WO1993013374A1 - Process and device for drying/spraying a product - Google Patents

Process and device for drying/spraying a product Download PDF

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Publication number
WO1993013374A1
WO1993013374A1 PCT/FR1992/001227 FR9201227W WO9313374A1 WO 1993013374 A1 WO1993013374 A1 WO 1993013374A1 FR 9201227 W FR9201227 W FR 9201227W WO 9313374 A1 WO9313374 A1 WO 9313374A1
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WO
WIPO (PCT)
Prior art keywords
waveguide
solution
suspension
product
injected
Prior art date
Application number
PCT/FR1992/001227
Other languages
French (fr)
Inventor
Bruno Aubert
Original Assignee
Societe Generale Pour Les Techniques Nouvelles S.G.N.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Societe Generale Pour Les Techniques Nouvelles S.G.N. filed Critical Societe Generale Pour Les Techniques Nouvelles S.G.N.
Priority to EP93902369A priority Critical patent/EP0617783A1/en
Priority to JP5511491A priority patent/JPH07506526A/en
Publication of WO1993013374A1 publication Critical patent/WO1993013374A1/en

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/32—Drying solid materials or objects by processes involving the application of heat by development of heat within the materials or objects to be dried, e.g. by fermentation or other microbiological action
    • F26B3/34—Drying solid materials or objects by processes involving the application of heat by development of heat within the materials or objects to be dried, e.g. by fermentation or other microbiological action by using electrical effects
    • F26B3/347—Electromagnetic heating, e.g. induction heating or heating using microwave energy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B01D1/18—Evaporating by spraying to obtain dry solids
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/10—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour carrying the materials or objects to be dried with it
    • F26B3/12—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour carrying the materials or objects to be dried with it in the form of a spray, i.e. sprayed or dispersed emulsions or suspensions

Definitions

  • the present invention relates to a method of drying / atomizing a product in solution or in suspension in a liquid. It also relates to a device for implementing said method.
  • the process of the invention makes it possible to dry quickly, homogeneously, in a very small volume and without generating pollution.
  • 11 is based on the direct use of the energy of microwave radiation.
  • microwaves can be used, the frequency of which is between 800 and 30,000 MHz.
  • drying / atomization processes are commonly used, in particular for drying aqueous suspensions of minerals, fruit extracts, pharmaceutical products.
  • the product - in solution or in suspension in a liquid generally water - is sprayed into a large chamber, within which a current of hot air is maintained, intended to remove the liquid from the droplets, in a very short time (of the order of 0.5 to 2 s).
  • the energy efficiency of this type of drying can be good with a wide range of heat treatment; it is poor if it is desired to obtain dry residues which are uniformly treated and of centered particle size.
  • the product in a thin layer on a carpet, can be dried continuously, by passing said carpet through a waveguide or under a slotted guide.
  • a slotted guide is described in particular in patent FR 1 488292.
  • the product can also be dried batchwise, in small quantities in a single-mode guide or in larger quantities by stirring said product or the waves.
  • REPLACEMENT SHEET Microwave energy has also been used to raise the temperature of a liquid; said liquid circulating in a tube which crosses a monomodaL waveguide
  • an original use of microwave energy is currently proposed to obtain, in powder form, a product initially in solution or in suspension in a liquid.
  • Said product is dried and atomized by injecting it through a waveguide in which an intense electromagnetic field is maintained.
  • the invention relates to a process for drying / atomizing a product in solution or in suspension in a liquid, which process comprises:
  • a direct energy transfer is carried out in a portion of the waveguide, in free space, until complete vaporization of the liquid and obtaining a dry residue.
  • the product in solution or in suspension, is introduced into a monomodal waveguide; it crosses the electromagnetic field maintained in said waveguide and leaves it, in the dry state.
  • TE 010 or TM 010 mode is generated in said waveguide, a standing wave characterized by the presence of at least one maximum (belly) of the electric field.
  • the solution or suspension is injected in order to transfer energy to it.
  • This energy transfer is optimized by carrying out said injection in a direction almost parallel to that of the electric field and better still, in such a direction in a zone for focusing the power of the waves.
  • the waveguide is previously perforated for said injection, said perforation advantageously authorizing an injection in a direction almost parallel to that of the electric field.
  • the resonant cavity of said waveguide is then advantageously adapted to locate the power at the injection zone.
  • Said injection should also be carried out with a minimum of energy to combat the overpressure generated by the evaporation of the liquid within the waveguide.
  • We will adjust the injection rate taking into account this fact and we can also counter it by aspirating the powdered product generated.
  • the solution or suspension is injected into the waveguide in the form of a continuous jet or sprayed in fine droplets.
  • a tube - of a diameter greater than that of the inlet piping - tube intended to guide the powder generated and not the transport of the feed solution or suspension.
  • a tube is obviously transparent to microwaves and it is arranged to prevent clogging. It is advantageously made of a self-cleaning substance and / or subjected to vibrations by ultrasound.
  • the gas used is advantageously air. It can consist of an inert gas.
  • the waveguide is a rectangular parallelepiped and the solution or suspension is injected perpendicular to the longest side of the parallelepiped.
  • the waveguide is a cylinder and the solution or suspension is injected along the axis of said cylinder.
  • the dry product obtained is advantageously recovered by gravity through an orifice in the waveguide, opposite the orifice for injecting the solution or suspension.
  • said orifices must not allow significant wave leakage.
  • an apparatus capable of treating a few liters per hour has a volume of the order of a liter while a conventional apparatus of the same capacity has a volume of the order of cubic meter.
  • the process of the invention is very clean in that in particular it does not generate pollution and it does not induce any contamination of the product. Said product can be dried without contact with walls and without pollution by a flame. .
  • the process of the invention is very flexible. It can be implemented continuously or discontinuously with very low thermal inertia.
  • the energy efficiency of said process is high, insofar as the energy is supplied to the core of the material.
  • Said method ensures a high degree of homogeneity of treatment, whence obtaining a homogeneous product by quenching the amorphous state of the starting solution or suspension.
  • They may especially be aqueous or alcoholic solutions or suspensions.
