Ionic liquids as solvents

 

(57) Abstract:

The invention relates to the regeneration of irradiated fuel and dissolution of metal oxides. The result of the invention: the creation of a new means of getting any fuel. The metal is in an oxidation state lower than its maximum oxidation state. The ionic liquid reacts with the metal and oxidizes it to a higher oxidation state. Initially, the metal may be in the form of compounds. The metal is irradiated nuclear fuel, containing UO2and/or PuO2and the fission products. The ionic liquid is liquid at nitrate based, for example, pyridine or replaced imidazole nitrate. It contains the acid Bronsted or acid Franklin to increase the oxidising power of nitrate. Suitable acids are HNO3H2SO4and [NO+]. 17 C.p. f-crystals, 7 PL.

The invention relates to the reprocessing of irradiated fuel, as well as to a method of dissolving the oxides of metals in ionic liquids and to new products or compositions comprising ionic liquids.

Irradiated fuel may be a fuel, which is formed, for example, in the use of fuel ele the invention is not limited to this and can be applied for the regeneration of any particular type of irradiated fuel.

Irradiated fuel from LWRs is located inside Zircaloy shells, which are oxidized as a result of irradiation. In the known method for the reprocessing of irradiated fuel PUREX processes the first stage involves slashing and cutting of fuel rods, so that the irradiated fuel itself could be dissolved in nitric acid.

Known use as solvents, molten salts, and they can presumably be used for the reprocessing of irradiated fuel from LWRs. These molten salts, usually represent a mixture of salts that are liquid at high temperatures and have a slight advantage when used as solvents in front of aqueous or organic media.

Recently become famous salt, a mixture of salts or mixtures of components which form a salt, melting below or slightly above room temperature (as defined in this invention the salt is composed entirely of cations and anions). Such a fluid known as "ionic liquids, although this term may be used for salt, melting at relatively high temperatures, such as temperatures up to 100oC. General t the activity and a wide range of temperature being in the liquid state (for example, 300oC).

Known ionic liquids include aluminum chloride (III) in combination with halides of imidazole, pyridinium or phosphonium. Examples include 1-ethyl-3-methylimidazolium chloride, N-butylpyridinium chloride and tetrabutylphosphonium chloride. An example of a known ionic liquid system is a mixture of 1-ethyl-3-methylimidazolium chloride and aluminium chloride (III). E. S. Lane (J. Chem. Soc., 1953, 1172-1175) described for some alkylpyridine nitrate ionic liquids, including second-butylpyridinium nitrate. Information about the use of fluids not cited, however, references were made to the pharmacological activity of decametre-bis-pyridine nitrate.

L. Heerman et al. (J. Electroanal. Chem., 1985, 193, 289) describes the dissolution of UO3in the system, including N-butylpyridinium chloride and aluminium chloride (III).

In WO 96/32729 revealed that the oxide nuclear fuel can be dissolved in molten carbonates of alkali metals to form compounds that can be further processed to separate the uranium.

WO 95/21871, WO 95/21872 and WO 95/21806 relate to ionic liquids and their use in the catalysis of the conversion reactions of hydrocarbons (such as polymerization or oligomerization of alkyl)-3-(C6-C30alkyl)imidazole chlorides, and especially 1-methyl-3-WITH10alkylimidazole chloride or 1-hydrocarbonbearing halide, in which gidrolabilna group represents, for example, ethyl, butyl or other alkyl.

The present invention provides in its first aspect containing oxidant ionic liquid for dissolution of the metal is not necessarily in the form of its compounds. The oxidizing agent oxidizes the metal to a higher oxidation state at which the metal becomes generally more soluble in ionic liquids compared with the metal in its original oxidation state. In particular, is provided by way of the initial oxidation state. In particular, is provided by way of dissolution in ionic liquid metal in the initial oxidation state lower than its maximum oxidation state, the method characterized by the fact that the ionic liquid reacts with the metal and oxidizes it to a higher oxidation state.

When used in this description, the term "metal" includes not only the metal elements in the (0) oxidation state, but also metals in oxidation state above zero, associated with other ü compound of the metal, for example, the metal oxide.

