EP0846016B1 - Method and plant for processing asbestos-containing waste - Google Patents

Method and plant for processing asbestos-containing waste Download PDF

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Publication number
EP0846016B1
EP0846016B1 EP96915921A EP96915921A EP0846016B1 EP 0846016 B1 EP0846016 B1 EP 0846016B1 EP 96915921 A EP96915921 A EP 96915921A EP 96915921 A EP96915921 A EP 96915921A EP 0846016 B1 EP0846016 B1 EP 0846016B1
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European Patent Office
Prior art keywords
reactor
accordance
waste
basic
digestion
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EP96915921A
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German (de)
French (fr)
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EP0846016A1 (en
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Gérard Debailleul
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Priority claimed from BE9500536A external-priority patent/BE1009413A6/en
Priority claimed from BE9500911A external-priority patent/BE1009724A6/en
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    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
    • A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
    • A62D3/36—Detoxification by using acid or alkaline reagents
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/40—Inorganic substances
    • A62D2101/41—Inorganic fibres, e.g. asbestos

Definitions

  • the present invention relates to a waste treatment process containing asbestos, from a site generating such waste, including a reaction by attack of said waste with a basic solution until a reaction product is obtained without asbestos fibers.
  • WO-A-93/18867 describes a process in which the waste is first of all very finely ground in the presence of at least one substance releasing OH ions - in water, so as to form an aqueous suspension . This suspension is optionally then transferred to an autoclave and treated at elevated temperature and pressure.
  • WO-A-94/08661 describes a method of treatment as indicated at the beginning. This process has only aim of producing waste that can be unloaded in a warehouse without the risks inherent in asbestos. The only installation described to realize this treatment is a fixed processing center, large dimension, which therefore provides no solution to waste transportation and storage issues containing asbestos. Finally, during treatment, waste undergoes energy-intensive compaction before their introduction into the treatment chamber.
  • the object of the present invention is to provide a process and installation which avoid the disadvantages mentioned above and which allow processing of waste on the site generating such waste.
  • site waste generator you have to hear not only a building in which we dismantle all the elements containing asbestos, but also for example a deposit rubbish where bags containing asbestos have been previously accumulated. It is therefore desirable that the installation is small and transportable.
  • the invention further aims to avoid any risk of pollution between the generating site and the reactor that will process the waste, i.e. risks of waste bagging and transport of these sachets to a remote processing center.
  • the bagging of construction debris is awkward and very often causes the piercing of sachets, which then allows the asbestos to spread in the atmosphere outside the site.
  • the invention also aims to prevent the maximum any product release occurring in the processing, insofar as it still contains asbestos fibers. Treatment products will be advantageously either recycled or suitable for revaluation.
  • the invention finally aims to avoid any crushing, crushing or compacting prior to entry in the reactor and therefore an introduction into it, without sorting, substrates loaded with asbestos.
  • the transfer takes place in a container removable, closed, and the method further comprises, during or after the transfer, an external washing of the container with washing liquid.
  • an external washing of the container with washing liquid This eliminates asbestos dust that may have settled on the container during its presence in the generating site of waste and therefore not to contaminate the place, near the site, where the basic attack will take place.
  • the container wash water is recycled in the formation of basic attack solution which avoids any pollution of the environment at the exit of the container closed off the waste generating site.
  • the removable container used for transfer aforementioned is also the reactor in which the attack reaction. There is therefore in this case no risk of asbestos pollution during transfer from one container to another, waste without sorters are directly introduced into the reactor at generator site itself.
  • the attack reaction is carried out with the basic attack solution at a temperature of the order of 175 to 190 ° C and under a pressure of about 8 to 10 kg / cm 2 .
  • the installation illustrated in FIGS. 1 to 3 comprises a reactor 1 in the form of an autoclave which can be sealed in a sealed manner by a cover, for example a flip-up cover.
  • This reactor is designed to be able to withstand internal pressures of up to 10 kg / cm 2 . He. is here movable on a carriage 3 provided with rollers 4.
  • This assembly is dimensioned so as to be able to enter buildings, and therefore to be able to pass through doors and enter an elevator. This makes it possible to fill the reactor 1 with waste dismantled in the building, containing asbestos fibers, without prior sorting or grinding. Once the reactor is filled at the waste generating site itself, and therefore without handling bags, the reactor is taken out of the building where the waste is dismantled.
  • He is then preferably brought to a post 5 (figure 1) which has a watering ramp 6 upper, preferably supplied with water under pressure, and a cabin 7, the floor of which is arranged in 8 wash water harvesting basin, which is then charged with the dust that has accumulated on the reactor during its passage through the generator site waste, dust which probably contains themselves asbestos fibers.
  • the collected wash water is sent to a collecting tank 9, via an outlet conduit 10, fitted with a pump 11.
  • the tank 9 is, in the illustrated embodiment, itself mounted so that it can be moved on wheels.
  • Reactor 1 was transferred from carriage 3 to a support 12 capable of tilting around a shaft 13.
  • the output shaft of a rotary motor 15 is coupled to an installed agitator in a known manner at the bottom of the reactor.
  • An engine, no shown, allows the shaft 13 to rotate on its axis and tilt the reactor. All these measures allow appropriate agitation of the contents of the reactor during the attack.
  • Quick connect fittings allow connect reactor 1 to an upper duct 16 and to a lower duct 17, each closable by means of valve.
  • the upper duct 16 is in communication with a multi-way valve 18.
  • the valve 18 allows a entry of rinse water into the reactor from the conduit 19 and / or a basic attack solution inlet from line 20.
  • Electric heating elements 21 are, in the illustrated embodiment, provided inside from reactor 1, and they are connected to a source current when the reactor is in place on the support 12.
  • the attack with the aqueous basic solution can therefore take place in the reactor 1, without possible exit of asbestos fibers to the outside.
  • the basic etching solution may for example be an aqueous solution of OH - ion generating agent, such as alkaline or alkaline-earth bases, in particular 25 M NaOH in flakes, obtained for example by dissolving in 0.5 part by volume of water of 1 part by volume of such NaOH flakes.
  • the attack preferably takes place at a temperature of 175 to 190 ° C and under a pressure of 8 to 10 kg / cm 2 , for a period of 20 to 30 minutes, advantageously with slow stirring, optionally intermittently. After this attack, there is substantially no more asbestos fibers in the reaction product which is of pasty consistency.
  • This reaction product is taken out of the reactor 1 by the lower pipe 17, after opening the corresponding valve, and it is brought to a running centrifuge 22. This transfer can be followed by an internal rinsing of the reactor by adding rinsing water. from
  • fresh water or rinse can still be supplied by a conduit water inlet 23.
  • the centrifuge separates in the pasty product a liquid phase and a precipitate solid.
  • the liquid phase consisting mainly of water and attack base is recovered at the bottom of the centrifuge to be recycled through a recycling conduit 24.
  • the solid precipitate is sent through the outlet 25 in a bin 26 from which a revaluation of this precipitate may take place.
  • Reactor 1 when it closed on the generating site, contains in addition to the waste introduced air heavily loaded with dust and therefore asbestos fibers. During the attack, these particles in suspension are washed and attacked in the same way as solid waste, and asbestos fibers that were suspended are therefore also destroyed.
  • the cover 2 of the reactor 1 can then be open without any danger of environmental pollution.
  • Debris that has been introduced with the waste asbestos on the generating site for example bricks, pieces of wood, etc Vietnamese, can then be discharged by tilting the reactor, and possibly scraping the interior. This debris, completely free of asbestos fibers, can then be routed to a depot or other destination.
  • the installation comprises a solution preparation tank 29, capable of withstanding a pressure of 10 kg / cm 2 and capable of being heated for example by a heating jacket 30 in which a thermal fluid circulates, including oil.
  • the thermal fluid enters at 31 into the jacket 30 and exits at 32.
  • Fresh or rinse water may be supplied in the tank 29 by the inlet duct 36.
  • a outlet conduit 37 of the basic etching solution allows the latter to be taken from the bottom of the tank 29, using a pump 38.
  • This outlet duct 37 is in communication with conduit 20 previously mentioned (see Figure 2) by a valve 39 which is open when reactor 1 must be supplied with basic solution of attack.
  • valve 39 When valve 39 is closed, the solution basic attack is recycled at the top of the tank 29 by a bypass 40, using a static mixer 41. In this tank the basic solution is brought to the desired concentration, at a temperature close to boiling, for example 120 ° C.
  • the installation also advantageously comprises an equalization tank 42 for the basic attack solution.
  • This tank is preferably capable of withstanding a pressure of 5 kg / cm 2 , and it is capable of being slightly heated, for example by a heating jacket 43 in which a thermal fluid, in particular oil, circulates. The thermal fluid enters 44 in the jacket 43 and exits 45.
  • Fresh or rinse water may be introduced into the tank 42 through the inlet conduit 48.
  • An outlet conduit 49 of the basic equalization solution allows to take it from the bottom of the tank 42, using a pump 50.
  • This outlet duct 49 is there is communication with a supply duct 51, by a valve 52.
  • This supply duct 51 allows introduce at the top of the preparation tank 29 a basic equalization solution and thus get a basic attack solution of uniform composition.
  • valve 52 is closed, the basic solution equalization is recycled to the top of the tank 42 by a bypass 53, using a static mixer 54.
  • FIG 4 there is shown the arrangement on a platform 56, transportable by trailer, training part of the basic attack solution the installation.
  • the tanks 29 and 42 of Figure 3 are supported on tray 56. Next to these tanks is a current thermal fluid heating device with a thermal fluid tank 57 and a boiler 58.
  • a battery is shown of reactors 1 supported on a transportable tray 64 by trailer.
  • the reactors are introduced into a heated enclosure 59, the upper part of which can be opened for insertion or the extraction of reactor 1.
  • This operation is carried out using a lifting device known per se 60.
  • the heated enclosure 59 is supported on two ends of the shaft 65 and 66 coaxial so as to be able to rotate around their axis.
  • An agitation of 40 at 50 rpm is for example favorable.
  • the left reactor in Figure 5 is supplied by a removable container in the form of a tray 61, whose upper wall 62 can be opened for the introduction of waste on the generating site.
  • the bottom of this tank 61 provided for transportable and displaceable between the generating site and the transportable unit of treatment according to the invention, is formed by a hopper 63 closable by a drawer, not shown.
  • the upper opening of the reactor is then closed by a corresponding drawer cover. When the two drawers are open, waste from bin 61 can flow into reactor 1, so as not to be able to come into contact with the surrounding environment.
  • the two plates 56 and 64 can be installed side by side and to allow communication between the different containers by the conduits cited above.
  • FIG. 6 a variant of improved installation of the following installation the invention, where the reactor 1 formed from an autoclave at high pressure of the installation according to Figures 1 at 3 is replaced by two successive reactors: 1) a removable reactor 1 'for example in the form a small autoclave capable of operating under extremely moderate pressure and 2 °) a 1 '' fixed reactor.
  • Autoclaves corresponding to requirements of the removable reactor 1 ' are those used commonly in chemistry labs, and they're readily available on the market at moderate cost. These autoclaves have the added benefit of can be expected to be much lighter and less pressure resistant, due to low pressure Implementation.
  • Waste containing asbestos is introduced into reactor 1 'as in reactor 1 of Figure 1 and it is advantageously washed with the same way when leaving the generator site waste. It is then connected to an upper conduit 16 ' which allows to put it in communication with the tank of preparation 29 of the basic attack solution.
  • treatment of waste in reactor 1 'with the basic solution attack at a temperature of 160 to 175 ° C, advantageously at 170 ° C for 15 minutes.
  • reaction product is then transferred by a conduit 17 'to a first centrifuge 22' where the liquid phase is separated from the solid phase.
  • sentence liquid is recycled through line 24 'to the tank preparation 29 or to the equalization tank 42.
  • the solid phase is in the form a paste which still contains asbestos fibers, totally separated. After analysis, we have already been able estimate that, in this state, the fibers obtained do not already pose more danger to human health.
  • This solid phase now has a reduced volume 70% compared to that introduced into the reactor 1 '. It is brought, via a pipe 25 ', to the reactor 1' '.
  • This is a fixed reactor, that is to say which no longer has need to be moved to the waste generating site, and yet it is of a small volume.
  • it is arranged horizontally in order to be able to rotate around an axis horizontal.
  • the basic etching solution is introduced through the 16 '' conduit and a temperature above 180 ° C, for example from 190 to 210 ° C, advantageously around 200 ° C, is maintained in the 1 '' reactor by a 21 '' heat source. There is then decomposition and total disappearance of the asbestos fibers, and formation of a pressure inside the reactor. However, since the treated volume of solid phase is reduced, a pressure of 2.5 kg to 10 kg / cm 2 , preferably 2.5 to 5 kg / cm 2 , may suffice.
  • the reaction product is then transferred in a second centrifuge 22 '' through the conduit 17 '', passing through a cooling device 70.
  • the temperature of the product from the 1 '' reactor is dropped below the temperature at which the soda vaporizes, i.e. around 180 ° C.
  • this centrifuge there is phase separation liquid and solid phase.
  • the liquid phase is recycled through the 24 '' pipe to the preparation tanks and / or equalization of the basic attack solution and the solid phase is brought through the 25 '' conduit to the tray 26.
  • the 16 'and 16' 'conduits can, like the conduit 16 in FIG. 2, serve as recycling means gaseous medium from the respective reactor to the source of basic attack solution.