  • liquids containing alcohol or other solvents will be treated with the usual precautions.
  • the drying can go as far as a thorough heat treatment of the dry product, initially in solution or suspension.
  • This variant of the invention can be developed in the context of the treatment of aqueous solutions containing uranium and / or plutonium salts, in particular nitrates.
  • the method of the invention can advantageously be implemented in many fields.
  • a waveguide the cavity of which can be adapted, and which comprises at least two opposite orifices, one upper for the injection of the solution or suspension, the other lower for the evacuation powdery product and generated gases; said orifices being advantageously positioned along an axis almost parallel to the electric field;
  • Said magnetron associated with a high-voltage transformer transforms, in a manner known per se, the energy of the network into microwave energy.
  • the transmitted wave propagates in the waveguide.
  • the cavity of the latter is adapted by, in particular, bringing into play, on the side opposite to said magnetron, a short-circuit piston and, on the magnetron side, an iris and / or impedance matching pistons and / or impedance screws (staub ).
  • Said adaptation consists in focusing the energy at the desired location (advantageously the zone of injection and passage of the product).
  • the wave and the material interact directly in a portion of the waveguide.
  • Said waveguide is perforated right through, in at least one place.
  • the upper port is used for injection, the lower port for recovery.
  • the diameter of said orifices is limited in order not to cause significant wave leakage. In principle, it must be less than 20 mm (at 2450 MHz), it being understood that the limit value of said diameter depends on the frequency of the wave.
  • the cavity is adapted for this purpose.
  • the waveguide can be cylindrical or parallelepiped (rectangle). In the case of a cylindrical waveguide, there is generally only one pair of orifices, in the axis of the cylinder.
  • a rectangular parallelepiped waveguide there are one or more pairs of orifices on the longest sides of the parallelepiped. Near the upper orifices, there are means - nozzles - for injecting the solution or suspension to be treated; near the lower orifices, means for recovering the treated product and the gases generated.
  • Said gases are generally evacuated by suction. Take care not to drag the powdered product with them. To this end, a cleanable filter may be used.
  • means can be found to channel the powdered product generated.
  • said means may consist of an annular gas curtain or of a tube transparent to microwaves and arranged to prevent clogging.
  • annular gas curtain it can be generated using a circular slot provided on the waveguide, supplied by a manifold maintained at a pressure compatible with the flow rate of solution or suspension to be treated and the diameter of the dried product discharge orifice. It emerges from the above remarks that the device for implementing the method of the invention is neither complicated nor bulky.
  • the liquid to be treated - solution or suspension - is stored in (1).
  • E is injected through the nozzle (2) into the waveguide (3). Its injection rate is regulated in (4) (pump whose motor is slaved to a flow meter).
  • the waveguide (3) is of parallelepiped shape. Its cavity is adapted, magnetron side by impedance screws (5) and side opposite to said magnetron, by a short circuit piston (6). The adjustment of said screws (5) and of said piston (6) makes it possible to position a maximum of power at the level of the injection axis.
  • Said waveguide comprises, facing each other, two orifices (7 and 8), the upper one (7) for introducing the liquid into the waveguide (3), the other lower ( 8) for the evacuation of gases and powder.
  • the diameter of said orifices should be less than 20 mm (at 2450 MHz), to avoid any significant wave leakage.
  • the liquid then the powder generated are channeled within said waveguide (3) by an air curtain (9).
  • compressed air is sent to (10).
  • the dry product is recovered in (12), using an endless extraction screw, in the form of a powder.
  • (13) we have schematized a cleanable filter plane, which retains said powder. The filter is regularly unclogged by back pressure.
  • a device of this type - without air curtain - was used for drying / atomizing, according to the invention, an aqueous solution containing, by weight, 50% of water, 50% silica.
  • the colloidal silica solution was injected at a rate of approximately 4 kg / h at approximately 0.5 bars, at the level of the upper orifice.
  • the temperature in the waveguide is about 100-1 ° C.
  • the dryer / atomizer chamber should have had a volume of approximately 3 m 3 .

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  • Engineering & Computer Science (AREA)
  • Microbiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Molecular Biology (AREA)
  • Biotechnology (AREA)
  • Biomedical Technology (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Electromagnetism (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Drying Of Solid Materials (AREA)
  • Constitution Of High-Frequency Heating (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

Process for drying/spraying a product in solution or suspended in a liquid. The process essentially consists in injecting the solution or suspension through a monomodal wave guide (3), traversed by a stationary mode of microwaves. The invention also concerns a device for carrying out said process.

Description

Procédé de séchage / atomisation et dispositif pour sa mise en oeuyre ' — ~ _ *" Drying / atomization process and device for its implementation '- ~ _ * "
La présente invention a pour objet un procédé de séchage / atomisation d'un produit en solution ou en suspension dans un liquide. Elle concerne également un dispositif pour la mise en oeuvre dudit procédé.The present invention relates to a method of drying / atomizing a product in solution or in suspension in a liquid. It also relates to a device for implementing said method.
Le procédé de l'invention permet de sécher rapidement, de façon homogène, dans un très faible volume et sans générer de pollution.The process of the invention makes it possible to dry quickly, homogeneously, in a very small volume and without generating pollution.
11 est basé sur l'utilisation directe de l'énergie d'un rayonnement micro¬ onde.11 is based on the direct use of the energy of microwave radiation.
On peut utiliser aux fins de l'invention, des micro-ondes dont la fréquence est comprise entre 800 et 30 000 MHz. Selon l'art antérieur, on met couramment en oeuvre des procédés de séchage / atomisation notamment pour sécher des suspensions aqueuses de minéraux, des extraits de fruits, des produits pharmaceutiques. Conformément à cette technique, le produit - en solution ou en suspension dans un liquide, généralement de l'eau - .est pulvérisé dans une grande chambre, au sein de laquelle est maintenu un courant d'air chaud, destiné à éliminer le liquide des gouttelettes, en un temps très court (de l'ordre de 0,5 à 2 s). On fige pratiquement ainsi la structure amorphe du produit : peu de réactions parasites type cristallisation, floculation... ont le temps de se développer.For the purposes of the invention, microwaves can be used, the frequency of which is between 800 and 30,000 MHz. According to the prior art, drying / atomization processes are commonly used, in particular for drying aqueous suspensions of minerals, fruit extracts, pharmaceutical products. In accordance with this technique, the product - in solution or in suspension in a liquid, generally water - is sprayed into a large chamber, within which a current of hot air is maintained, intended to remove the liquid from the droplets, in a very short time (of the order of 0.5 to 2 s). This practically freezes the amorphous structure of the product: few parasitic reactions such as crystallization, flocculation ... have time to develop.