This metal is uranium (in the form UO2) or plutonium (in the form of Rio2), or both, and, usually, the fission products. UO2or PuO2do not dissolve directly in the oxidizing ionic liquid, and the first oxide reacts with the ionic liquid with the formation of the oxidized product, which is soluble in the ionic liquid. Such preferred processes of dissolution can be used in the reprocessing of irradiated nuclear fuel.

Used ionic liquid may contain not only one anion and one cation, but in addition another component, the reinforcing ability of the liquid to react and oxidize the substrate. In the preferred implementation of the invention, the liquid contains as a mild oxidizing anion [NO3-] and acid, which can be acid Bronsted or Franklin, such as HNO3N2SO4or [NO+], for example, from [NO][BF4]. Acid makes the liquid more than capable of oxidation of substrates such as UO2and Rio2.

The ionic liquid includes a nitrate anion and organic cation, particularly nitrogen-containing heterocycles, including Quaternary nitrogen, such as, for example, PI is terpyridine nitrate, 1-butyl-3-methylimidazolium nitrate, 1-hexyl-3-methylimidazolium nitrate and 1-octyl-3-methylimidazolium nitrate.

The invention also includes the method for the reprocessing of irradiated fuel ionic liquid for dissolution of the fuel, as well as methods of regeneration, which include the stage of dissolution of the fuel in the ionic liquid.

The dissolution process is carried out at a temperature of from 50 to 100oC.

Solvent

The solvent includes the ionic liquid, which usually contains the agent or particles, giving the solvent ability to oxidize between other selected substrates, although the presence of this agent is not required if all aspects of the invention (as explained below in the section entitled "Metal"). The agent can be an oxidant dissolved in a non-oxidizing liquid or an additional agent for increasing oxidising power of other oxidizing particles. If the solvent contains nitrate ions, the agent increases the oxidizing capacity of the solvent in excess of that which should provide themselves nitrate ions; as described above, such agents include acid Bronsted and Franklin.

The solvent, in principle, may include any IO is one or more organic cations, especially nitrogen-containing heterocycles containing Quaternary nitrogen, in particular N-substituted, pyridine or N,N'-disubstituted of imidazole. The substituents are preferably hydrocarbide and, more preferably, alkali that, for example, can be branched. Gidrolabilna (e.g., alkyl) groups typically contain from 1 to 18 carbon atoms and more typically contain from 1 to 8 atoms.

Cation, thus, can be ion the disubstituted imidazole, in which the substituents have the formula CnH2n+1where 1 n 8, and are linear or branched. In the preferred disubstituted ions imidazole one Deputy has n=1, 2, or 3 (of which methyl is particularly preferred) and the other has n= 4, 5, 6, 7, or 8 (of which octyl, hexyl and, preferably, WITH4especially butyl, are preferred). Linear group is preferable. Alternative cation can be substituted pyridinium ion, in which the substituting group has the formula CnH2n+1where 1 n 8, and is linear or branched; suitable substituents are butyl, 2-(2-methyl)propyl, 2-butyl and octyl, however, linear alkali, especially butyl, are preferred.

From the above it can be concluded that ionic liquids can have nitrate based, for example, have nitrate as an anion. Ionic liquids containing nitrate, are new and are included in the invention except for some alkylpyridinium nitrates and polymethylene-bis-(pyridine nitrate)compounds, disclosed Lane. New also is the use of nitrosoureas ionic liquids as a reaction medium or solvent. The ionic liquid according to this invention includes nitrate and cation component, which is not only of alkylpyridine nitrate or polymethylene-bis-(pyridine nitrate). However, 1 butylpyridinium nitrate is particularly preferred ionic liquid, which is new and is also included in the invention. Products, including new ionic liquids, are the subject of this invention.

New ionic liquids on nitrate base can be obtained by mixing an aqueous silver nitrate (I) with an appropriate organic halide. As an example of one such liquid is obtained by mixing water solutions of silver nitrate (I) and 1-butyl-3-methylimidazolium chloride (bmim). Silver chloride precipitates and forms a liquid 1-butyl-3-m is TA.

1-Hexyl-3-methylimidazolium nitrate receive a similar way, and this product is liquid at room temperature.

Cations, alternative pyridinium and imidazolium include Quaternary postname cations, for example, Tetra(hydrocarbon)phosphonium. Suitable gidrolabilna group are the same as described above for pyridinium and imidazolium cations.

