CN118060316A - Method for preparing apatite-based molten salt waste solidified body through hydrothermal method - Google Patents
Method for preparing apatite-based molten salt waste solidified body through hydrothermal method Download PDFInfo
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- CN118060316A CN118060316A CN202410399256.8A CN202410399256A CN118060316A CN 118060316 A CN118060316 A CN 118060316A CN 202410399256 A CN202410399256 A CN 202410399256A CN 118060316 A CN118060316 A CN 118060316A
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- Prior art keywords
- salt waste
- molten salt
- solidified body
- apatite
- telescopic rod
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- 239000002699 waste material Substances 0.000 title claims abstract description 62
- 150000003839 salts Chemical class 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910052586 apatite Inorganic materials 0.000 title claims abstract description 19
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 title claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 26
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000002955 isolation Methods 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 abstract description 12
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 6
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001424 calcium ion Inorganic materials 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 4
- 238000005342 ion exchange Methods 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 4
- 229910021645 metal ion Inorganic materials 0.000 abstract description 4
- 238000012856 packing Methods 0.000 abstract description 4
- 238000007711 solidification Methods 0.000 abstract description 4
- 230000008023 solidification Effects 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 238000006467 substitution reaction Methods 0.000 abstract description 4
- 229910019142 PO4 Inorganic materials 0.000 description 7
- 239000011575 calcium Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 4
- 150000001669 calcium Chemical class 0.000 description 3
- 229910052585 phosphate mineral Inorganic materials 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- HCQWRNRRURULEY-UHFFFAOYSA-L lithium;potassium;dichloride Chemical compound [Li+].[Cl-].[Cl-].[K+] HCQWRNRRURULEY-UHFFFAOYSA-L 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000005025 nuclear technology Methods 0.000 description 1
- -1 phosphate Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The application discloses a method for preparing an apatite-based fused salt waste solidified body by using hydrothermal method, which comprises the following steps: s1, uniformly mixing molten salt waste and hydroxyapatite powder to obtain a mixture; s2, placing the mixture into a heating device for hydrothermal reaction to synthesize a fused salt waste solidified body. The hydroxyapatite has good adsorption capacity, acid-base regulation, ion exchange capacity and thermal stability. Since the hydroxyl and calcium ions can be replaced by chloride and various metal ions, respectively, the fused salt waste is immobilized by the hydroxyapatite, and the waste ions are introduced into the crystal lattice through substitution reaction, i.e. the effective solidification of the fused salt waste can be realized by the hydroxyapatite. The obtained fused salt waste solidified body has the advantages of large packing capacity, good chemical stability and the like, and can effectively inhibit the pollution of fused salt waste to the ecological environment. The method has higher use value and development potential.
Description
Technical Field
The invention relates to the field of molten salt waste treatment, in particular to a method for preparing an apatite-based molten salt waste solidified body by using hydrothermal method.
Background
With the continuous development of nuclear technology, fused salt reactors have attracted wide attention due to the advantages of good neutron performance, inherent safety, online aftertreatment, sustainable development, nuclear diffusion prevention and the like. During operation of the reactor, significant amounts of radioactive waste from fission may accumulate in the lithium chloride-potassium chloride melting medium, forming molten salt waste. In addition, a large amount of molten salt waste is generated in the process of recovering fuel and noble metal by the conventional reactor spent fuel electrorefining. The fused salt waste has the characteristics of strong radioactivity, long half-life, strong diffusion capacity, high toxicity and the like, and forms a potential threat to human health and living environment.
The molten salt waste is treated by two ways, namely, a proper matrix is selected for inclusion treatment, and the conventional silicate glass has low compatibility with chloride and cannot be directly used for solidifying the waste molten salt; and secondly, firstly converting the chloride into other compounds such as phosphate, oxide and the like, and then performing curing treatment. The use of the converted method certainly creates more procedures that are difficult to meet with the long-term disposal of molten salt waste.
Disclosure of Invention
The invention aims at the problems and provides a method for preparing an apatite-based fused salt waste solidified body by hydrothermal method.
The technical scheme adopted by the invention is as follows:
a method for hydrothermally preparing an apatite-based molten salt waste solidified body, comprising the steps of:
s1, uniformly mixing molten salt waste and hydroxyapatite powder to obtain a mixture;
S2, placing the mixture into a heating device for hydrothermal reaction to synthesize a fused salt waste solidified body.