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  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Business, Economics & Management (AREA)
  • Emergency Management (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

A method for processing asbestos-containing waste from a waste generating site, wherein the waste is transferred from the site to a processing reactor without exposing the waste to an external environment, a basic reaction solution is fed into the reactor, a reaction is carried out to give a substantially fiber-free reaction product, and the reaction product is separated into a solid phase and a liquid phase. The separated liquid phase is optionally recycled to form the basic reaction solution and the separated solid phase is optionally recovered to enable upgrading thereof.

Description

La présente invention est relative à un procédé de traitement de déchets contenant de l'amiante, provenant d'un site générateur de tels déchets, comprenant une réaction par attaque desdits déchets avec une solution basique jusqu'à obtention d'un produit réactionnel sans fibres d'amiante.The present invention relates to a waste treatment process containing asbestos, from a site generating such waste, including a reaction by attack of said waste with a basic solution until a reaction product is obtained without asbestos fibers.

Les effets nocifs de l'amiante dans le circuit respiratoire humain sont bien connus. La plupart des pays du monde prennent des dispositions pour le démontage de l'amiante en particulier dans le bâtiment. Actuellement, lors des démontages, l'amiante est stockée dans des doubles sacs et est ensuite transportée vers des centres de traitement.The harmful effects of asbestos in the circuit respiratory systems are well known. Most of countries of the world arrange for disassembly asbestos especially in the building. Currently, during dismantling, asbestos is stored in double bags and is then transported to treatment centers.

