CN109913901B - Preparation method of metallic uranium - Google Patents
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Abstract
A preparation method of metallic uranium relates to the field of uranium preparation methods, in particular to the field of uranium preparation methods by using molten salt electrochemical technology. The specific technical scheme is as follows: heating U3O8 to remove water, mixing CCl4 gas with high-purity nitrogen, and introducing into a quartz tube at 400-460 ℃ for 2-6h to obtain UCl4; mixing the product A with LiCl and KCl mixed molten salt, electrifying for 1 to 20 hours at 673-873K with the current of 0.1A to 1A, and taking out the electrode of the crude metallic uranium or the U-Ga alloy; the material B is used as an anode, the molybdenum sheet is used as a cathode, and the high-purity uranium metal can be separated from the material B by electrolysis for 1-40h under the condition of 0.1A-1A. Each embodiment shows that the patent can greatly improve the speed and purity of the metal uranium precipitation, and has certain significance for nuclear energy construction in China.
Description
Technical Field
The invention relates to the field of a method for preparing uranium, in particular to the field of a method for preparing uranium by applying molten salt electrochemical technology.
Background
In the prior art, U is adopted when metal uranium is prepared by electrolysis 3 O 8 Direct electrolysis, which is time-consuming, low in productivity, and generates a large amount of chlorine gas and waste molten salt, korean institute of atomic energy Cui Enyu et al in LiCl-Li 2 Attempts to supply U in O fused salt 3 O 8 The product is obtained after electrolysis is carried out for more than 40 hours at high temperature, and meanwhile, the constant potential electrolysis method adopted by the product can decompose a large amount of molten salt to generate a byproduct chlorine gas, so that the experiment is seriously influenced.
Zhang Yu et al in the national institutes of defense and technology and technical bureau of China uses triuranium octoxide as a sheet electrode for reaction, and directly performs electrolytic theoretical analysis and intermediate product analysis in LiCl molten salt at 650 ℃, but is not finally directly proved by metal uranium.
Although the prior art can electrolyze metallic uranium, there are a plurality of problems to be solved:
direct U of the prior art 3 O 8 The electrolysis time is too long, and the reason is difficult to solve: u (U) 3 O 8 The solubility is too low, and the electrolyte can be deposited at the bottom of molten salt and cannot fully contact with current, so that the electrolysis efficiency is reduced, and the ionic bond energy is very large, so that the electrolyte has the electrolysis difficulty.
The above problems are difficult to solve by using the prior art, and the specific reasons are as follows:
the prior art cannot quickly and efficiently obtain the metal uranium, because of U 3 O 8 The solubility is too low, the electrolyte can be deposited at the bottom of molten salt and cannot fully contact with current, so that the electrolysis efficiency is reduced, and the ionic bond energy is very large, so that the electrolyte has the electrolysis difficulty;
uranium metal has great demands in the fields of energy, military industry, medical treatment and the like, the impurity content in the metal uranium has important influence on corrosion resistance, mechanical property, long-term storage property and the like, and the rapid acquisition of high-purity metal uranium has certain significance for nuclear energy construction in China.
Disclosure of Invention
To above-mentioned problem, this patent proposes following solution thinking: UCl is prepared firstly 4 Powder, and then UCl is added again 4 And (3) electrolyzing the powder to obtain an intermediate product, and finally adopting technologies such as electrochemical directional separation and the like to obtain the high-purity uranium metal.
1) In the first step of chlorination, the high-purity carbon tetrachloride obtained through vacuum reflux is placed in a flask, heated to a boiling point in a water bath kettle to generate carbon tetrachloride gas, high-purity nitrogen is introduced at the same time to control the flow rate of the carbon tetrachloride so as to control the reaction quantity, and certain time is introduced to chlorinate the triuranium octoxide to obtain high-purity uranium tetrachloride.
2) Second step of electrolysis, UCl 4 The solubility is higher, and the easily soluble ionic compound can be rapidly obtained to prepare metallic uranium or U-Ga alloy under the condition of constant current electrolysis.