Le rendement énergétique de ce type de séchage peut être bon avec une plage de traitement thermique étalée ; il est médiocre si l'on souhaite obtenir des résidus secs uniformément traités et de granulométrie centrée.The energy efficiency of this type of drying can be good with a wide range of heat treatment; it is poor if it is desired to obtain dry residues which are uniformly treated and of centered particle size.
La technique est éprouvée mais nécessite un appareillage volumineux, pour sa mise en oeuvre. De plus, la production et l'entretien du courant d'air chaud engendrent un volume important de gaz de combustion. On a, selon d'autres techniques, utilisé l'énergie des micro-ondes pour sécher un produit solide.The technique is proven but requires a bulky apparatus, for its implementation. In addition, the production and maintenance of the hot air stream generates a large volume of combustion gases. Other techniques have used the energy of microwaves to dry a solid product.
Le produit, en couche mince sur un tapis, peut être séché en continu, par défilement dudit tapis dans un guide d'onde ou sous un guide à fentes. L'utilisation d'un guide à fentes est notamment décrite dans le brevet FR 1 488292.The product, in a thin layer on a carpet, can be dried continuously, by passing said carpet through a waveguide or under a slotted guide. The use of a slotted guide is described in particular in patent FR 1 488292.
Le produit peut également être séché en discontinu, en petite quantité dans un guide monomodal ou en plus grosse quantité en brassant ledit produit ou les ondes.The product can also be dried batchwise, in small quantities in a single-mode guide or in larger quantities by stirring said product or the waves.
Le passage dudit produit d'un état humide à un état sec se fait ainsi en un temps suffisamment long pour provoquer des réactions parasites.The passage of said product from a wet state to a dry state thus takes place in a time long enough to cause parasitic reactions.
FEUILLE DE REMPLACEMENT On a également utilisé l'énergie des micro-ondes pour élever la température d'un liquide ; ledit liquide circulant dans un tube qui traverse un guide d'onde monomodaLREPLACEMENT SHEET Microwave energy has also been used to raise the temperature of a liquid; said liquid circulating in a tube which crosses a monomodaL waveguide
Selon l'invention, on propose présentement une utilisation originale de l'énergie des micro-ondes pour obtenir, sous forme pulvérulente, un produit initialement en solution ou en suspension dans un liquide. On sèche et atomise ledit produit en l'injectant au travers d'un guide d'onde dans lequel est maintenu un champ électromagnétique intense.According to the invention, an original use of microwave energy is currently proposed to obtain, in powder form, a product initially in solution or in suspension in a liquid. Said product is dried and atomized by injecting it through a waveguide in which an intense electromagnetic field is maintained.
Plus précisément, l'invention concerne un procédé de séchage/ atomisation d'un produit en solution ou en suspension dans un liquide, procédé qui comprend :More specifically, the invention relates to a process for drying / atomizing a product in solution or in suspension in a liquid, which process comprises:
- L'injection de la solution ou suspension dudit produit au travers d'un guide d'onde monomodal, parcouru par un régime stationnaire de micro-ondes ;- The injection of the solution or suspension of said product through a single-mode waveguide, traversed by a stationary microwave regime;
- la vaporisation dudit liquide dans ledit guide d'onde par transfert direct d'énergie ;- vaporization of said liquid in said waveguide by direct transfer of energy;
- la récupération dudit produit, sous forme pulvérulente ;- the recovery of said product, in powder form;
- l'évacuation des gaz générés.- the evacuation of the gases generated.
De façon originale, on réalise dans une portion de guide d'onde, un transfert d'énergie direct, en espace libre, jusqu'à vaporisation complète du liquide et obtention d'un résidu sec.In an original way, a direct energy transfer is carried out in a portion of the waveguide, in free space, until complete vaporization of the liquid and obtaining a dry residue.
Selon l'invention, le produit, en solution ou en suspension, est introduit dans un guide d'onde monomodal ; il traverse le champ électromagnétique maintenu dans ledit guide d'onde et ressort de celui-ci, à l'état sec.According to the invention, the product, in solution or in suspension, is introduced into a monomodal waveguide; it crosses the electromagnetic field maintained in said waveguide and leaves it, in the dry state.
De façon connue en soi, on génère en mode TE 010 ou TM 010 dans ledit guide d'onde, une onde stationnaire caractérisée par la présence d'au moins un maximum (ventre) du champ électrique.In a manner known per se, in TE 010 or TM 010 mode is generated in said waveguide, a standing wave characterized by the presence of at least one maximum (belly) of the electric field.
On injecte la solution ou suspension dans le but de lui transférer de l'énergie.The solution or suspension is injected in order to transfer energy to it.
On optimise ce transfert d'énergie en effectuant ladite injection selon une direction quasi parallèle à celle du champ électrique et mieux encore, selon une telle direction dans une zone de focalisation de la puissance des ondes.This energy transfer is optimized by carrying out said injection in a direction almost parallel to that of the electric field and better still, in such a direction in a zone for focusing the power of the waves.