Les centres de traitement les plus importants procèdent

  • a) à un enrobage dans des liants hydrauliques et à une mise en décharge du produit obtenu, ou
  • b) à une incinération par vitrification à très haute température.
    • The most important treatment centers proceed
  • a) a coating in hydraulic binders and a landfill of the product obtained, or
  • b) incineration by vitrification at very high temperature.

    • Dans les deux cas, il y a de gros inconvénients :

    • les risques liés au transport et au stockage, au cours desquels le moindre incident peut résulter en la pollution de l'environnement,
    • la solution a) ne fait que postposer le problème, puisqu'elle ne détruit pas les fibres d'amiante,
    • la solution b) coûte très cher,
    • les solutions a) et b) ne procurent aucune revalorisation des produits issus du traitement.
    In both cases, there are big drawbacks:
    • transport and storage risks, during which the slightest incident can result in environmental pollution,
    • solution a) only postulates the problem, since it does not destroy the asbestos fibers,
    • solution b) is very expensive,
    • solutions a) and b) do not provide any revaluation of the products resulting from the treatment.

    On connaít par ailleurs des traitements par des acides qui présentent l'inconvénient de polluer l'environnement par d'autres déchets dangereux.We also know treatments by acids which have the disadvantage of polluting the environment by other hazardous wastes.

    On connaít enfin des traitements des déchets contenant de l'amiante en milieu alcalin.We finally know about waste treatment containing asbestos in an alkaline environment.

    Dans le WO-A-93/18867 on décrit un procédé dans lequel les déchets sont tout d'abord très finement broyés en présence d'au moins une substance libérant des ions OH- dans l'eau, de façon à former une suspension aqueuse. Cette suspension est éventuellement ensuite transvasée dans un autoclave et traitée à température et pression élevées.WO-A-93/18867 describes a process in which the waste is first of all very finely ground in the presence of at least one substance releasing OH ions - in water, so as to form an aqueous suspension . This suspension is optionally then transferred to an autoclave and treated at elevated temperature and pressure.

    Ce procédé présente l'inconvénient d'une étape préalable de broyage très fin, qui nécessite une installation très puissante, et donc fixe. Le procédé ne résout donc pas les problèmes inhérents au transport et au stockage des déchets, et il apparaít fort coûteux. Par ailleurs rien n'est prévu en ce qui concerne les vapeurs et effluents liquides qui se dégagent au cours du procédé et qui risquent à leur tour de polluer l'environnement.This process has the disadvantage of a step very fine grinding prerequisite, which requires installation very powerful, and therefore fixed. The process does not therefore does not solve the problems inherent in transport and waste storage, and it appears very expensive. Furthermore, nothing is planned with regard to vapors and liquid effluents released during of the process and which in turn risk polluting the environment.

    Dans le WO-A-94/08661, on décrit un procédé de traitement tel qu'indiqué au début. Ce procédé a uniquement pour but de réaliser des déchets qui puissent être déchargés dans un dépôt sans les risques inhérents à l'amiante. La seule installation décrite pour réaliser ce traitement est un centre de traitement fixe, de grande dimension, qui n'apporte donc aucune solution aux problèmes de transport et de stockage des déchets contenant de l'amiante. Enfin, pendant le traitement, les déchets subissent un compactage coûteux en énergie avant leur introduction dans la chambre de traitement. WO-A-94/08661 describes a method of treatment as indicated at the beginning. This process has only aim of producing waste that can be unloaded in a warehouse without the risks inherent in asbestos. The only installation described to realize this treatment is a fixed processing center, large dimension, which therefore provides no solution to waste transportation and storage issues containing asbestos. Finally, during treatment, waste undergoes energy-intensive compaction before their introduction into the treatment chamber.

    La présente invention a pour but de prévoir un procédé et une installation qui évitent les inconvénients précités et qui permettent un traitement des déchets sur le site générateur de tels déchets. Par site générateur de déchets il faut entendre non seulement un bâtiment dans lequel on démonte tous les éléments contenant de l'amiante, mais aussi par exemple un dépôt d'immondices où des sachets contenant de l'amiante ont été préalablement accumulés. Il est donc souhaitable que l'installation soit de petite dimension et transportable.The object of the present invention is to provide a process and installation which avoid the disadvantages mentioned above and which allow processing of waste on the site generating such waste. By site waste generator you have to hear not only a building in which we dismantle all the elements containing asbestos, but also for example a deposit rubbish where bags containing asbestos have been previously accumulated. It is therefore desirable that the installation is small and transportable.

    L'invention a en outre pour but d'éviter tout risque de pollution entre le site générateur et le réacteur qui va traiter les déchets, c'est-à-dire les risques de la mise en sachets des déchets et du transport de ces sachets vers un centre de traitement éloigné. La mise en sachet de débris de construction est malaisée et provoque très fréquement le percement de sachets, ce qui permet ensuite à l'amiante de se répandre dans l'atmosphère en dehors du site.The invention further aims to avoid any risk of pollution between the generating site and the reactor that will process the waste, i.e. risks of waste bagging and transport of these sachets to a remote processing center. The bagging of construction debris is awkward and very often causes the piercing of sachets, which then allows the asbestos to spread in the atmosphere outside the site.

    L'invention a aussi pour but d'empêcher au maximum toute sortie de produit intervenant dans le traitement, dans la mesure où il contient encore des fibres d'amiante. Les produits issus du traitement seront avantageusement ou recyclés ou aptes à une revalorisation.The invention also aims to prevent the maximum any product release occurring in the processing, insofar as it still contains asbestos fibers. Treatment products will be advantageously either recycled or suitable for revaluation.

    L'invention a enfin pour but d'éviter tout broyage, concassage ou compactage préalable à l'entrée dans le réacteur et donc une introduction dans celui-ci, sans triage, des substrats chargés d'amiante.The invention finally aims to avoid any crushing, crushing or compacting prior to entry in the reactor and therefore an introduction into it, without sorting, substrates loaded with asbestos.

    On résout ces problèmes, suivant l'invention, par un procédé tel que décrit au début, comprenant

    • un transfert des déchets contenant de l'amiante depuis le site générateur jusqu'à l'intérieur d'un réacteur de traitement, sans que les déchets ne soient en contact avec un milieu extérieur,
    • une alimentation du réacteur en solution basique d'attaque,
    • l'attaque susdite jusqu'à l'obtention dudit produit réactionnel, sans fibres,
    • une séparation du produit réactionnel en une phase solide et une phase liquide,
    • un recyclage de la phase liquide issue de la séparation et éventuellement d'un milieu gazeux soutiré du réacteur après l'attaque, pour une formation de la solution basique d'attaque,
    • une récupération de la phase solide issue de la séparation en vue d'une éventuelle revalorisation, et
    • une décharge hors du réacteur d'une faible quantité de déchets irrécupérables, ne contenant pas de fibres d'amiante,
      les étapes susdites étant effectuées dans un circuit sans sortie possible de fibres d'amiante vers l'extérieur, tout produit issu de ce circuit étant dépourvu de toute fibre d'amiante.
    These problems are solved, according to the invention, by a method as described at the beginning, comprising
    • transfer of waste containing asbestos from the generator site to the interior of a treatment reactor, without the waste being in contact with an external environment,
    • supplying the reactor with basic attack solution,
    • the above attack until said reaction product, without fibers, is obtained,
    • separation of the reaction product into a solid phase and a liquid phase,
    • recycling of the liquid phase resulting from the separation and optionally from a gaseous medium withdrawn from the reactor after the attack, for the formation of the basic attack solution,
    • recovery of the solid phase resulting from the separation with a view to possible revalorization, and
    • a discharge from the reactor of a small quantity of irrecoverable waste, not containing asbestos fibers,
      the aforementioned steps being carried out in a circuit without possible outlet of asbestos fibers to the outside, any product from this circuit being free of any asbestos fiber.