The agent for enhancing the oxidizing capacity of the ionic liquid (when used - section under the heading "Metal") is typically an acid Bronsted (e.g., HNO3or H2SO4or acid Franklin, for example, [NO+], is useful in one or the other case, in order to make the nitrate is more reactive to oxidation of these substrates as, for example, UO2and Rio2. In other words, one class of ionic liquids according to the invention contains an oxidant, including nitrate, and the substance that increase its action. Oxidant when mixed with the ionic liquid can react with it to form new particles, which are also ionic liquids. So, presumably, [NR] [F4] reacts with nitrate salts of organic cations, forming tetrafluoroborate>4],

where Bu-py represents a 1-butylpyridinium. [Bu-py][BF4] is novel and included in this invention. The result of the reaction is a three-component ionic liquid. The invention includes the use of other composite ionic liquids.

The reaction tetrafluoroborate (III) salts and ionic liquids leads to anhydrous tetrafluoroborate (III) product. Getting tetrafluoroborate salt (III) of this reaction is novel and included in this invention; such a method of obtaining finds particular application in the manufacture of organic tetrafluoroborate (III) salts, for example salts of imidazole, pyridinium and phosphonium.

Accordingly, the ionic liquid may include organic cations, as described above, and tetrafluoroborate (III) anions, for example, be tetrafluoroborate (III) salt of Quaternary nitrogen-containing heterocycle.

Metal

The nature of the metal is not limiting for the present invention. In the first aspect, the metal until dissolution is relatively low oxidation state and composition of the ionic liquid is oxidizing. Preferably, the metal until dissolution is in the condition in which it is less soluble in the ion is shining. The metal is usually in the form of oxide. Preferably, the metal oxides include various oxides of uranium and plutonium oxide (IV). So, experimentally it was found that UO2can react with the ionic liquid, which oxidizes the atoms of uranium (IV) to atoms of uranium (VI), for example, oxidizes the uranium oxide to TRANS-dioxolane (VI) in complex form. Similarly, the plutonium (IV), usually in the form of Rio2, can react with the ionic liquid, oxidizing the plutonium (IV) to PU (VI), for example, it oxidizes plutonium dioxide to TRANS-dioxolane (VI) in complex form.

In accordance with one way of carrying out the invention the metal oxide include oxides of plutonium and uranium, primarily in the form of irradiated nuclear fuel, for example, in the irradiated fuel rods. Nuclear fuel rods consist of fuel pellets contained in the shell, and in accordance with the invention is that the shell is removed when the oxidation of the ionic liquid. The shell usually is a zirconium alloy, for example, of the kind sold under the trademark Zircaloy. In another implementation of this invention, the ionic liquid can be used in order to dissolve its the metal fuel, for example, metallic uranium containing the fission products and actinides, and who begin to use or as a pure uranium metal, or an alloy of uranium and at least one other metal.

In some aspects the invention relates to ionic liquids that do not contain any acid or other amplifier oxidation. Thus, ionic liquids on nitrate-based without the addition of acid can be used as a reaction medium or solvent. For example, they can be used as the reaction medium for the oxidation of substances capable of oxidation by nitrate. Suitable oxide to be dissolved in such solvents nitrate basis may include the oxide of thorium (IV).

The invention is not limited to one path by which the metal is dissolved in the solvent of the ionic liquid. Typically, the dissolution is carried out at elevated temperatures in the 50oOr more, e.g. up to 350oC. Most preferably the use of elevated temperature from 50oWith up to 100oC. Metal usually dissolve when turbulent mixing.

The resulting solution may be subjected to further processing, for example, for selective udalenka uranium and plutonium; alternatively, a mixed oxide of uranium / plutonium can be separated from the other components of the solution. There is a method of electrodeposition can be used to extract from a solution of uranium and/or plutonium, while the fission products remain in the solution and the solution can then be subjected to pyrohydrolysis to make oxides ready for removal. To ensure a sustainable form of waste destined for removal, can be used in other chemical processes. An alternative method similar to the known PUREX processes-the process comprising solvent extraction, can be used after the initial dissolution of the fuel in the ionic liquid. In this way the fuel and, preferably, the shell is dissolved in the ionic liquid and spend several stages of extraction to remove the fission products from the ionic liquid system and to separate the uranium product from the plutonium product, ready for their subsequent reuse.