L'homme du métier n'éprouvera aucune difficulté à générer dans un guide d'onde un régime stationnaire de micro-ondes d'une puissance donnée, à optimiser la direction et le positionnement de l'injection au travers dudit guide d'onde. En pratique, le guide d'onde est préalablement perforé pour ladite injection, ladite perforation autorisant avantageusement une injection dans une direction quasi parallèle à celle du champ électrique. On adapte ensuite avantageusement la cavité résonnante dudit guide d'onde pour localiser la puissance au niveau de la zone d'injection. II convient également de mettre en oeuvre ladite injection avec un minimum d'énergie pour lutter contre la surpression générée par l'évaporation du liquide au sein du guide d'onde. On réglera le débit d'injection en tenant compte de ce fait et l'on pourra également le contrer en aspirant le produit pulvérulent généré. Selon l'invention, la solution ou suspension est injectée dans le guide d'onde sous la forme d'un jet continu ou pulvérisée en fines gouttelettes.Those skilled in the art will experience no difficulty in generating in a waveguide a stationary regime of microwaves of a given power, in optimizing the direction and positioning of the injection through said waveguide. In practice, the waveguide is previously perforated for said injection, said perforation advantageously authorizing an injection in a direction almost parallel to that of the electric field. The resonant cavity of said waveguide is then advantageously adapted to locate the power at the injection zone. Said injection should also be carried out with a minimum of energy to combat the overpressure generated by the evaporation of the liquid within the waveguide. We will adjust the injection rate taking into account this fact and we can also counter it by aspirating the powdered product generated. According to the invention, the solution or suspension is injected into the waveguide in the form of a continuous jet or sprayed in fine droplets.
Pour obtenir le résultat recherché au niveau de ladite injection, on utilisera une buse adéquate.To obtain the desired result at the level of said injection, an adequate nozzle will be used.
Pour la mise en oeuvre du procédé de l'invention, on effectuera évidemment des calculs et réglages préalables pour adapter la puissance fournie par les micro-ondes à celle nécessaire au traitement souhaité (séchage pouvant aller jusqu'à un traitement thermique poussé du produit sec) d'un volume donné de solution ou suspension, introduit sous la forme d'un jet continu ou pulvérisé en fines gouttelettes, et présentant des caractéristiques intrinsèques. On a précisé ci-dessus que selon le procédé de l'invention, la solution ou suspension était chauffée directement, en espace libre. Le liquide ne remplit pas un tube dans le prolongement de la tuyauterie d'arrivée, tube qui assurerait son transport au travers du guide d'onde. Au sein d'un tel tube, on risquerait de générer des explosions du fait de la forte expansion de volume due à l'évaporation.For the implementation of the process of the invention, obviously calculations and preliminary adjustments will be made to adapt the power supplied by the microwaves to that necessary for the desired treatment (drying can go up to a thorough heat treatment of the dry product ) a given volume of solution or suspension, introduced in the form of a continuous jet or sprayed in fine droplets, and having intrinsic characteristics. It was specified above that according to the method of the invention, the solution or suspension was heated directly, in free space. The liquid does not fill a tube in the extension of the inlet piping, which tube would ensure its transport through the waveguide. Within such a tube, there is a risk of generating explosions due to the large volume expansion due to evaporation.
On n'exclut pourtant pas, selon l'invention, la présence d'un tube - d'un diamètre supérieur à celui de la tuyauterie d'arrivée - tube, destiné à assurer le guidage de la poudre générée et non pas le transport de la solution ou suspension d'alimentation. Un tel tube est évidemment transparent aux micro-ondes et il est agencé pour éviter tout colmatage. Il est avantageusement en une substance autonettoyante et/ou soumis à des vibrations par ultrasons.However, it is not excluded, according to the invention, the presence of a tube - of a diameter greater than that of the inlet piping - tube, intended to guide the powder generated and not the transport of the feed solution or suspension. Such a tube is obviously transparent to microwaves and it is arranged to prevent clogging. It is advantageously made of a self-cleaning substance and / or subjected to vibrations by ultrasound.
En tout état de cause, son diamètre est supérieur à celui de la tuyauterie d'alimentation. On peut, selon une autre variante du procédé de l'invention -variante préférée-, canaliser, grâce à un rideau de gaz annulaire, la poudre générée au sein du guide d'onde.In any event, its diameter is greater than that of the supply piping. It is possible, according to another variant of the method of the invention - preferred variant -, channeling, by means of an annular gas curtain, the powder generated within the waveguide.
Le gaz utilisé est avantageusement de l'air. Il peut consister en un gaz inerte.The gas used is advantageously air. It can consist of an inert gas.
On veillera en effet à ce que ledit gaz soit compatible avec les produits en solution ou en suspension, avec les liquides desdites solution ou suspension et les vapeurs correspondantes.It will in fact be ensured that said gas is compatible with the products in solution or in suspension, with the liquids of said solution or suspension and the corresponding vapors.
Ledit gaz et lesdites vapeurs sont alors évacués simultanément (extraction).Said gas and said vapors are then removed simultaneously (extraction).
L'intervention d'un tel rideau de gaz est particulièrement avantageuse. Outre la canalisation de la poudre générée, ledit rideau de gaz assure notamment :The intervention of such a gas curtain is particularly advantageous. In addition to channeling the powder generated, said gas curtain ensures in particular:
- le guidage de la solution ou suspension à traiter ; - la focalisation du brouillard et/ou jet ; ce qui augmente sa densité et permet ainsi une meilleure dissipation de l'énergie ;- guiding the solution or suspension to be treated; - focusing the fog and / or jet; which increases its density and thus allows better energy dissipation;
- la protection contre toute contamination du produit généré.- protection against contamination of the generated product.
Selon une variante préférée de l'invention, le guide d'onde est un parallélépipède rectangle et la solution ou suspension est injectée perpendiculairement au plus grand côté du parallélépipède.According to a preferred variant of the invention, the waveguide is a rectangular parallelepiped and the solution or suspension is injected perpendicular to the longest side of the parallelepiped.
Selon une autre variante, le guide d'onde est un cylindre et la solution ou suspension est injectée selon l'axe dudit cylindre.According to another variant, the waveguide is a cylinder and the solution or suspension is injected along the axis of said cylinder.
Le produit sec obtenu est avantageusement récupéré par gravité au travers d'un orifice du guide d'onde, en vis-à-vis de l'orifice d'injection de la solution ou suspension.The dry product obtained is advantageously recovered by gravity through an orifice in the waveguide, opposite the orifice for injecting the solution or suspension.