    Suivant un mode de réalisation avantageux de l'invention, le transfert a lieu dans un récipient amovible, fermé, et le procédé comprend en outre, pendant ou après le transfert, un lavage extérieur du récipient par un liquide de lavage. Cela permet d'éliminer les poussières d'amiante qui ont pu se déposer sur le récipient pendant sa présence dans le site générateur de déchets et donc de ne pas contaminer l'endroit, proche du site, où l'attaque basique va avoir lieu. De préférence, l'eau de lavage du récipient est recyclée dans la formation de solution basique d'attaque ce qui évite toute pollution de l'environnement à la sortie du récipient fermé hors du site générateur de déchets. According to an advantageous embodiment of the invention, the transfer takes place in a container removable, closed, and the method further comprises, during or after the transfer, an external washing of the container with washing liquid. This eliminates asbestos dust that may have settled on the container during its presence in the generating site of waste and therefore not to contaminate the place, near the site, where the basic attack will take place. Of preferably the container wash water is recycled in the formation of basic attack solution which avoids any pollution of the environment at the exit of the container closed off the waste generating site.

    Suivant un mode particulièrement avantageux de l'invention, le récipient amovible servant au transfert susdit est aussi le réacteur dans lequel se passe la réaction d'attaque. Il n'y a donc dans ce cas aucun risque de pollution par de l'amiante lors du transvasement d'un récipient dans un autre, les déchets sans triage sont directement introduits dans le réacteur au site générateur lui-même.According to a particularly advantageous mode of the invention, the removable container used for transfer aforementioned is also the reactor in which the attack reaction. There is therefore in this case no risk of asbestos pollution during transfer from one container to another, waste without sorters are directly introduced into the reactor at generator site itself.

    Suivant un mode de réalisation préféré de l'invention, la réaction d'attaque est effectuée avec la solution basique d'attaque à une température de l'ordre de 175 à 190°C et sous une pression d'environ 8 à 10 kg/cm2.According to a preferred embodiment of the invention, the attack reaction is carried out with the basic attack solution at a temperature of the order of 175 to 190 ° C and under a pressure of about 8 to 10 kg / cm 2 .

    Suivant un mode de réalisation perfectionné de l'invention, l'attaque comprend

    • une première attaque dans le réacteur par la solution basique d'attaque à une température et une pression permettant l'obtention d'un produit de désolidarisation des fibres d'amiante par rapport aux autres déchets,
    • une séparation du produit de désolidarisation susdit en une phase solide présentant un volume concentré par rapport aux déchets contenant de l'amiante transférés dans le réacteur et une phase liquide,
    • un recyclage de cette phase liquide pour la formation de la solution basique d'attaque,
    • une introduction de la phase solide de volume concentré, issue du produit de désolidarisation, dans un réacteur supplémentaire,
    • une deuxième attaque, dans le réacteur supplémentaire, de cette phase solide de volume concentré par la solution basique d'attaque, à une température et une pression suffisamment élevées pour obtenir ledit produit réactionnel sans fibres,
    • la température et la pression au cours de la première attaque ayant des valeurs inférieures à celles des température et pression appliquées lors de la deuxième attaque, et
    • un refroidissement dudit produit réactionnel avant sa séparation précitée. Ce mode de traitement permet dans une première étape de réduire le volume des déchets contenant de l'amiante. Par exemple les déchets d'amiante de flocage se présentent généralement, lors du démontage, sous une forme d'ouate dont le poids spécifique est de l'ordre de 150 à 300 g par litre. Au cours de la première attaque, effectuée à une température relativement modérée, on peut utiliser des réacteurs, par exemple des autoclaves, beaucoup moins lourds et surtout moins coûteux en raison de la faible pression mise en oeuvre. Dans la deuxième étape d'attaque, la phase solide traitée présente un volume réduit de 70% par rapport au volume des déchets mis en oeuvre dans la première attaque. Le deuxième réacteur utilisé peut alors soumettre cette phase solide à une température élevée, suffisante pour faire disparaítre les fibres d'amiante, sans devoir nécessairement atteindre dans ce deuxième réacteur, une pression exagérément élevée. On peut ainsi augmenter le rendement, en diminuant de manière drastique le coût des réacteurs amovibles. D'autres modes de réalisation du procédé suivant l'invention sont indiqués en particulier dans les revendications de procédé annexées.
    According to an improved embodiment of the invention, the attack comprises
    • a first attack in the reactor with the basic attack solution at a temperature and a pressure making it possible to obtain a product for separating the asbestos fibers from the other waste,
    • separation of the above-mentioned separation product into a solid phase having a concentrated volume with respect to the waste containing asbestos transferred to the reactor and a liquid phase,
    • recycling of this liquid phase to form the basic attack solution,
    • introduction of the solid phase of concentrated volume, obtained from the decoupling product, into an additional reactor,
    • a second attack, in the additional reactor, of this solid phase of concentrated volume with the basic attack solution, at a temperature and a pressure sufficiently high to obtain said reaction product without fibers,
    • the temperature and pressure during the first attack having values lower than those of the temperature and pressure applied during the second attack, and
    • cooling said reaction product before its aforementioned separation. This method of treatment allows in a first step to reduce the volume of waste containing asbestos. For example, flocking asbestos waste is generally present, during disassembly, in the form of a cotton wool whose specific weight is of the order of 150 to 300 g per liter. During the first attack, carried out at a relatively moderate temperature, reactors, for example autoclaves, which are much lighter and above all less expensive due to the low pressure used, can be used. In the second attack step, the solid phase treated has a volume reduced by 70% compared to the volume of waste used in the first attack. The second reactor used can then subject this solid phase to a high temperature, sufficient to cause the asbestos fibers to disappear, without necessarily having to reach in this second reactor, an excessively high pressure. It is thus possible to increase the yield, by drastically reducing the cost of the removable reactors. Other embodiments of the process according to the invention are indicated in particular in the appended process claims.

    Suivant l'invention, on a également résolu les problèmes posés avec une installation pour la mise en oeuvre du procédé suivant l'invention. Ces installations sont indiquées en particulier dans les revendications d'installation annexées.According to the invention, the problems with an installation for setting work of the process according to the invention. These facilities are indicated in particular in the claims installation instructions.

    D'autres détails et particularités de l'invention ressortiront de la description donnée ci-après, à titre non limitatif et avec référence aux dessins annexés.

  • Les figures 1 à 3 représentent ensemble d'une manière schématique une installation de traitement suivant l'invention.
  • La figure 4 représente une vue schématique, partiellement en coupe, d'une partie de l'installation suivant l'invention sur un plateau transportable sur remorque.
  • La figure 5 représente une vue schématique, partiellement en coupe, d'une autre partie de l'installation suivant l'invention sur un autre plateau transportable sur remorque.
  • La figure 6 représente de manière schématique, en combinaison avec les figures 1 et 3, une variante de réalisation d'installation de traitement suivant l'invention.
    • Other details and particularities of the invention will emerge from the description given below, without implied limitation and with reference to the attached drawings.
  • Figures 1 to 3 together show schematically a treatment installation according to the invention.
  • FIG. 4 represents a schematic view, partially in section, of a part of the installation according to the invention on a platform transportable on a trailer.
  • FIG. 5 represents a schematic view, partially in section, of another part of the installation according to the invention on another plate transportable on a trailer.
  • FIG. 6 schematically represents, in combination with FIGS. 1 and 3, an alternative embodiment of a treatment installation according to the invention.