3) And thirdly, separating by utilizing technologies such as directional crystallization separation, crystallization separation by utilizing a temperature gradient and the like, and obtaining the uranium metal with high purity.
The solution idea is completed through the following technical scheme, and the method for preparing uranium by applying the molten salt electrolysis technology comprises the following steps:
a method for preparing uranium by applying molten salt electrolysis technology, comprising the following steps:
step 1:5g to 20g of triuranium octoxide are put into a tube furnace, high-purity nitrogen is introduced for 30 to 300min, the triuranium octoxide is heated at 100 ℃ for 1 hour, and then the triuranium octoxide is heated at 250 ℃ for 1 hour; regulating the temperature of the water bath kettle to 85 ℃, heating carbon tetrachloride in the flask, mixing carbon tetrachloride gas with high-purity nitrogen, and controlling the flow rate of the mixed gas to be 3cm 3 Introducing mixed gas into a quartz tube, heating the quartz tube to 400-460 ℃ for 2-6 hours, immediately opening a tube furnace for cooling after the reaction is finished, and taking out a porcelain boat to obtain a powdery product A (A is uranium tetrachloride);
step 2: placing 4g to 12g of powdery product A at the bottom of a crucible, pouring 100 g to 300g of LiCl and KCl mixed molten salt with the mass content of 99% -99.99%, wherein the mass ratio of LiCl to KCl is 1:1, taking a silver/silver chloride reference electrode as a reference electrode, taking a spectrum pure graphite rod as an auxiliary electrode, taking molybdenum sheets or liquid gallium as a working electrode, jointly assembling into a three-electrode system, well installing and placing the three-electrode system into a LiCl-KCl molten body, controlling the temperature to be 673K to 873K, setting the current to be 0.1A to 1A, electrifying for 1 to 40 hours, carrying out the operation in a container under the protection of nitrogen, and then taking out the cooled electrode to take out a material B (B is a metal uranium crude product or an electrode of U-Ga alloy);
step 3: and (3) taking the material B as an anode, taking a molybdenum sheet with the same size of 2cm and the thickness of 0.2cm as a cathode, and electrolyzing for 1 to 40 hours under the condition of 0.1A-1A to obtain refined metal uranium, wherein high-purity uranium metal can be separated from the material B.
Description of the techniques
Description 1: in the first step of chlorination, the specific temperature of the patent is 100 ℃ for heating to remove the moisture of reactants, and if the requirement is not met, various byproducts are generated, so that the final low-purity metal uranium is obtained; heating at a specific temperature of 250 ℃ is to remove bound water in reactants, the effect can be achieved only at the specific temperature, uranium hydroxide and high-valence uranium oxide can be generated when the temperature is too high, the electrolysis time is increased, chlorination is carried out at the specific temperature of 400-460 ℃, and an intermediate product uranium tetrachloride with the purity of 99.3% can be obtained only at the specific temperature.
Description 2: in the second step alone, the conventional idea is to directly give electrons to uranium ions in high-temperature molten salt by using an electrochemical method, so that the uranium ions are directly electrochemically reduced into metallic uranium simple substances. The new idea of the patent in the second step is to solve the loss caused by high temperature and the inefficiency of single electrolyte effect under the specific current value, namely 0.1A, and gradually reduce metal when electrons are introduced, so that the obtained product is more uniform and the time is shorter.
Description 3: this patent is loaded with the triuranium octoxide of specific quality in porcelain boat and is carried out the chlorination, because porcelain boat bears too much reactant, is unfavorable for carrying out the reaction with carbon tetrachloride gas, and too thick reactant can lead to the productivity of upper and lower floor's product to cause differently.