Pour la bonne marche du procédé de l'invention, lesdits orifices ne doivent pas autoriser de fuite d'onde significative.For the proper functioning of the process of the invention, said orifices must not allow significant wave leakage.
Pour faciliter la récupération dudit produit sec et l'évacuation des gaz, on peut avantageusement créer une dépression au sein du guide d'onde. II ressort de la description ci-dessus les nombreux avantages du procédé de l'invention.To facilitate the recovery of said dry product and the evacuation of gases, it is advantageously possible to create a vacuum within the waveguide. The numerous advantages of the process of the invention emerge from the description above.
. Celui-ci permet notamment un séchage très rapide (de 10 à 100 fois plus rapide que celui mis en oeuvre dans un sécheur / atomiseur classique ; un séchage en 1/100 s environ) ; séchage qui induit une véritable trempe de la structure du produit. On obtient un extrait sec amorphe et homogène. . Il nécessite pour sa mise en oeuvre un appareil de très faible volume, qui peut facilement être nucléarisé. Selon l'invention, un appareil capable de traiter quelques litres par heure, a un volume de l'ordre du litre alors qu'un appareil conventionnel de même capacité présente un volume de l'ordre du mètre cube.. This allows in particular very fast drying (10 to 100 times faster than that used in a conventional dryer / atomizer; drying in about 1/100 s); drying which induces a real hardening of the product structure. An amorphous and homogeneous dry extract is obtained. . For its implementation, it requires a device of very small volume, which can easily be nuclearized. According to the invention, an apparatus capable of treating a few liters per hour has a volume of the order of a liter while a conventional apparatus of the same capacity has a volume of the order of cubic meter.
. Le procédé de l'invention est très propre en ce que notamment il ne génère pas de pollution et il n'induit aucune contamination du produit. Ledit produit peut être séché sans contact avec des parois et sans pollution par une flamme. . Le procédé de l'invention est très souple. Il peut être mis en oeuvre en continu ou en discontinu avec une très faible inertie thermique.. The process of the invention is very clean in that in particular it does not generate pollution and it does not induce any contamination of the product. Said product can be dried without contact with walls and without pollution by a flame. . The process of the invention is very flexible. It can be implemented continuously or discontinuously with very low thermal inertia.
. Le rendement énergétique dudit procédé est élevé, dans la mesure où l'énergie est apportée au coeur du matériau.. The energy efficiency of said process is high, insofar as the energy is supplied to the core of the material.
. Ledit procédé assure une grande homogénéité de traitement, d'où l'obtention d'un produit homogène par trempe de l'état amorphe de la solution ou suspension de départ.. Said method ensures a high degree of homogeneity of treatment, whence obtaining a homogeneous product by quenching the amorphous state of the starting solution or suspension.
On insistera par ailleurs sur les nombreuses et diverses applications possibles dudit procédé.We will also emphasize the many and various possible applications of the process.
Il peut notamment être mis en oeuvre : - pour le séchage flash de liquides instables,It can in particular be used: - for flash drying of unstable liquids,
- pour le séchage propre de produits à forte valeur ajoutée (en chimie fine, pharmacie,...),- for the proper drying of products with high added value (in fine chemicals, pharmacy, ...),
- pour le séchage d'oxydes purs préparés en phase liquide,- for the drying of pure oxides prepared in the liquid phase,
- pour le séchage de boues de stations de traitement, d'effluents notamment radioactifs,- for the drying of sludge from treatment stations, effluents, in particular radioactive,
- pour le séchage / traitement thermique de produits.- for drying / heat treatment of products.
Il est mis en oeuvre avec des solutions ou suspensions du produit, que l'on souhaite récupérer sec.It is implemented with solutions or suspensions of the product, which one wishes to recover dry.
Il peut notamment s'agir de solutions ou suspensions aqueuses ou alcooliques.They may especially be aqueous or alcoholic solutions or suspensions.
On traitera, selon l'invention, les liquides contenant de l'alcool ou d'autres solvants avec les précautions d'usage.According to the invention, liquids containing alcohol or other solvents will be treated with the usual precautions.
On peut également mettre en oeuvre le procédé de l'invention avec des gels, et notamment des alcogels. En fait, dans la présente description et les revendications qui suivent on inclut dans le terme générique "solution" lesdits gels.The process of the invention can also be implemented with gels, and in particular alkogels. In fact, in the present description and the claims which follow, said gels are included in the generic term "solution".
Selon une variante de l'invention, le séchage peut aller jusqu'à un traitement thermique poussé du produit sec, initialement en solution ou suspension.According to a variant of the invention, the drying can go as far as a thorough heat treatment of the dry product, initially in solution or suspension.
Pour maîtriser un tel traitement thermique, on optimisera, de la même façon que pour un simple séchage / atomisation, la puissance délivrée, le temps de séjour du produit sec...To control such a heat treatment, we will optimize, in the same way as for a simple drying / atomization, the power delivered, the residence time of the dry product ...
Cette variante de l'invention peut être développée dans le cadre du traitement de solutions aqueuses contenant des sels d'uranium et/ou de plutonium, notamment des nitrates.This variant of the invention can be developed in the context of the treatment of aqueous solutions containing uranium and / or plutonium salts, in particular nitrates.
On peut ainsi, injecter une solution de nitrate d'uranyle ou de plutonium, en éliminer l'eau dans un premier temps, détruire les nitrates dans un second temps et récupérer, sous forme de poudre des oxydes d'uranium et/ou de plutonium.It is thus possible to inject a solution of uranyl or plutonium nitrate, to eliminate the water in a first step, to destroy the nitrates in a second step and to recover, in the form of powder, uranium and / or plutonium oxides. .
Comme cela ressort des propos ci-dessus, le procédé de l'invention peut avantageusement être mis en oeuvre dans de nombreux domaines.As is apparent from the above remarks, the method of the invention can advantageously be implemented in many fields.
Sa mise en oeuvre est aisée ; elle nécessite un dispositif de très faible volume. Un tel dispositif constitue un autre objet de la présente invention.Its implementation is easy; it requires a device of very small volume. Such a device constitutes another object of the present invention.