    • Sur les différents dessins les éléments identiques ou analogues sont désignés par les mêmes références.On the different drawings the elements identical or analogous are designated by the same references.

    L'installation illustrée sur les figures 1 à 3 comprend un réacteur 1 sous la forme d'un autoclave obturable de manière étanche par un couvercle par exemple rabattable 2. Ce réacteur est prévu pour pouvoir supporter des pressions internes allant jusqu'à 10 kg/cm2. Il. est ici déplaçable sur un chariot 3 muni de roulettes 4. Cet ensemble est dimensionné de manière à pouvoir pénétrer dans des bâtiments, et donc pour pouvoir traverser des portes et entrer dans un ascenseur. Cela permet de remplir le réacteur 1 des déchets démontés dans le bâtiment, contenant des fibres d'amiante, sans tri ni broyage préalable. Une fois le réacteur rempli au site générateur de déchets même, et donc sans manipulation de sacs, le réacteur est sorti du bâtiment où les déchets sont démontés.The installation illustrated in FIGS. 1 to 3 comprises a reactor 1 in the form of an autoclave which can be sealed in a sealed manner by a cover, for example a flip-up cover. This reactor is designed to be able to withstand internal pressures of up to 10 kg / cm 2 . He. is here movable on a carriage 3 provided with rollers 4. This assembly is dimensioned so as to be able to enter buildings, and therefore to be able to pass through doors and enter an elevator. This makes it possible to fill the reactor 1 with waste dismantled in the building, containing asbestos fibers, without prior sorting or grinding. Once the reactor is filled at the waste generating site itself, and therefore without handling bags, the reactor is taken out of the building where the waste is dismantled.

    Il est alors de préférence amené à un poste d'arrosage 5 (figure 1) qui est doté d'une rampe d'arrosage 6 supérieure, alimentée en eau de préférence sous pression, et d'une cabine 7 dont le sol est aménagé en bassin de récolte 8 de l'eau de lavage, qui est alors chargée des poussières qui se sont accumulées sur le réacteur pendant son passage dans le site générateur de déchets, poussières qui contiennent probablement elles-mêmes des fibres d'amiante. L'eau de lavage récoltée est envoyée à une citerne collectrice 9, par l'intermédiaire d'un conduit de sortie 10, muni d'une pompe 11. La citerne 9 est, dans l'exemple de réalisation illustré, elle-même montée de manière à pouvoir être déplacée sur roues.He is then preferably brought to a post 5 (figure 1) which has a watering ramp 6 upper, preferably supplied with water under pressure, and a cabin 7, the floor of which is arranged in 8 wash water harvesting basin, which is then charged with the dust that has accumulated on the reactor during its passage through the generator site waste, dust which probably contains themselves asbestos fibers. The collected wash water is sent to a collecting tank 9, via an outlet conduit 10, fitted with a pump 11. The tank 9 is, in the illustrated embodiment, itself mounted so that it can be moved on wheels.

    Sur la figure 2, on peut voir la partie d'une installation suivant l'invention dans laquelle le contenu du réacteur est soumis à une attaque par une solution basique aqueuse.In Figure 2, we can see the part of a installation according to the invention in which the contents of the reactor is under attack by a basic aqueous solution.

    Le réacteur 1 a été transféré du chariot 3 sur un support 12 capable de basculer autour d'un arbre 13. Par un accouplement rapide 14, l'arbre de sortie d'un moteur rotatif 15 est accouplé à un agitateur installé d'une manière connue au tond du réacteur. Un moteur, non représenté, permet de faire tourner l'arbre 13 sur son axe et de basculer le réacteur. Toutes ces mesures permettent une agitation appropriée du contenu du réacteur pendant l'attaque.Reactor 1 was transferred from carriage 3 to a support 12 capable of tilting around a shaft 13. By a quick coupling 14, the output shaft of a rotary motor 15 is coupled to an installed agitator in a known manner at the bottom of the reactor. An engine, no shown, allows the shaft 13 to rotate on its axis and tilt the reactor. All these measures allow appropriate agitation of the contents of the reactor during the attack.

    Des raccords à connexion rapide permettent de relier le réacteur 1 à un conduit supérieur 16 et à un conduit inférieur 17, obturables chacun par un moyen de vanne.Quick connect fittings allow connect reactor 1 to an upper duct 16 and to a lower duct 17, each closable by means of valve.

    Dans l'exemple illustré, le conduit supérieur 16 est en communication avec une vanne à voies multiples 18. Selon l'ouverture commandée, la vanne 18 permet une entrée d'eau de rinçage dans le réacteur depuis le conduit 19 et/ou une entrée de solution basique d'attaque depuis le conduit 20. In the example illustrated, the upper duct 16 is in communication with a multi-way valve 18. Depending on the controlled opening, the valve 18 allows a entry of rinse water into the reactor from the conduit 19 and / or a basic attack solution inlet from line 20.

    Des éléments chauffants électriques 21 sont, dans l'exemple de réalisation illustré, prévus à l'intérieur du réacteur 1, et ils sont connectés à une source de courant lorsque le réacteur est en place sur le support 12.Electric heating elements 21 are, in the illustrated embodiment, provided inside from reactor 1, and they are connected to a source current when the reactor is in place on the support 12.

    L'attaque par la solution basique aqueuse peut donc avoir lieu dans le réacteur 1, sans sortie possible de fibres d'amiante vers l'extérieur. La solution basique d'attaque peut être par exemple une solution aqueuse d'agent générateur d'ions OH-, comme des bases alcalines ou alcalino-terreuses, notamment du NaOH 25 M en paillettes, obtenue par exemple par dissolution dans 0,5 partie en volume d'eau de 1 partie en volume de telles paillettes de NaOH. L'attaque a lieu de préférence à une température de 175 à 190°C et sous une pression de 8 à 10 kg/cm2, pendant une durée de 20 à 30 minutes, avantageusement sous lente agitation, éventuellement de manière intermittente. Après cette attaque, il n'y a sensiblement plus de fibres d'amiante dans le produit réactionnel qui est de consistance pâteuse. Ce produit réactionnel est sorti du réacteur 1 par le conduit inférieur 17, après ouverture de la vanne correspondante, et il est amené à une centrifugeuse courante 22. Ce transfert peut être suivi d'un rinçage intérieur du réacteur par apport d'eau de rinçage depuis le conduit 19.The attack with the aqueous basic solution can therefore take place in the reactor 1, without possible exit of asbestos fibers to the outside. The basic etching solution may for example be an aqueous solution of OH - ion generating agent, such as alkaline or alkaline-earth bases, in particular 25 M NaOH in flakes, obtained for example by dissolving in 0.5 part by volume of water of 1 part by volume of such NaOH flakes. The attack preferably takes place at a temperature of 175 to 190 ° C and under a pressure of 8 to 10 kg / cm 2 , for a period of 20 to 30 minutes, advantageously with slow stirring, optionally intermittently. After this attack, there is substantially no more asbestos fibers in the reaction product which is of pasty consistency. This reaction product is taken out of the reactor 1 by the lower pipe 17, after opening the corresponding valve, and it is brought to a running centrifuge 22. This transfer can be followed by an internal rinsing of the reactor by adding rinsing water. from conduit 19.