The invention preferably relates to the reprocessing of irradiated nuclear fuel. In one of the ways of the fuel rods are placed in the oxidizing ionic liquid, and a first shell, and then the uranium and plutonium dissolved in ion is m suitable way, after extraction of the ionic liquid. The first group of methods includes a step of mechanical destruction of the shell in order to expose the tablet of fuel to the action of ionic liquids. In accordance with another way of implementing the method of the fuel rods placed first in first ionic liquid for dissolution of the shell and then the second ionic liquid for dissolution of uranium and plutonium. Uranium and plutonium are usually in the form of their oxides.

The methods according to this invention, which relate to the recovery of nuclear fuel may include one or more stages for the conversion of dissolved fuel in the form of intermediate or end-product of nuclear fuel, for example, gel, powder, pellets, fuel rods or fuel assemblies.

The invention can be used for regeneration of any irradiated fuel, for example, LWRs, fast reactors and metal fuels. It can also be used for the production of purified nitrate dioxolane (VI) of uranium ore or uranium ore concentrate (yellowcake).

The invention is illustrated by the following examples.

Examples

The examples use the following abbreviations:
what I have.m.R.

s:singlet

d:doublet

t:triplet

quin:pentablet

sex:exaple

m:multiplet

br:broad

Example 1

Reagents

Solid UO2from the company BNFL. UO2(NO3)26N2O from BDH company and tetrafluoroborate (III) of nitronium ([NO][BF4]) from the firm Aldrich were used in the form in which they are supplied.

1-Mei is distilled under vacuum and stored under nitrogen atmosphere until use. Salts of 1-alkyl-3-imidazole or 1-alkylpyridine prepared by the direct reaction of a suitable alkylhalogenide or halogenoalkane with 1-methylimidazole or pyridine, respectively, and precrystallization from acetonitrile or ethyl acetate.

Spectra

UV - visible spectra are taken in a ditch, having a width of 1 mm and quartz Windows were used for comparison the corresponding net ionic liquid. Infrared spectra are taken in thin films using NaCl plates.

Receiving nitrate ionic liquids

All nitrate ionic liquids are prepared by analogy with the method, according to which receive 1-butyl-3-methylimidazolium nitrate.

1-Butyl-3-methylimidazolium chloride (8,04 g, 46,0 mmol) dissolved in water (15 cm3. The acetonitrile is removed under vacuum and the resulting slightly yellow product, which represents the ionic liquid is dried by heating in vacuum (approximately 50oWith 2-3 days). Some staining of the product appears as if the heat was too energetic. The obtained ionic liquid stored in a nitrogen atmosphere to prevent the ingress of moisture.

Range1N. I. m R. and microanalysis of ionic liquids on nitrate base, prepared in accordance with the described process are shown in table.1-6.

Example 2

Getting [NO][BF4] there is a green colour, which, however, disappears once the mixture is stirred for two days. In addition, there is a selection of brown gas. The infrared spectrum clearly shows the removal of water from ionic liquids with [NO][BF4].

Example 3

Getting [NO][BF4]:[Bu-py][NO3] in the ratio 1:2

Under stirring for 1 butylpyridinium nitrate (3,000 g, 15.1 mmol) was added nitrone tetrafluoroborate (III) (0.910 g, 7.8 mmol). Immediately appears brown smoke, and the solution quickly becomes a dark green-blue color. After stirring over night all [NO][BF4] dissolved with the formation of a green-blue solution, which is much less viscous than the starting material, 1-butylpyridinium nitrate (see table.7).

Example 4

The dissolution of UO2in a mixture of nitrate ionic liquid:nitric acid 1:1

Prepare a mixture of 1-butylpyridinium nitrate and concentrated nitric acid in a molar ratio of 1:1, which is removed on the rotary evaporator as much water. To 0.5 cm3this solution add UO2(approximately 0.01 g) and Bachleda 90oC, 6 hours), and at this time the solution becomes yellow with almost complete dissolution of UO2. UV - visible spectrum of the solution shows a strip with a fine structure having a center at =438 nm, which confirms the presence of the complex ion [UO2]+2.