Il comprend :He understands :
- un magnétron convenablement alimenté ;- a magnetron suitably supplied;
- un guide d'onde, dont on peut adapter la cavité, et qui comporte au moins deux orifices en vis-à-vis, l'un supérieur pour l'injection de la solution ou suspension, l'autre inférieur pour l'évacuation du produit pulvérulent et des gaz générés ; lesdits orifices étant avantageusement positionnés suivant un axe quasi parallèle au champ électrique ;- A waveguide, the cavity of which can be adapted, and which comprises at least two opposite orifices, one upper for the injection of the solution or suspension, the other lower for the evacuation powdery product and generated gases; said orifices being advantageously positioned along an axis almost parallel to the electric field;
- des moyens pour l'injection de ladite solution ou suspension au travers dudit (desdits) orifice(s) supérieurs) ; - des moyens pour la récupération dudit produit pulvérulent sous ledit- means for injecting said solution or suspension through said (said) orifice (s) above); means for recovering said pulverulent product under said
(lesdits) orifice(s) inférieurs) ;(said) lower orifice (s));
- des moyens pour l'évacuation desdits gaz ;- means for the evacuation of said gases;
- et éventuellement des moyens de canalisation dudit produit pulvérulent, au sein dudit guide d'onde. Ledit magnétron associé à un transformateur haute-tension transforme de façon connue en soi l'énergie du réseau en énergie micro-onde.- And possibly means for channeling said pulverulent product, within said waveguide. Said magnetron associated with a high-voltage transformer transforms, in a manner known per se, the energy of the network into microwave energy.
L'onde émise se propage dans le guide d'onde. On adapte la cavité de celui-ci en faisant notamment intervenir, côté opposé audit magnétron un piston de court-circuit et côté magnétron, un iris et/ou des pistons d'adaptation d'impédance et/ou des vis d'impédance (staub). Ladite adaptation consiste à focaliser l'énergie à l'endroit souhaité (avantageusement la zone d'injection et de passage du produit).The transmitted wave propagates in the waveguide. The cavity of the latter is adapted by, in particular, bringing into play, on the side opposite to said magnetron, a short-circuit piston and, on the magnetron side, an iris and / or impedance matching pistons and / or impedance screws (staub ). Said adaptation consists in focusing the energy at the desired location (advantageously the zone of injection and passage of the product).
On insistera sur le fait que, de façon originale, selon le procédé de l'invention, l'onde et la matière interagissent directement dans une portion du guide d'onde.It will be emphasized that, in an original manner, according to the method of the invention, the wave and the material interact directly in a portion of the waveguide.
Ledit guide d'onde est perforé de part en part, en au moins un endroit. L'orifice supérieur est utilisé pour l'injection, l'orifice inférieur pour la récupération. Le diamètre desdits orifices est limité dans le but de ne pas occasionner de fuite d'onde significative. En principe, il doit être inférieur à 20 mm (en 2450 MHz), étant entendu que la valeur limite dudit diamètre dépend de la fréquence de l'onde.Said waveguide is perforated right through, in at least one place. The upper port is used for injection, the lower port for recovery. The diameter of said orifices is limited in order not to cause significant wave leakage. In principle, it must be less than 20 mm (at 2450 MHz), it being understood that the limit value of said diameter depends on the frequency of the wave.
On peut également trouver, sur un même guide d'onde plusieurs couples d'orifices, en vis-à-vis. Lesdits orifices sont avantageusement positionnés suivant un axe quasi parallèle au champ électrique.One can also find, on the same waveguide several pairs of orifices, facing each other. Said orifices are advantageously positioned along an axis almost parallel to the electric field.
Au niveau de chacun desdits couples d'orifice, on trouve avantageusement un maximum de puissance. La cavité est adaptée à cet effet. Le guide d'onde peut être cylindrique ou parallélépipédique (rectangle). Dans le cas d'un guide d'onde cylindrique, on trouve généralement un seul couple d'orifices, dans l'axe du cylindre.At each of said pairs of orifices, there is advantageously a maximum of power. The cavity is adapted for this purpose. The waveguide can be cylindrical or parallelepiped (rectangle). In the case of a cylindrical waveguide, there is generally only one pair of orifices, in the axis of the cylinder.
Dans le cas d'un guide d'onde parallélépipédique rectangle, on trouve un ou plusieurs couple(s) d'orifices sur les plus grands côtés du parallélépipède. A proximité des orifices supérieurs, on trouve des moyens - buses - pour l'injection de la solution ou suspension à traiter ; à proximité des orifices inférieurs, des moyens pour la récupération du produit traité et des gaz générés. L'homme de l'art peut agencer lesdits moyens selon diverses variantes. On évacue généralement lesdits gaz, par aspiration. On veillera à ne pas entraîner avec ceux-ci le produit en poudre. A cette fin, on pourra faire intervenir un filtre décolmatable. Au sein du guide d'onde, on peut trouver des moyens pour canaliser le produit pulvérulent généré. Comme précisé ci-dessus, lesdits moyens peuvent consister en un rideau de gaz annulaire ou en un tube transparent aux micro- ondes et agencé pour éviter tout colmatage. On a préalablement insisté sur le diamètre d'un tel tube qui doit être supérieur à celui de la tuyauterie d'alimentation. En ce qui concerne le rideau de gaz annulaire, il peut être généré à l'aide d'une fente circulaire prévue sur le guide d'onde, alimentée par une nourrice maintenue à une pression compatible avec le débit de solution ou suspension à traiter et le diamètre de l'orifice d'évacuation du produit séché. II ressort des propos ci-dessus que le dispositif pour la mise en oeuvre du procédé de l'invention n'est ni compliqué, ni volumineux.In the case of a rectangular parallelepiped waveguide, there are one or more pairs of orifices on the longest sides of the parallelepiped. Near the upper orifices, there are means - nozzles - for injecting the solution or suspension to be treated; near the lower orifices, means for recovering the treated product and the gases generated. Those skilled in the art can arrange said means according to various variants. Said gases are generally evacuated by suction. Take care not to drag the powdered product with them. To this end, a cleanable filter may be used. Within the waveguide, means can be found to channel the powdered product generated. As specified above, said means may consist of an annular gas curtain or of a tube transparent to microwaves and arranged to prevent clogging. We previously insisted on the diameter of such a tube which must be greater than that of the supply piping. As regards the annular gas curtain, it can be generated using a circular slot provided on the waveguide, supplied by a manifold maintained at a pressure compatible with the flow rate of solution or suspension to be treated and the diameter of the dried product discharge orifice. It emerges from the above remarks that the device for implementing the method of the invention is neither complicated nor bulky.
