uranium trichloride, the difference with embodiment 1 is only that: by 100g
AlCl3- NaCl salt is changed to 100g NaAlCl4-LiAlCl4-KAlCl4(molar ratio group becomes 50:30:20), electrolysis temperature is
140℃.The rate of recovery that this method prepares uranium trichloride is 97%.
Embodiment 3
The present embodiment provides a kind of method for preparing uranium trichloride, the difference with embodiment 1 is only that: uranium anode is changed to
U-Al alloy anode.It was found that Faradaic current is bigger, it is greater than 1.0A.The rate of recovery that this method prepares uranium trichloride is 92%.
Comparative example 1
Uranium is considered to be worth doing and reacts generation uranium hydride with hydrogen, then will by the method that this comparative example prepares uranium trichloride using tradition
Uranium trichloride is made in uranium hydride and hydrogen chloride gas precursor reactant, reacts as follows:
This method needs to use the clast of uranium, and hydrogen is inconvenient, and hydrogen chloride gas used has very strong thorn
Swash property and corrosivity.
Comparative example 2
This comparative example is implemented using a kind of (CN107779615) uranium-bearing low-temperature molten salt system, preparation method and in applying
The method of example 1: in 400 DEG C of LiCl-KCl fused salt, oxidant is made with zinc chloride, according to equation 3ZnCl2+ 2U=3Zn+
2UCl3, a certain amount of zinc chloride and excessive metallic uranium is added, the fuse salt of the uranium trichloride containing 10wt% can be prepared.Control
Temperature processed is 450 DEG C；The fuse salt of the uranium trichloride containing 20wt% can be prepared.Controlled at 500 DEG C, it can prepare and contain
The fuse salt of 30wt% uranium trichloride.But impurity can be brought into using such oxidant, later separation is complicated, it is difficult to isolated
Pure uranium trichloride.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of uranium trichloride, which is characterized in that using uranium or uranium alloy as anode, in aluminium chloride molten salt system
Middle electrolysis, the aluminium chloride molten salt system are AlCl3- NaCl fused salt, AlCl3- LiCl fused salt, AlCl3- KCl fused salt or
NaAlCl4-LiAlCl4-KAlCl4Fused salt.
2. the method according to claim 1, wherein the AlCl3AlCl in-NaCl fused salt3With NaCl molar ratio
For 30:70~63:37；
The AlCl3AlCl in-LiCl fused salt3It is 30:70~63:37 with LiCl molar ratio；
The AlCl3AlCl in-KCl fused salt3It is 30:70~63:37 with KCl molar ratio；
The NaAlCl4-LiAlCl4-KAlCl4Fused salt group becomes any molar ratio；
Preferably, the AlCl3The molar ratio of sodium chloride and aluminium chloride is 1:1~1:1.5 in-NaCl fused salt；
The AlCl3The molar ratio of lithium chloride and aluminium chloride is 1:1~1:1.5 in-LiCl fused salt；
The AlCl3The molar ratio of potassium chloride and aluminium chloride is 1:1~1:1.5 in-KCl fused salt；
The NaAlCl4-LiAlCl4-KAlCl4Fused salt becomes 50:30:20 with molar ratio group.
3. according to the method described in claim 2, it is characterized in that, the aluminium chloride molten salt system temperature is 100~300 DEG C；
Preferably, the AlCl3- NaCl temperature of molten salt is 150-170 DEG C；The AlCl3- LiCl temperature of molten salt is 160 DEG C；It is described
AlCl3- KCl temperature of molten salt is 170 DEG C；The NaAlCl4-LiAlCl4-KAlCl4Temperature of molten salt is 140 DEG C.
4. the method according to claim 1, wherein the anode is pure uranium, U-Al alloy, U-Mo Alloy, uranium
Silicon alloy or uranium zircaloy；And/or cathode is aluminium, molybdenum, tungsten, copper, nickel or chromium.
5. the method according to claim 1, wherein between the anode and cathode apply voltage be 0.2~
3.0V, preferably 1.5~2.5V.
6. method according to any one of claims 1-5, which is characterized in that uranium is melted in anode, and in anode region shape
It precipitates, filters at uranium trichloride, purifying obtains uranium trichloride；Preferably, the filtering uses metal mesh filter or decantation；
And/or the purifying is to be evaporated in vacuo at 400~500 DEG C.
7. according to the method described in claim 6, it is characterized in that, the metal mesh is made of metal screen, it is preferred that described
Metal screen is metal molybdenum strainer, platinum strainer, tungsten strainer or stainless steel filtering net；And/or the mesh of the metal screen
For 200~2000 mesh.
8. method according to any one of claims 1-7, which is characterized in that electrolysis carries out under the conditions of anhydrous and oxygen-free；
And/or carry out under a shielding gas, it is preferred that the protective gas is selected from one of argon gas, nitrogen and helium or a variety of.
9. method according to claim 1 to 8, which is characterized in that comprise the steps of:
1) molten chloride of chloride containing aluminium is placed in crucible and is heated to 100~300 DEG C of preferably 140~180 DEG C of temperature, make it
Fusing；
2) two electrode systems are electrolysed: under the conditions of anhydrous and oxygen-free, using uranium or uranium alloy as anode；With aluminium, molybdenum, tungsten, copper, nickel or
Chromium applies 0.2~3V preferably tank voltage of 1.5~2.5V, reacts 1~10 hour, obtain tri-chlorination in anode region as cathode
Uranium precipitating；Alternatively, three-electrode system is electrolysed: under the conditions of anhydrous and oxygen-free, using uranium or uranium alloy as anode, doing reference with aluminium bar
Electrode, using aluminium, molybdenum, tungsten, copper, nickel or chromium as cathode, control working electrode potential is in 0.2~2V preferably 0.5~1.5V, reaction
1~10 hour, uranium trichloride precipitating was obtained in anode region；
3) crucible bottom precipitating is obtained by the metal mesh filter of the yellow-green precipitate in crucible or using decantation, 400~
It is evaporated in vacuo at 500 DEG C, obtains uranium trichloride.
10. method according to claim 1 to 9 is applied in the separation of uranium alloy or preparation nuclear industry product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041512A (en) * | 2019-12-25 | 2020-04-21 | 中国科学院高能物理研究所 | Preparation method of variable-valence metal low-valence halide |
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| CN111041512A (en) * | 2019-12-25 | 2020-04-21 | 中国科学院高能物理研究所 | Preparation method of variable-valence metal low-valence halide |
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