Apatite is a class of calcium-containing phosphate minerals, which is generally called Ca 5(PO4)3 (F, cl, OH) as a chemical component, wherein, the hydroxyapatite Ca 5(PO4)3(OH)2 has good adsorption capacity, acid-base regulation, ion exchange capacity and thermal stability. Since the hydroxyl and calcium ions can be replaced by chloride and various metal ions, respectively, the fused salt waste is immobilized by the hydroxyapatite, and the waste ions are introduced into the crystal lattice through substitution reaction, i.e. the effective solidification of the fused salt waste can be realized by the hydroxyapatite. The obtained fused salt waste solidified body has the advantages of large packing capacity, good chemical stability and the like, and can effectively inhibit the pollution of fused salt waste to the ecological environment. The method has higher use value and development potential.
In one embodiment of the present invention, in the step S1, the molten salt waste and the hydroxyapatite powder are performed in a liquid environment, and the molten salt waste and the hydroxyapatite powder are stirred on a magnetic stirrer for a set time by using water as a medium.
In an embodiment of the present invention, the set time is 30min.
In one embodiment of the present invention, the method further includes step S3: and naturally cooling the molten salt waste solidified body.
In one embodiment of the invention, the mass ratio of the molten salt waste to the hydroxyapatite powder is 1 (10-15).
In one embodiment of the present invention, in the step S2, the temperature of the heating device is 100 ℃ to 200 ℃.
In an embodiment of the invention, in the step S2, the time for maintaining the heating device is 3h to 96h.
In one embodiment of the present invention, the magnetic stirrer includes:
the rotating base can generate a magnetic field which continuously rotates;
a container for placement on the swivel base;
the magnetic rotating piece is arranged at the bottom of the container, and the rotating base can drive the magnetic rotating piece to rotate when working so as to stir the mixture in the container;
The first telescopic element is positioned right above the container and provided with a first telescopic rod, and the end part of the first telescopic rod is provided with a magnet;
The isolation cover is sleeved at the end part of the first telescopic rod in a sliding manner, the isolation cover is provided with a conical body, the lower end of the body is small, the upper end of the body is large, a conical groove is formed in the lower end face of the isolation cover, and the magnetic rotary piece can be at least partially embedded into the conical groove;
The second telescopic element is fixed on the first telescopic rod and is provided with a second telescopic rod, the second telescopic rod is connected with the upper end of the isolation cover, and the second telescopic element can drive the isolation cover to move up and down relative to the first telescopic rod, so that the bottom surface of the isolation cover is close to or far away from a magnet at the end part of the first telescopic rod.
The lower extreme of body is little, the upper end is big, combines the design of conical tank, and when the cage left the mixture, a large amount of mixtures can drop into the container fast.
Magnetic stirrers are effective in reducing the amount of stirring device in contact with the mixture relative to conventional paddles, but require the mixture to be transferred after mixing is complete, in which case the magnetic rotating member is removed from the vessel. According to the application, the first telescopic element, the second telescopic element, the isolation cover and the magnet are arranged, so that the magnetic parts can be automatically taken out and put into the container.
A working process of placing magnetic stirring equipment into a magnetic rotating piece:
in the initial state, the second telescopic element is retracted, the bottom surface of the isolation cover is close to the magnet at the end part of the first telescopic rod, and the magnet can firmly adsorb the magnetic rotating piece in the conical groove though the isolation cover;
The first telescopic element works to drive the isolation cover and the second telescopic element to synchronously move downwards for a set distance;
After the first telescopic element moves downwards, the second telescopic element works to drive the movable isolation cover to move downwards relative to the first telescopic rod, so that the bottom surface of the isolation cover is far away from the magnet at the end part of the first telescopic rod, and the magnetic rotating piece can automatically fall into the container from the conical groove.
The mixture is not easy to be separated out by the way of putting in, and the mixture cannot enter the inside of the isolation cover because of the isolation cover.
A process for the magnetic stirring device to remove a magnetic rotating member from a container:
the first telescopic element works to drive the isolation cover and the second telescopic element to synchronously move downwards to the bottom of the container;
the magnetic rotator can be attracted to the tapered slot by a magnet, preferably a powerful magnet, which moves up with the first telescopic element.
This way of extraction, because of the presence of the cage, the mixture does not enter the inside of the cage.
In an embodiment of the invention, the first telescopic element is located on the electric push rod, and the second telescopic element is located on the cylinder or the electric push rod.
The beneficial effects of the invention are as follows: apatite is a class of calcium-containing phosphate minerals, which is generally called Ca 5(PO4)3 (F, cl, OH) as a chemical component, wherein, the hydroxyapatite Ca 5(PO4)3(OH)2 has good adsorption capacity, acid-base regulation, ion exchange capacity and thermal stability. Since the hydroxyl and calcium ions can be replaced by chloride and various metal ions, respectively, the fused salt waste is immobilized by the hydroxyapatite, and the waste ions are introduced into the crystal lattice through substitution reaction, i.e. the effective solidification of the fused salt waste can be realized by the hydroxyapatite. The obtained fused salt waste solidified body has the advantages of large packing capacity, good chemical stability and the like, and can effectively inhibit the pollution of fused salt waste to the ecological environment. The method has higher use value and development potential.