Example 5

The dissolution of UO2[NO][BF4]:[Bu-py][NO3] 1:10.

UO2(0.02 g, 0,074 mmol) was added to a mixture of [NO][BF4]:[Bu-py][NO3] 1:10 (1,656 g). Stirring at room temperature does not change color mixture (pale yellow), so the mixture is heated (90oC, 5 hours). At this stage, most UO2already dissolved and the solution became more intense yellow color. At this stage add another portion UO2(0,101 g and 0.37 mmol) to the reaction mixture and continue heating (100oC, 48 hours). By the end of this time will remain a small amount of undissolved UO2but the solution has an intense yellow color. UV - visible spectrum shows a strip with a fine structure having a center at =436 nm, confirming the presence of the complex ion [UO2]+2. Collect the solid reaction residue and weigh it (0,018 g), which shows that only UO2the number 0,103 g (0.38 mmol) proreader the O2(0,059 g, 0.22 mmol) was added to a mixture of [NO][BF4]:[Bu-py][NO3] 1:2 (of 2.45 g) in a nitrogen atmosphere, to prevent any ingress of moisture. The mixture is heated (at approximately 65oC, 16 hours), after which the entire black UO2is dissolved and forms a yellow solution. Additionally added to the solution UO2(1,140 g, 0.52 mmol) and continue heating ( approximately 65oWith 44 hours). At the end of this time the solution becomes intensely yellow, but it nevertheless remains undissolved some indefinite quantity UO2. Again the UV - visible spectrum and infrared spectrum clearly confirm the presence of the complex ion [UO2]+2.

1. Method of dissolving in the solvent metal in the initial oxidation state lower than its maximum oxidation state, in accordance with which the solvent interacts with the metal and oxidizes it to a higher oxidation state, wherein the solvent is an ionic liquid containing an organic cation having a melting point of not more than 100oAnd the metal in its original oxidation state is a UO2or Rio2or their mixture.

2. Spookily, than the initial degree of oxidation.

3. The method according to p. 1-2, characterized in that the ionic liquid contains ions of nitrate.

4. The method according to p. 3, characterized in that the ionic liquid further comprises an acid.

5. The method according to p. 4, wherein the acid is an acid Bronsted or acid Franklin.

6. The method according to p. 5, wherein the acid is an NGO3N2SO4or [NO+] .

7. The method according to p. 6, characterized in that the ionic liquid containing [NO+] , is obtained by dissolving [NR] [F4] in the ionic liquid with the nitrate anions.

8. The method according to any of the preceding paragraphs, characterized in that the cations in ionic liquids represent a nitrogen-containing heterocycles having a Quaternary nitrogen atom.

9. The method according to p. 8, characterized in that the cations are N-substituted, pyridine or N, N1-disubstituted of imidazole.

10. The method according to p. 9, characterized in that the cations are (C1-C8alkyl)-pyridine or 1-(C4-C8alkyl)-3-methylimidazole.

11. The method according to any of the preceding paragraphs, characterized in that it prisa fact, what it is used for the reprocessing of irradiated fuel, and it involves the step of dissolving the fuel in the ionic liquid.

13. The method according to any of the preceding paragraphs, characterized in that the metal contained in the irradiated fuel and the method includes its regeneration by dissolution in ionic liquids, and irradiated fuel is oxidized.

14. The method according to p. 13, characterized in that the fuel is dissolved in the ionic liquid together with its sheath.

15. The method according to p. 13, characterized in that for the dissolution of shell use the first ionic liquid for dissolution of the fuel using the second ionic liquid.

16. The method according to any of the preceding paragraphs, characterized in that the dissolved uranium is extracted from the ionic liquid by using the liquid-liquid extraction or electrochemical method.

17. The method according to p. 15, characterized in that the stage of dissolution is carried out at a temperature of from 50 to 100oC.

18. The method according to p. 13, characterized in that it includes the process of converting the dissolved fuel product, which represents the nuclear fuel.

 

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EFFECT: simplified preparation technology and imparted hydrogen sulfide bacteria growth suppression.

4 tbl, 10 ex

Ionic liquids ii // 2272043

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3 ex

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2 ex

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