L'invention est illustrée sur l'unique dessin - figure 1 - joint à la présente description.The invention is illustrated in the single drawing - Figure 1 - attached to this description.
Sur celui-ci, on a représenté en coupe une installation de séchage / atomisation, au sein de laquelle le procédé de l'invention est mis en oeuvre.On this, there is shown in section a drying / atomization installation, within which the method of the invention is implemented.
Le liquide à traiter - solution ou suspension - est stocké en (1). E est injecté, grâce à la buse (2) dans le guide d'onde (3). Son débit d'injection est régulé en (4) (pompe dont le moteur est asservi à un débitmètre).The liquid to be treated - solution or suspension - is stored in (1). E is injected through the nozzle (2) into the waveguide (3). Its injection rate is regulated in (4) (pump whose motor is slaved to a flow meter).
Le guide d'onde (3) est de forme parallélépipédique. Sa cavité est adaptée, côté magnétron par des vis d'impédance (5) et côte opposé audit magnétron, par un piston de court circuit (6). Le réglage desdites vis (5) et dudit piston (6) permet de positionner un maximum de puissance au niveau de l'axe d'injection.The waveguide (3) is of parallelepiped shape. Its cavity is adapted, magnetron side by impedance screws (5) and side opposite to said magnetron, by a short circuit piston (6). The adjustment of said screws (5) and of said piston (6) makes it possible to position a maximum of power at the level of the injection axis.
Ledit guide d'onde comporte, en vis-à-vis, deux orifices (7 et 8), l'un supérieur (7) pour l'introduction du liquide dans le guide d'ondes (3), l'autre inférieur (8) pour l'évacuation des gaz et de la poudre. On a vu que le diamètre desdits orifices devait être inférieur à 20 mm (en 2450 MHz), pour éviter toute fuite d'onde significative.Said waveguide comprises, facing each other, two orifices (7 and 8), the upper one (7) for introducing the liquid into the waveguide (3), the other lower ( 8) for the evacuation of gases and powder. We have seen that the diameter of said orifices should be less than 20 mm (at 2450 MHz), to avoid any significant wave leakage.
Le liquide puis la poudre générée sont canalisés au sein dudit guide d'onde (3) par un rideau d'air (9). Pour générer ledit rideau d'air, on envoie en (10) de l'air comprimé.The liquid then the powder generated are channeled within said waveguide (3) by an air curtain (9). To generate said air curtain, compressed air is sent to (10).
Ledit air ainsi que les vapeurs générées lors du séchage sont évacués en (11), par extraction.Said air as well as the vapors generated during drying are removed in (11), by extraction.
On récupère en (12), à l'aide d'une vis sans fin d'extraction, le produit sec, sous la forme d'une poudre. En (13), on a schématisé un filtre décolmatable plan, qui retient ladite poudre. Régulièrement on décolmate ledit filtre par contre-pression.The dry product is recovered in (12), using an endless extraction screw, in the form of a powder. In (13), we have schematized a cleanable filter plane, which retains said powder. The filter is regularly unclogged by back pressure.
A titre d'exemple, on précise qu'un dispositif de ce type - sans rideau d'air - a été utilisé pour le séchage / atomisation, selon l'invention, d'une solution aqueuse contenant, en poids, 50 % d'eau, 50 % de silice.For example, it is specified that a device of this type - without air curtain - was used for drying / atomizing, according to the invention, an aqueous solution containing, by weight, 50% of water, 50% silica.
A l'intérieur d'un guide d'onde parallélépipédique, à section rectangulaire, fonctionnant en mode TE 010, sous une puissance de 5 kW micro-ondes environ en 2450 MHz, on a généré une cavité résonnante (de dimensions : 100 mm environ x 86,6 mm x 43,3 mm). Au sein de ladite cavité, le champ électrique passe par un seul maximum (dit ventre de puissance). Au niveau de celui-ci, le guide d'onde est percé de part en part. Les orifices d'injection et de récupération ont le même diamètre : φ = 16 mm. La solution colloïdale de silice a été injectée à raison de 4 kg/h environ sous 0,5 bars environ, au niveau de l'orifice supérieur. La température dans le guide d'onde est d'environ 100 - 1 ÎO'C.Inside a parallelepipedic waveguide, with rectangular section, operating in TE 010 mode, under a power of about 5 kW microwave at 2450 MHz, a resonant cavity has been generated (of dimensions: about 100 mm x 86.6 mm x 43.3 mm). Within said cavity, the electric field passes through a single maximum (called the power belly). At this level, the waveguide is drilled right through. The injection and recovery ports have the same diameter: φ = 16 mm. The colloidal silica solution was injected at a rate of approximately 4 kg / h at approximately 0.5 bars, at the level of the upper orifice. The temperature in the waveguide is about 100-1 ° C.
En partie inférieure du guide, on a récupéré une poudre de silice, relativement uniforme, à raison de 2 kg/h environ.In the lower part of the guide, a relatively uniform silica powder was recovered, at a rate of approximately 2 kg / h.
Pour obtenir un tel résultat, selon l'art antérieur, la chambre du sécheur / atomiseur aurait dû présenter un volume d'environ 3 m3. To obtain such a result, according to the prior art, the dryer / atomizer chamber should have had a volume of approximately 3 m 3 .