Description 4: the patent must specifically introduce inert gas, such as high-purity nitrogen, for 30-300min at a flow rate of 3cm 3 The method is characterized in that the method is used in chloridizing-electrolyzing-refining, because the reaction concentration of carbon tetrachloride is determined by controlling the flow rate of nitrogen, however, the carbon tetrachloride gas is cooled when contacting with high-purity inert gas, so that condensation reflux is caused, the experiment adopts a three-neck flask, and the left end is filled with high-purity nitrogenHeating the mixture in a container, and then mixing the other end of the mixture with carbon tetrachloride which becomes gas and then introducing the mixture into a reaction container; when in electrolysis, the flow rate of inert gas is controlled within a certain range, too much can reduce the temperature in the electrolytic tank, and too little can not ensure the removal of impurity gas and the maintenance of inert atmosphere.
Description 5: this specific tail gas of this patent is collected and detects liquid and is concentrated sulfuric acid, if adopt inorganic aqueous solution, vapor can get into quartz tube and reactant and take place side reaction, so get rid of, if adopt the organic matter, volatility is stronger, can take place side reaction equally or decompose under the high temperature and cause the influence, so concentrated sulfuric acid is adopted here, because it has hydroscopicity and oily difficult volatilizing, whether have the strong reducibility also can detect through the change of colour and have the passage of carbon tetrachloride gas, still have as gas velocity of flow detection and tail gas collection device's basic function.
Description 6: this patent is specific to adopt liquid gallium as the negative pole to carry out the electrolysis, and the effect is increase area of contact when the electrolysis, prevents the influence of external atmosphere in to the fused salt, can be accelerated to obtain the alloy, and the alloy can obtain simple substance metal fast through the high temperature refining that follows.
Description 7: u is specifically adopted in this patent 3 O 8 As a raw material, free metallic uranium is not present in nature because of its very active chemical nature, and is always present in a combined state. Uranium minerals 170 are known in more than one but only 20-30 of them of industrial exploitation value, the most important of which are asphaltic uranium minerals (mainly composed of triuranium octoxide). The method has the advantages that the source of raw materials is wide, the preparation process is simple and direct, meanwhile, the uranium oxide is the most stable, uranium trioxide can not be gradually oxidized to generate under the chlorination condition, wherein the oxidation condition of the uranium trioxide is 200-500 ℃, namely the chlorination temperature in the process, and the bad influence can be overcome in the method.
Description 8: UCl is specifically adopted in the patent 4 As an electrolyte in the intermediate process, uranium chloride (UCl) 4 /UCl 3 ) Is weaker and is easy to form U in molten salt 4+ And Cl - Is easier to be reduced in the electrolytic process, eliminates UCl 3 Unstable in air, thus UCl 4 Are more suitable as electrolytic substances in this patent. For converting triuranium octoxide into uranium tetrachloride, chloride ions must be present in the reactant, and according to other experimental results, pure chlorine gas can be used to obtain uranium tetrachloride, however, the yield is reduced, and considering that oxygen ions exist in triuranium octoxide, nonmetallic elements such as H, C, S, P, N are required to be found to combine with oxygen ions to generate gas, and then discharged, wherein water formed by H and O oxidizes low-valent uranium, S, N and P generate flammable and highly toxic gas with H, and if a hydrochlorination agent is adopted, nitric acid and sulfuric acid can be generated to dissolve reactant triuranium octoxide, so that the reactant is reduced; in other studies, many have been chlorinated with metal chlorides, however, metal impurities are introduced, and if carbon tetrachloride reactants containing only C and Cl are used as in this patent, high yields are most desirable.
Description 9: the patent adopts inert nitrogen gas of specific velocity to mix into carbon tetrachloride gas, only reduces the loss of the product and improves the yield after carbon tetrachloride gas contacts with high-purity nitrogen. The reasons for the loss are from the instrument and the method, the instrument is special in structure, and the chlorine source is supplemented in a dropwise adding mode, so that the local chlorine concentration in the internal contact reaction space is overlarge, high-price and volatile substances such as uranium pentachloride and the like are generated, and the substances are solidified on the tube wall, so that the loss is caused. The reason for the volatile substances is that the concentration of chloride ions is too great or that a reaction for producing chlorine gas occurs. However, they encounter new problems with this mixture, causing further losses, since it is mixed with 8% -26% chloroform added dropwise in carbon tetrachloride, which reacts with uranium oxychloride, oxidizing the lower uranium to higher uranium, which has a great impact on the yield of the chlorination process.