Drawings
FIG. 1 is a schematic diagram of a magnetic stirrer;
FIG. 2 is an exploded view of a magnetic stirrer;
Fig. 3 is a cross-sectional view of the cage.
The reference numerals in the drawings are as follows:
1. A rotating base; 2. a container; 3. a magnetic rotating member; 4. a first telescopic element; 41. a first telescopic rod; 5. an isolation cover; 51. a body; 511. a conical groove; 6. a second telescopic element; 61. and a second telescopic rod.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. It will be apparent that the described embodiments are some, but not all, embodiments of the application. The components of the embodiments of the present application generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
In the description of the present application, it should be noted that, the azimuth or positional relationship indicated by the terms "inner", "outer", etc. are based on the azimuth or positional relationship shown in the drawings, or the azimuth or positional relationship that is commonly put in use of the product of this application, are merely for convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element to be referred to must have a specific azimuth, be configured and operated in a specific azimuth, and therefore should not be construed as limiting the present application. Furthermore, the terms "first," "second," and the like, are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
In the description of the present application, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed", "connected" and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected or integrally connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present application will be understood in specific cases by those of ordinary skill in the art.
The present invention will be described in detail with reference to the accompanying drawings.
A method for hydrothermally preparing an apatite-based molten salt waste solidified body, comprising the steps of:
S1, weighing LiCl-KCl-NdCl simulated molten salt waste with the mass ratio of 1:1:1;
Uniformly mixing molten salt waste and hydroxyapatite powder to obtain a mixture; the mass ratio of the fused salt waste to the hydroxyapatite powder is 1:10.
S2, putting the mixture into a heating device for hydrothermal reaction, wherein the temperature of the heating device is 180 ℃, and the heating time is 24 hours, so as to synthesize a molten salt waste solidified body;
s3: and naturally cooling the molten salt waste solidified body.
Apatite is a class of calcium-containing phosphate minerals, which is generally called Ca 5(PO4)3 (F, cl, OH) as a chemical component, wherein, the hydroxyapatite Ca 5(PO4)3(OH)2 has good adsorption capacity, acid-base regulation, ion exchange capacity and thermal stability. Since the hydroxyl and calcium ions can be replaced by chloride and various metal ions, respectively, the fused salt waste is immobilized by the hydroxyapatite, and the waste ions are introduced into the crystal lattice through substitution reaction, i.e. the effective solidification of the fused salt waste can be realized by the hydroxyapatite. The obtained fused salt waste solidified body has the advantages of large packing capacity, good chemical stability and the like, and can effectively inhibit the pollution of fused salt waste to the ecological environment. The method has higher use value and development potential.
In this example, in step S1, molten salt waste and hydroxyapatite powder are carried out in a liquid environment, with water as a medium, and stirred on a magnetic stirrer for 30min.
As shown in fig. 1,2 and 3, in the present embodiment, the magnetic stirrer includes:
A rotating base 1 capable of generating a magnetic field that rotates continuously;
A container 2 for placement on the swivel base 1;
the magnetic rotating piece 3 is arranged at the bottom of the container 2, and the rotating base 1 can drive the magnetic rotating piece 3 to rotate when working so as to stir the mixture in the container 2;
The first telescopic element 4 is positioned right above the container 2 and provided with a first telescopic rod 41, and the end part of the first telescopic rod 41 is provided with a magnet;
the shielding cover 5 is sleeved at the end part of the first telescopic rod 41 in a sliding manner, the shielding cover 5 is provided with a conical body 51, the lower end of the body 51 is small, the upper end of the body 51 is large, a conical groove 511 is formed in the lower end face of the shielding cover 5, and the magnetic attraction rotating piece can be at least partially embedded into the conical groove 511;
The second telescopic element 6 is fixed on the first telescopic rod 41, the second telescopic element 6 is provided with a second telescopic rod 61, the second telescopic rod 61 is connected with the upper end of the isolation cover 5, and the second telescopic element 6 can drive the isolation cover 5 to move up and down relative to the first telescopic rod 41, so that the bottom surface of the isolation cover 5 is close to or far away from a magnet at the end part of the first telescopic rod 41.
The lower end of the body 51 is small and the upper end is large, and in combination with the design of the tapered slot 511, a large amount of the mixture can quickly fall into the container 2 when the shield 5 leaves the mixture.