    Dans la centrifugeuse, de l'eau fraíche ou de rinçage peut encore être alimentée par un conduit d'entrée d'eau 23. La centrifugeuse permet de séparer dans le produit pâteux une phase liquide et un précipité solide. La phase liquide constituée principalement d'eau et de base d'attaque est récupérée au bas de la centrifugeuse pour être recyclée par un conduit de recyclage 24. Le précipité solide est envoyé par le conduit de sortie 25 dans un bac 26 à partir duquel une revalorisation de ce précipité pourra avoir lieu.In the centrifuge, fresh water or rinse can still be supplied by a conduit water inlet 23. The centrifuge separates in the pasty product a liquid phase and a precipitate solid. The liquid phase consisting mainly of water and attack base is recovered at the bottom of the centrifuge to be recycled through a recycling conduit 24. The solid precipitate is sent through the outlet 25 in a bin 26 from which a revaluation of this precipitate may take place.

    Selon la nature de l'amiante traitée on obtiendra des matières solides différentes. Dans le cas des amphiboles, on obtiendra un précipité de ferrate (hydroxyde de fer complexe) qui pourra être aménagé en fonction de son utilisation, en particulier comme floculant des métaux lourds dans les eaux industrielles ou dans des solutions hydrométallurgiques. Pour les autres types d'amiante, comme les chrysotiles, les précipités seront par exemple mélangés dans une composition à base de ciment, ou introduits comme adjuvants dans des matériaux réfractaires.Depending on the nature of the asbestos treated, will get different solids. In the case amphiboles, we will get a ferrate precipitate (complex iron hydroxide) which can be converted into depending on its use, especially as flocculating heavy metals in industrial waters or in hydrometallurgical solutions. For the other types of asbestos, such as chrysotiles, precipitates will for example be mixed in a composition based on cement, or introduced as adjuvants in refractory materials.

    Le réacteur 1, au moment de sa fermeture sur le site générateur, contient en plus des déchets introduits de l'air fortement chargé en poussières et donc en fibres d'amiante. Au cours de l'attaque, ces particules en suspension sont lavées et attaquées au même titre que les déchets solides, et les fibres d'amiante qui étaient en suspension sont donc aussi détruites.Reactor 1, when it closed on the generating site, contains in addition to the waste introduced air heavily loaded with dust and therefore asbestos fibers. During the attack, these particles in suspension are washed and attacked in the same way as solid waste, and asbestos fibers that were suspended are therefore also destroyed.

    Après fermeture du conduit 17, lorsque toute la masse pâteuse formant le produit réactionnel a quitté le réacteur, le conduit supérieur 16 est à nouveau ouvert, après avoir fermé les voies de la vanne multiple 18 menant aux conduits 19 et 20. Une troisième voie est alors ouverte qui communique avec un conduit à gaz 27 muni d'une pompe à vide 28. Le milieu gazeux présent dans le réacteur 1 est alors aspiré dans le conduit 28. Lorsqu'une légère dépression s'est établie dans le réacteur 1, la voie vers le conduit 27 est à son tour fermée, et la communication entre le conduit 16 et le réacteur 1 peut être obturée.After closing line 17, when all the pasty mass forming the reaction product has left the reactor, the upper pipe 16 is again open, after closing the multiple valve channels 18 leading to conduits 19 and 20. A third path is then open which communicates with a gas pipe 27 fitted with a vacuum pump 28. The gaseous medium present in reactor 1 is then sucked into line 28. When a slight depression has established in the reactor 1, the route to line 27 is in turn closed, and the communication between the conduit 16 and the reactor 1 can be closed.

    Le couvercle 2 du réacteur 1 peut alors être ouvert sans aucun danger de pollution de l'environnement. Les débris qui ont été introduits avec les déchets d'amiante sur le site générateur, par exemple des briques, des morceaux de bois, etc....., peuvent alors être déchargés en basculant le réacteur, et éventuellement en raclant l'intérieur. Ces débris, complètement dépourvus de fibres d'amiante, peuvent alors être acheminés vers un dépôt ou une autre destination.The cover 2 of the reactor 1 can then be open without any danger of environmental pollution. Debris that has been introduced with the waste asbestos on the generating site, for example bricks, pieces of wood, etc ....., can then be discharged by tilting the reactor, and possibly scraping the interior. This debris, completely free of asbestos fibers, can then be routed to a depot or other destination.

    Sur la figure 3, on a représenté la partie de l'installation servant à la formation de la solution basique d'attaque suivant l'invention.In Figure 3, the part of the installation used to form the solution basic attack according to the invention.

    Dans l'exemple illustré, l'installation comprend une cuve de préparation de solution 29, capable de résister à une pression de 10 kg/cm2 et susceptible d'être chauffée par exemple par une chemise chauffante 30 dans laquelle circule un fluide thermique, notamment de l'huile. Le fluide thermique entre en 31 dans la chemise 30 et en sort en 32.In the example illustrated, the installation comprises a solution preparation tank 29, capable of withstanding a pressure of 10 kg / cm 2 and capable of being heated for example by a heating jacket 30 in which a thermal fluid circulates, including oil. The thermal fluid enters at 31 into the jacket 30 and exits at 32.

    Les paillettes de soude caustique sont alimentées par le haut en 33 dans la cuve 29, à partir d'un silo 34 et en passant par une vis transporteuse 35.Caustic soda flakes are fed from above at 33 in tank 29, from a silo 34 and passing through a conveyor screw 35.

    De l'eau fraíche ou de rinçage peut être fournie dans la cuve 29 par le conduit d'entrée 36. Un conduit de sortie 37 de la solution basique d'attaque permet de prélever celle-ci au fond de la cuve 29, à l'aide d'une pompe 38. Ce conduit de sortie 37 est en communication avec le conduit 20 précédemment mentionné (voir figure 2) par une vanne 39 qui est ouverte lorsque le réacteur 1 doit être alimenté en solution basique d'attaque. Lorsque la vanne 39 est fermée, la solution basique d'attaque est recyclée au haut de la cuve 29 par une dérivation 40, à l'aide d'un mélangeur statique 41. Dans cette cuve la solution basique est amenée à la concentration souhaitée, à une température proche de l'ébullition, par exemple de 120°C.Fresh or rinse water may be supplied in the tank 29 by the inlet duct 36. A outlet conduit 37 of the basic etching solution allows the latter to be taken from the bottom of the tank 29, using a pump 38. This outlet duct 37 is in communication with conduit 20 previously mentioned (see Figure 2) by a valve 39 which is open when reactor 1 must be supplied with basic solution of attack. When valve 39 is closed, the solution basic attack is recycled at the top of the tank 29 by a bypass 40, using a static mixer 41. In this tank the basic solution is brought to the desired concentration, at a temperature close to boiling, for example 120 ° C.

    Dans l'exemple illustré, l'installation comprend également, d'une manière avantageuse, une cuve d'égalisation 42 de la solution basique d'attaque. Cette cuve est capable de préférence de résister à une pression de 5 kg/cm2, et elle est susceptible d'être faiblement chauffée par exemple par une chemise chauffante 43 dans laquelle circule un fluide thermique, notamment de l'huile. Le fluide thermique entre on 44 dans la chemise 43 et on sort on 45.In the example illustrated, the installation also advantageously comprises an equalization tank 42 for the basic attack solution. This tank is preferably capable of withstanding a pressure of 5 kg / cm 2 , and it is capable of being slightly heated, for example by a heating jacket 43 in which a thermal fluid, in particular oil, circulates. The thermal fluid enters 44 in the jacket 43 and exits 45.