Description 10: the specific carbon tetrachloride is adopted as the chlorinating agent, the yield is higher than that of the chloroform-carbon tetrachloride mixed gas adopted in other articles due to the adoption of single carbon tetrachloride gas, the adopted chloroform can reduce the byproduct chlorine, so that the generation of volatile byproducts is indirectly reduced, however, the chloroform in the carbon tetrachloride and chloroform mixed liquid adopted in other technologies is sensitive to light and is easy to decompose, other impurities are generated, and can be uniformly mixed, the boiling point of the chloroform is 61-62 ℃, the chloroform can be changed into gas earlier in the process of dropping liquid at high temperature, the reaction can be carried out with reactant octauranium oxide in advance, the combination of hydrogen and oxygen is caused, the inhibition of the reaction by the generation of side reaction product water is not eliminated, the stability of the chloroform is poor, and if the chlorination temperature is higher than 450 ℃, the thermal decomposition can be carried out to form carbon tetrachloride, and the reaction is a side reaction for the chlorination reaction. Not only can the toxicity of chloroform be strong, but also the chloroform can be decomposed into extremely toxic gas, and the chloroform can cause great harm to human bodies. Therefore, the yield of the method adopts carbon tetrachloride as a reactant to chlorinate the triuranium octoxide, and can exceed the yield of the mixed gas of carbon tetrachloride and chloroform adopted in other articles. In the carbon tetrachloride introducing process, high-purity nitrogen is introduced at the same time, so that the concentration of introduced carbon tetrachloride gas is diluted, and chloride ions with low concentration can fully react with reactants, thereby avoiding uranium pentachloride or having little influence on the patent.
The beneficial effects are that:
1. specifically, carbon tetrachloride with fixed concentration is used as a chlorinating agent, the ionic bond energy of uranium oxide is weakened, metal is precipitated more rapidly during constant current electrolysis, the metal uranium electrolysis precipitation time is greatly reduced, and compared with other technologies, metal uranium can be electrolyzed out after more than 40 hours, the metal uranium can be obtained after 17.5 hours, the U-Ga alloy can be obtained after 1 hour, and then other means are used for separation, refining and purification.
2 specifically adopts the rectification reflux method to purify the carbon tetrachloride, and the gas flow speed and the temperature time during chlorination are jointly determined to obtain the UCl with higher purity of 99.3 percent 4 The powder reduces the introduction of impurities and improves the purity of the finally electrolyzed metallic uranium.
Drawings
FIG. 1 example 1 electrolytic melting of LiCl-KCl-UCl 4 And the cathode potential is related to time. Electrolysis temperature 773K, electrolysis time 17.5 h, electrolysis current 0.1A.
FIG. 2 example 2 LiCl-KCl-UCl 4 XRD pattern after electrolysis. Electrolysis temperature 873K, electrolysis time 14 h, electrolysis current 0.2A.
FIG. 3 LiCl-KCl-UCl in example 3 4 Fused salt on molybdenum wire electrode (s=0.26 cm) 2 ) Cyclic voltammogram, temperature 873K, scan rate 0.10V s −1 。
FIG. 4 example 4 the chlorination process of the present patent chlorinates U 3 O 8 Conversion to UCl 4 XRD analysis pattern of (c).