The magnetic stirrer is effective in reducing the contact of the stirring device with the mixture relative to conventional paddles, but the mixture needs to be transferred after mixing is completed, at which time the magnetic rotating member 3 needs to be removed from the container 2. The application can realize better automatic taking-out and putting-in of the magnetic parts into the container 2 by arranging the first telescopic element 4, the second telescopic element 6, the isolating cover 5 and the magnet.
A working process of the magnetic stirring device into the magnetic rotating member 3:
in the initial state, the second telescopic element 6 is retracted, the bottom surface of the isolation cover 5 is close to the magnet at the end part of the first telescopic rod 41, and the magnet can firmly adsorb the magnetic rotating member 3 in the conical groove 511 though the isolation cover 5 is arranged;
the first telescopic element 4 works to drive the isolation cover 5 and the second telescopic element 6 to synchronously move downwards for a set distance;
After the first telescopic element 4 moves downwards, the second telescopic element 6 works to drive the movable isolation cover 5 to move downwards relative to the first telescopic rod 41, so that the bottom surface of the isolation cover 5 is far away from the magnet at the end part of the first telescopic rod 41, and at the moment, the magnetic rotating piece 3 can automatically fall into the container 2 from the conical groove 511.
This way of placement does not easily allow the mixture to come out of the way and because of the presence of the cage 5, the mixture does not enter the interior of the cage 5.
A process of the magnetic stirring device for removing the magnetic rotating member 3 from the container 2:
the first telescopic element 4 works to drive the isolation cover 5 and the second telescopic element 6 to synchronously move down to the bottom of the container 2;
The magnetic rotator 3 can be attracted to the tapered slot 511 by a magnet (preferably a powerful magnet) and the magnetic rotator 3 moves up together as the first telescopic element 4 moves up.
This way of extraction, because of the presence of the screen 5, the mixture does not enter the interior of the screen 5.
In this embodiment, the first telescopic element is a 4-position electric putter, and the second telescopic element is a 6-position cylinder or electric putter.
The foregoing description is only of the preferred embodiments of the present invention, and is not intended to limit the scope of the invention, but rather is intended to cover all equivalent structures as modifications within the scope of the invention, either directly or indirectly, as may be contemplated by the present invention.
Claims (9)
1. A method for hydrothermally preparing an apatite-based molten salt waste solidified body, comprising the steps of:
s1, uniformly mixing molten salt waste and hydroxyapatite powder to obtain a mixture;
S2, placing the mixture into a heating device for hydrothermal reaction to synthesize a fused salt waste solidified body.
2. The method for preparing an apatite-based molten salt waste solidified body according to claim 1, wherein in the step S1, molten salt waste and hydroxyapatite powder are performed in a liquid environment, and water is used as a medium, and the mixture is stirred on a magnetic stirrer for a set time.
3. The method for hydrothermally preparing an apatite-based molten salt waste solidified body according to claim 2, wherein the set time is 30min.
4. The method for the hydrothermal preparation of an apatite-based molten salt waste solidified body according to claim 1, further comprising step S3: and naturally cooling the molten salt waste solidified body.
5. The method for preparing an apatite-based molten salt waste solidified body according to claim 1, wherein the mass ratio of the molten salt waste to the hydroxyapatite powder is 1 (10-15).
6. The method for producing an apatite-based molten salt waste solidified body according to claim 1, wherein in the step S2, the temperature of the heating device is 100 ℃ to 200 ℃.
7. The method for preparing an apatite-based molten salt waste solidified body according to claim 1, wherein the heating device is maintained for 3-96 hours in the step S2.
8. The method of hydrothermally preparing an apatite-based molten salt waste solidified body according to claim 2, wherein the magnetic stirrer includes:
the rotating base can generate a magnetic field which continuously rotates;
a container for placement on the swivel base;
the magnetic rotating piece is arranged at the bottom of the container, and the rotating base can drive the magnetic rotating piece to rotate when working so as to stir the mixture in the container;
The first telescopic element is positioned right above the container and provided with a first telescopic rod, and the end part of the first telescopic rod is provided with a magnet;
The isolation cover is sleeved at the end part of the first telescopic rod in a sliding manner, the isolation cover is provided with a conical body, the lower end of the body is small, the upper end of the body is large, a conical groove is formed in the lower end face of the isolation cover, and the magnetic rotary piece can be at least partially embedded into the conical groove;
The second telescopic element is fixed on the first telescopic rod and is provided with a second telescopic rod, the second telescopic rod is connected with the upper end of the isolation cover, and the second telescopic element can drive the isolation cover to move up and down relative to the first telescopic rod, so that the bottom surface of the isolation cover is close to or far away from a magnet at the end part of the first telescopic rod.
9. The method of hydrothermally preparing an apatite-based molten salt waste solidified body according to claim 8, wherein the first telescopic member is located at an electric putter, and the second telescopic member is located at a cylinder or an electric putter.
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