    Les paillettes de soude caustique sont alimentées par le haut en 46 dans la cuve 42, à partir du silo 34 et en passant par une vis transporteuse 47.Caustic soda flakes are fed from above at 46 in tank 42, from the silo 34 and passing through a conveyor screw 47.

    De l'eau fraíche ou de rinçage peut être introduite dans la cuve 42 par le conduit d'entrée 48. Un conduit de sortie 49 de la solution basique d'égalisation permet de prélever celle-ci au fond de la cuve 42, à l'aide d'une pompe 50. Ce conduit de sortie 49 est on communication avec un conduit d'alimentation 51, par une vanne 52. Ce conduit d'alimentation 51 permet d'introduire au haut de la cuve de préparation 29 une solution basique d'égalisation et d'obtenir ainsi une solution basique d'attaque de composition uniforme. Lorsque la vanne 52 est fermée, la solution basique d'égalisation est recyclée au haut de la cuve 42 par une dérivation 53, à l'aide d'un mélangeur statique 54.Fresh or rinse water may be introduced into the tank 42 through the inlet conduit 48. An outlet conduit 49 of the basic equalization solution allows to take it from the bottom of the tank 42, using a pump 50. This outlet duct 49 is there is communication with a supply duct 51, by a valve 52. This supply duct 51 allows introduce at the top of the preparation tank 29 a basic equalization solution and thus get a basic attack solution of uniform composition. When valve 52 is closed, the basic solution equalization is recycled to the top of the tank 42 by a bypass 53, using a static mixer 54.

    Dans cette cuve 42, la phase liquide séparée dans la centrifugeuse est amenée par le conduit 24 (voir figure 2), ce qui permet de récupérer une part importante de la solution basique d'attaque ayant déjà servi. Le conduit 27, par lequel le milieu gazeux du réacteur 1 sort après l'attaque, débouche lui aussi au haut de la cuve d'égalisation 42. Enfin, la citerne collectrice 9 (voir figure 1) peut aussi être mise en communication avec la cuve 42, par le conduit 55, pour y introduire l'eau du lavage extérieur du réacteur 1. On peut aussi prévoir, suivant une autre forme de réalisation, que l'eau du rinçage intérieur du réacteur soit directement recyclée dans le conduit de recyclage 24 sans passer par la centrifugeuse. Dans ce milieu formé de liquides et de gaz de diverses provenances, la base d'attaque est dissoute à température basse jusqu'à atteindre le seuil de saturation.In this tank 42, the separated liquid phase into the centrifuge is brought through line 24 (see figure 2), which makes it possible to recover a large proportion of the basic attack solution which has already served. Line 27, through which the gaseous medium of the reactor 1 comes out after the attack, also leads to the top of the equalization tank 42. Finally, the collecting tank 9 (see figure 1) can also be connected with the tank 42, through the conduit 55, to introduce there the wash water outside the reactor 1. We can also provide, according to another embodiment, that the water inside the reactor rinsing either directly recycled in recycling conduit 24 without passing through the centrifuge. In this environment formed by liquids and gases from various sources, the base of attack is dissolved at low temperature until reaching the threshold saturation.

    Comme on peut le constater, dans cette installation, tous les réactifs sont introduits dans un circuit d'une manière étanche vis-à-vis de l'atmosphère, et tous les effluents liquides et gazeux sont recyclés. Il ne sort du procédé mis en oeuvre dans cette installation qu'un produit réactionnel solide revalorisable et des débris non attaquables par la solution basique d'attaque. Ces deux produits de sortie ne contiennent pas de fibres d'amiante après analyse.As we can see, in this installation, all the reagents are introduced into a circuit in a sealed manner vis-à-vis the atmosphere, and all liquid and gaseous effluents are recycled. It does not leave the process implemented in this installation that a revalorizable solid reaction product and debris not attackable by the basic solution of attack. These two output products do not contain no asbestos fibers after analysis.

    Sur la figure 4, on a représenté l'agencement sur un plateau 56, transportable par remorque, de la partie de formation de la solution basique d'attaque de l'installation.In Figure 4, there is shown the arrangement on a platform 56, transportable by trailer, training part of the basic attack solution the installation.

    Les cuves 29 et 42 de la figure 3 sont supportées sur le plateau 56. A côté de ces cuves se trouve un dispositif courant de chauffage de fluide thermique avec une cuve à fluide thermique 57 et une chaudière 58.The tanks 29 and 42 of Figure 3 are supported on tray 56. Next to these tanks is a current thermal fluid heating device with a thermal fluid tank 57 and a boiler 58.

    Sur la figure 5, on a représenté une batterie de réacteurs 1 supportés sur un plateau 64 transportable par remorque. Dans cet exemple de réalisation les réacteurs sont introduits dans une enceinte chauffée 59, dont la partie supérieure peut être ouverte pour l'introduction ou l'extraction du réacteur 1. Cette opération est effectuée à l'aide d'un dispositif de levage connu en soi 60. L'enceinte chauffée 59 est supportée sur deux bouts d'arbre 65 et 66 coaxiaux de manière à pouvoir tourner autour de leur axe. Une agitation de 40 à 50 tours par minute est par exemple favorable.In Figure 5, a battery is shown of reactors 1 supported on a transportable tray 64 by trailer. In this exemplary embodiment the reactors are introduced into a heated enclosure 59, the upper part of which can be opened for insertion or the extraction of reactor 1. This operation is carried out using a lifting device known per se 60. The heated enclosure 59 is supported on two ends of the shaft 65 and 66 coaxial so as to be able to rotate around their axis. An agitation of 40 at 50 rpm is for example favorable.

    Le réacteur de gauche sur la figure 5 est alimenté par un récipient amovible en forme de bac 61, dont la paroi supérieure 62 peut être ouverte pour l'introduction des déchets sur le site générateur. Le fond de ce bac 61, prévu transportable et déplaçable entre le site générateur et l'unité transportable de traitement suivant l'invention, est formé d'une trémie 63 obturable par un tiroir, non représenté. De même, l'ouverture supérieure du réacteur est alors fermée par un couvercle à tiroir correspondant. Lorsque les deux tiroirs sont ouverts, les déchets du bac 61 peuvent s'écouler dans le réacteur 1, de manière à ne pas pouvoir entrer en contact avec le milieu environnant.The left reactor in Figure 5 is supplied by a removable container in the form of a tray 61, whose upper wall 62 can be opened for the introduction of waste on the generating site. The bottom of this tank 61, provided for transportable and displaceable between the generating site and the transportable unit of treatment according to the invention, is formed by a hopper 63 closable by a drawer, not shown. Likewise, the upper opening of the reactor is then closed by a corresponding drawer cover. When the two drawers are open, waste from bin 61 can flow into reactor 1, so as not to be able to come into contact with the surrounding environment.

    A côté des réacteurs 1, la centrifugeuse 22 est installée. Les deux plateaux 56 et 64 peuvent être installés côte à côte et pour permettre une communication entre les différents récipients par les conduits cités ci-dessus.Next to the reactors 1, the centrifuge 22 is installed. The two plates 56 and 64 can be installed side by side and to allow communication between the different containers by the conduits cited above.

    Il doit être entendu que la présente invention n'est en aucune façon limitée aux formes de réalisation décrites ci-dessus et que bien des modifications peuvent y être apportées sans sortir du cadre des revendications ci-après.It should be understood that the present invention is in no way limited to the embodiments described above and that many modifications can be made without departing from the scope of the claims below.