FIG. 5 example 5 melting LiCl-KCl-UCl 4 XRD pattern after electrolysis. Electrolysis time 2 h, electrolysis current 1A.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
Example 1
The preparation method of the metal uranium comprises the following steps:
step 1:5g to 20g of triuranium octoxide are put into a tube furnace, high-purity nitrogen is introduced for 30 to 300min, the triuranium octoxide is heated at 100 ℃ for 1 hour, and then the triuranium octoxide is heated at 250 ℃ for 1 hour; regulating the temperature of the water bath kettle to 85 ℃, heating carbon tetrachloride in the flask, mixing carbon tetrachloride gas with high-purity nitrogen, and controlling the flow rate of the mixed gas to be 3cm 3 Introducing mixed gas into a quartz tube, heating the quartz tube to 400-460 ℃ for 2-6 hours, immediately opening a tube furnace for cooling after the reaction is finished, and taking out a porcelain boat to obtain a powdery product A (A is uranium tetrachloride);
step 2: placing 4g to 12g of powdery product A at the bottom of a crucible, pouring 100 g to 300g of LiCl and KCl mixed molten salt with the mass content of 99% -99.99%, taking a silver/silver chloride reference electrode as a reference electrode, taking a spectrum pure graphite rod as an auxiliary electrode, taking molybdenum sheets or liquid gallium as a working electrode, assembling the three electrodes together into a three-electrode system, placing the three-electrode system into a LiCl-KCl molten body, controlling the temperature to be 673K to 873K, setting the current to be 0.1A to 1A, electrifying for 1 to 40 hours, carrying out the operation in a container under the protection of nitrogen, and then taking out the cooled electrode to take out a material B (B is an electrode of a metal uranium crude product or U-Ga alloy);
step 3: and (3) taking the material B as an anode, taking a molybdenum sheet with the same size of 2cm and the thickness of 0.2cm as a cathode, and electrolyzing for 1 to 40 hours under the condition of 0.1A-1A to obtain refined metal uranium, wherein high-purity uranium metal can be separated from the material B.
Example 2
The preparation method of the metal uranium is basically the same as that of the embodiment 1, except that in the step 2, a spectrally pure graphite rod is used as an auxiliary electrode, and a molybdenum sheet is used as a working electrode to realize the electrolysis temperature of 873K; in the step 3, molybdenum sheets with the size of 2cm and the thickness of 0.2cm are used as cathodes, and electrolysis is carried out for 1-40 hours under the condition of 0.1A-1A.
Example 3
A method for preparing metallic uranium is basically the same as that of example 1, except that in step 2, the electrolysis temperature is 873K.
Technical description: by adjusting the temperature parameters, additional heat is provided, which results in an electrolysis reaction time of less than 17.05 hours.
Example 4
A method for preparing metallic uranium, the present example being substantially the same as example 1, except that: in step 1, the chlorination time was adjusted to 4 hours and the chlorination temperature was adjusted to 440 degrees celsius.
Technical description: by adjusting the reduction of the time parameter to 1 hour and the temperature to 713K, UCl with purity of 99.48% can be obtained 4 And (3) powder.
Example 5
A method for preparing metallic uranium, the present example being substantially the same as example 1, except that: in step 2, an electrolytic treatment is carried out under a current of 1A for 2 hours.
Technical description: the cathodic potential was extended to 1A after 2 hours to give a metal product.
Claims (5)
1. The preparation method of the metal uranium comprises the following steps:
step 1:5g to 20g of triuranium octoxide are put into a tube furnace, high-purity nitrogen is introduced for 30 to 300min, the triuranium octoxide is heated at 100 ℃ for 1 hour, and then the triuranium octoxide is heated at 250 ℃ for 1 hour; regulating the temperature of the water bath kettle to 85 ℃, heating carbon tetrachloride in the flask, mixing carbon tetrachloride gas with high-purity nitrogen, and controlling the flow rate of the mixed gas to be 3cm 3 Introducing mixed gas into a quartz tube, heating the quartz tube to 400-460 ℃ for 2-6 hours, immediately opening a tube furnace for cooling after the reaction is finished, and taking out a porcelain boat to obtain a powdery product A;
step 2: placing 4g to 12g of powdery product A at the bottom of a crucible, pouring 100 g to 300g of LiCl and KCl mixed molten salt with the mass content of 99% -99.99%, wherein the mass ratio of LiCl to KCl is 1:1, taking a silver/silver chloride reference electrode as a reference electrode, taking a spectrum pure graphite rod as an auxiliary electrode, taking molybdenum sheets or liquid gallium as a working electrode, assembling the mixture into a three-electrode system, placing the three-electrode system into a LiCl-KCl melt, controlling the temperature to be 673K to 873K, setting the current to be 0.1A to 1A, electrifying for 1 to 40 hours, carrying out the operation in a container under the protection of nitrogen, and then taking out the cooled electrode to take out a material B;
step 3: and (3) taking the material B as an anode, taking a molybdenum sheet with the same size of 2cm and the thickness of 0.2cm as a cathode, and electrolyzing for 1 to 40 hours under the condition of 0.1A-1A to obtain refined metal uranium, wherein high-purity uranium metal can be separated from the material B.