Claims

R E V E N D I C A TI O N SR E V E N D I C A TI O N S
1 Procédé de séchage / atomisation d'un produit en solution ou en suspension dans un liquide, caractérisé en ce qu'il comprend : - l'injection de la solution ou suspension contenant ledit produit au travers d'un guide d'onde monomodal (3), parcouru par un régime stationnaire de micro-ondes ;1 drying / atomization process of a product in solution or in suspension in a liquid, characterized in that it comprises: - the injection of the solution or suspension containing said product through a monomodal waveguide ( 3), traversed by a stationary microwave regime;
- la vaporisation dudit liquide dans ledit guide d'onde (3) par transfert direct d'énergie en espace libre ; - la récupération dudit produit, sous forme pulvérulente ;- vaporization of said liquid in said waveguide (3) by direct transfer of energy in free space; - the recovery of said product, in powder form;
- l'évacuation des gaz générés.- the evacuation of the gases generated.
2. Procédé selon la revendication 1, caractérisé en ce que ladite solution ou suspension est injectée selon une direction quasi parallèle à celle du champ électrique. 2. Method according to claim 1, characterized in that said solution or suspension is injected in a direction almost parallel to that of the electric field.
3. Procédé selon l'une des revendications 1 ou 2, caractérisé en ce que ladite solution ou suspension est injectée dans une zone de focalisation de la puissance des ondes.3. Method according to one of claims 1 or 2, characterized in that said solution or suspension is injected into a focusing area of the power of the waves.
4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que ladite solution ou suspension est injectée sous la forme d'un jet continu ou pulvérisée en fines gouttelettes dans ledit guide d'onde (3).4. Method according to any one of claims 1 to 3, characterized in that said solution or suspension is injected in the form of a continuous jet or sprayed into fine droplets in said waveguide (3).
5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que la poudre générée est canalisée au sein dudit guide d'onde(3), par un rideau de gaz annulaire (9).5. Method according to any one of claims 1 to 4, characterized in that the powder generated is channeled within said waveguide (3), by an annular gas curtain (9).
6. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que la poudre générée est canalisée au sein dudit guide d'onde (3) par un tube, transparent aux micro-ondes et agencé pour éviter tout colmatage.6. Method according to any one of claims 1 to 4, characterized in that the powder generated is channeled within said waveguide (3) by a tube, transparent to microwaves and arranged to avoid clogging.
7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que le guide d'onde (3) est un parallélépipède rectangle et en ce que ladite solution ou suspension est injectée perpendiculairement au plus grand côté du parallélépipède.7. Method according to any one of claims 1 to 6, characterized in that the waveguide (3) is a rectangular parallelepiped and in that said solution or suspension is injected perpendicular to the largest side of the parallelepiped.
8. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que le guide d'onde (3) est un cylindre et en ce que ladite solution ou suspension est injectée selon l'axe dudit cylindre. 8. Method according to any one of claims 1 to 6, characterized in that the waveguide (3) is a cylinder and in that said solution or suspension is injected along the axis of said cylinder.
9. Procédé selon l'une quelconque des revendications 1 à 8, caractérisé en ce qu'il est mis en oeuvre avec des solutions ou suspensions, aqueuses ou alcooliques et notamment des gels.9. Method according to any one of claims 1 to 8, characterized in that it is implemented with solutions or suspensions, aqueous or alcoholic and in particular gels.
10. Procédé selon l'un quelconque des revendications 1 à 9, caractérisé en ce qu'il est mis en oeuvre avec des solutions aqueuses contenant des sels d'uranium et/ou de plutonium, notamment des nitrates.10. Method according to any one of claims 1 to 9, characterized in that it is used with aqueous solutions containing uranium and / or plutonium salts, in particular nitrates.
11. Dispositif pour la mise en oeuvre d'un procédé selon l'une quelconque des revendications précédentes, caractérisé en ce qu'il comprend :11. Device for implementing a method according to any one of the preceding claims, characterized in that it comprises:
- un magnétron convenablement alimenté ; - un guide d'onde (3), dont on peut adapter la cavité, et qui comporte au moins deux orifices (7,8) en vis-à-vis, l'un supérieur (7) pour l'injection de la solution ou suspension, l'autre inférieur (8) pour l'évacuation du produit pulvérulent et des gaz générés ; lesdits orifices (7,8) étant avantageusement positionnés suivant un axe quasi parallèle au champ électrique ; - des moyens (2) pour l'injection de ladite solution ou suspension au travers dudit (desdits) orifice(s) supérieur(s) (7);- a magnetron suitably supplied; - A waveguide (3), the cavity of which can be adapted, and which comprises at least two orifices (7,8) facing each other, the upper one (7) for injecting the solution or suspension, the other lower (8) for the evacuation of the pulverulent product and the gases generated; said orifices (7,8) being advantageously positioned along an axis almost parallel to the electric field; - Means (2) for the injection of said solution or suspension through said (said) orifice (s) upper (s) (7);
- des moyens pour la récupération dudit produit pulvérulent sous ledit (lesdits) orifice(s) inférieur(s) (8);- Means for recovering said pulverulent product under said (said) orifice (s) lower (s) (8);
- des moyens pour l'évacuation desdits gaz ; - et éventuellement des moyens de canalisation dudit produit pulvérulent, au sein dudit guide d'onde.- means for the evacuation of said gases; - And possibly means for channeling said pulverulent product, within said waveguide.
12. Dispositif selon la revendication 11, caractérisé en ce que les moyens pour l'adaptation du guide d'onde consistent, côté magnétron, en un iris et/ou des pistons d'adaptation d'impédance et/ou des vis d'impédance (5), et côté opposé audit magnétron, en un piston de court-circuit (6). 12. Device according to claim 11, characterized in that the means for adapting the waveguide consist, on the magnetron side, of an iris and / or impedance matching pistons and / or impedance screws (5), and opposite side to said magnetron, in a short-circuit piston (6).
PCT/FR1992/001227 1991-12-23 1992-12-22 Process and device for drying/spraying a product WO1993013374A1 (en)

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JPH07506526A (en) 1995-07-20
EP0617783A1 (en) 1994-10-05
CZ154694A3 (en) 1995-01-18
FR2685461A1 (en) 1993-06-25
AU3357493A (en) 1993-07-28
RU94031203A (en) 1996-06-20

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