2. The method for preparing metallic uranium according to claim 1, wherein in step 2, a spectrally pure graphite rod is used as an auxiliary electrode, and a molybdenum sheet is used as a working electrode to achieve an electrolysis temperature of 873K; in the step 3, molybdenum sheets with the size of 2cm and the thickness of 0.2cm are used as cathodes, and electrolysis is carried out for 1-40 hours under the condition of 0.1A-1A.
3. A method of producing metallic uranium according to claim 1, wherein in step 2 the electrolysis temperature is 873K.
4. A process for the preparation of metallic uranium according to claim 1, characterised in that in step 1 the chlorination time is set to 4 hours and the chlorination temperature is set to 440 ℃.
5. A process for the preparation of metallic uranium according to claim 1, characterised in that in step 2, an electrolytic treatment is carried out, the treatment conditions being maintained at a current of 1A for 2 hours.
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| CN111155136B (en) * | 2019-12-23 | 2022-03-18 | 哈尔滨工程大学 | Fused salt electrolysis U3O8Direct preparation of UO2Apparatus and method of |
| CN111394741B (en) * | 2020-03-25 | 2022-04-05 | 哈尔滨工程大学 | Fluorinated U3O8Or UO3Method for dissolving in chloride molten salt |
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| US2772142A (en) * | 1944-04-21 | 1956-11-27 | Cummings Ross | Process of reclaiming uranium from solutions |
| US5164050A (en) * | 1989-07-06 | 1992-11-17 | Compagnie Europeenne Du Zirconium Cezus | Method of obtaining uranium from oxide using a chloride process |
| CA2107921A1 (en) * | 1992-10-07 | 1995-04-15 | Geoffrey Horrocks Bailey | Method and apparatus for the production of uranium |
| US5421855A (en) * | 1993-05-27 | 1995-06-06 | The United States Of America As Represented By The United States Department Of Energy | Process for continuous production of metallic uranium and uranium alloys |
| CN104562089A (en) * | 2014-10-17 | 2015-04-29 | 中国原子能科学研究院 | Method for preparing initial molten salt system in molten salt electrolysis dry after-treatment process |
| CN107779615A (en) * | 2017-08-28 | 2018-03-09 | 中国工程物理研究院材料研究所 | A kind of uranium-bearing low-temperature molten salt system, its preparation method and application |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2772142A (en) * | 1944-04-21 | 1956-11-27 | Cummings Ross | Process of reclaiming uranium from solutions |
| US5164050A (en) * | 1989-07-06 | 1992-11-17 | Compagnie Europeenne Du Zirconium Cezus | Method of obtaining uranium from oxide using a chloride process |
| CA2107921A1 (en) * | 1992-10-07 | 1995-04-15 | Geoffrey Horrocks Bailey | Method and apparatus for the production of uranium |
| US5421855A (en) * | 1993-05-27 | 1995-06-06 | The United States Of America As Represented By The United States Department Of Energy | Process for continuous production of metallic uranium and uranium alloys |
| CN104562089A (en) * | 2014-10-17 | 2015-04-29 | 中国原子能科学研究院 | Method for preparing initial molten salt system in molten salt electrolysis dry after-treatment process |
| CN107779615A (en) * | 2017-08-28 | 2018-03-09 | 中国工程物理研究院材料研究所 | A kind of uranium-bearing low-temperature molten salt system, its preparation method and application |
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