    On peut par exemple concevoir que l'installation doive procéder au traitement de déchets contenant de l'amiante déjà ensachés et abandonnés dans un dépôt, ou des déchets du type tapis, feutres, etc.... Dans ce cas, il peut être avantageux de prévoir un déchiquetage mécanique des déchets. Celui-ci peut avoir lieu suivant l'invention à l'intérieur du réacteur 1, en introduisant dans celui-ci quelques fragments d'acier inoxydable. On peut aussi pourvoir la surface interne du réacteur d'éléments de déchiquetage, par exemple en forme de petits crochets.We can for example imagine that the installation must process waste containing asbestos already bagged and abandoned in a repository, or waste such as carpets, felts, etc. In this case, it may be advantageous to provide a shredding mechanical waste. This can take place according to the invention inside reactor 1, by introducing in it some fragments of stainless steel. We can also fill the internal surface of the reactor shredding elements, for example in the form of small hooks.

    Sur la figure 6, on a illustré une variante de réalisation perfectionnée de l'installation suivant l'invention, où le réacteur 1 formé d'un autoclave à haute pression de l'installation suivant les figures 1 à 3 est remplacé par deux réacteurs successifs : 1°) un réacteur amovible 1' par exemple sous la forme d'un autoclave de petite dimension et capable de fonctionner sous une pression extrêmement modérée et 2°) un réacteur fixe 1''. Des autoclaves correspondant aux exigences du réacteur amovible 1' sont ceux utilisés couramment dans des laboratoires de chimie, et ils sont aisément disponibles sur le marché à un coût modéré. Ces autoclaves présentent l'avantage supplémentaire de pouvoir être prévus beaucoup moins lourds et moins résistant à la pression, en raison de la faible pression mise en oeuvre.In FIG. 6, a variant of improved installation of the following installation the invention, where the reactor 1 formed from an autoclave at high pressure of the installation according to Figures 1 at 3 is replaced by two successive reactors: 1) a removable reactor 1 'for example in the form a small autoclave capable of operating under extremely moderate pressure and 2 °) a 1 '' fixed reactor. Autoclaves corresponding to requirements of the removable reactor 1 'are those used commonly in chemistry labs, and they're readily available on the market at moderate cost. These autoclaves have the added benefit of can be expected to be much lighter and less pressure resistant, due to low pressure Implementation.

    Les déchets contenant de l'amiante sont introduits dans le réacteur 1' comme dans le réacteur 1 de la figure 1 et celui-ci est avantageusement lavé de la même manière à la sortie du site générateur de déchets. Il est ensuite relié à un conduit supérieur 16' qui permet de le mettre en communication avec la cuve de préparation 29 de la solution basique d'attaque.Waste containing asbestos is introduced into reactor 1 'as in reactor 1 of Figure 1 and it is advantageously washed with the same way when leaving the generator site waste. It is then connected to an upper conduit 16 ' which allows to put it in communication with the tank of preparation 29 of the basic attack solution.

    Il est connu qu'une solution de NaOH à 100% (25 molaires) provoque un dégagement de vapeur uniquement à partir de 180°C. Si une température inférieure à celle-ci est maintenue dans le réacteur 1' par l'élément chauffant 21', la pression n'augmente pas de manière notable dans le réacteur 1', alors que l'action de la soude permet de désolidariser les différents déchets solides. Les déchets d'amiante provenant de flocage ou d'industrie se présentent au départ sous une forme d'ouate dont le poids spécifique est compris entre 150 et 300g par litre, ce qui a pour conséquence un grand volume à traiter pour peu d'amiante éliminée.It is known that a 100% NaOH solution (25 molars) only gives off steam from 180 ° C. If a temperature below this is maintained in the reactor 1 'by the element heating 21 ', the pressure does not increase so notable in reactor 1 ', while the action of soda allows to separate the different wastes solid. Asbestos waste from flocking or of industry are initially presented in a form wadding whose specific weight is between 150 and 300g per liter, which results in a large volume to be treated for little asbestos eliminated.

    On prévoit par exemple un traitement des déchets dans le réacteur 1' par la solution basique d'attaque à une température de 160 à 175°C, avantageusement de 170°C, pendant 15 minutes.For example, treatment of waste in reactor 1 'with the basic solution attack at a temperature of 160 to 175 ° C, advantageously at 170 ° C for 15 minutes.

    Le produit réactionnel est alors transféré par un conduit 17' à une première centrifugeuse 22' où la phase liquide est séparée de la phase solide. La phase liquide est recyclée par le conduit 24' à la cuve de préparation 29 ou à la cuve d'égalisation 42.The reaction product is then transferred by a conduit 17 'to a first centrifuge 22' where the liquid phase is separated from the solid phase. The sentence liquid is recycled through line 24 'to the tank preparation 29 or to the equalization tank 42.

    La phase solide se présente sous la forme d'une pâte qui contient encore des fibres d'amiante, totalement désolidarisées. Après analyse, on a déjà pu estimer que, dans cet état, les fibres obtenues ne représentent déjà plus de danger pour la santé humaine. Cette phase solide présente à présent un volume réduit de 70% par rapport à celui introduit dans le réacteur 1'. On l'amène, par un conduit 25', au réacteur 1''. Celui-ci est un réacteur fixe, c'est-à-dire qui n'a plus besoin d'être déplacé vers le site générateur de déchets, et il est pourtant d'un petit volume. On peut prévoir qu'il soit agencé horizontalement en vue de pouvoir être entraíné en rotation autour d'un axe horizontal.The solid phase is in the form a paste which still contains asbestos fibers, totally separated. After analysis, we have already been able estimate that, in this state, the fibers obtained do not already pose more danger to human health. This solid phase now has a reduced volume 70% compared to that introduced into the reactor 1 '. It is brought, via a pipe 25 ', to the reactor 1' '. This is a fixed reactor, that is to say which no longer has need to be moved to the waste generating site, and yet it is of a small volume. We can provide that it is arranged horizontally in order to be able to rotate around an axis horizontal.

    La solution basique d'attaque est introduite par le conduit 16'' et une température supérieure à 180°C, par exemple de 190 à 210°C, avantageusement d'environ 200°C, est maintenue dans le réacteur 1'' par une source de chaleur 21''. Il y a alors décomposition et disparition totale des fibres d'amiante, et formation d'une pression à l'intérieur du réacteur. Toutefois, comme le volume traité de phase solide est réduit, une pression de 2,5 kg à 10 kg/cm2, de préférence de 2,5 à 5 kg/cm2, peut suffire.The basic etching solution is introduced through the 16 '' conduit and a temperature above 180 ° C, for example from 190 to 210 ° C, advantageously around 200 ° C, is maintained in the 1 '' reactor by a 21 '' heat source. There is then decomposition and total disappearance of the asbestos fibers, and formation of a pressure inside the reactor. However, since the treated volume of solid phase is reduced, a pressure of 2.5 kg to 10 kg / cm 2 , preferably 2.5 to 5 kg / cm 2 , may suffice.

    Le produit réactionnel est alors transféré dans une deuxième centrifugeuse 22'' par le conduit 17'', en passant par un dispositif de refroidissement 70. Ici, la température du produit issu du réacteur 1'' est descendue en dessous de la température à laquelle la soude se vaporise, c'est-à-dire environ 180°C. Dans cette centrifugeuse il y a séparation de la phase liquide et de la phase solide. La phase liquide est recyclée par le conduit 24'' vers les cuves de préparation et/ou d'égalisation de la solution basique d'attaque et la phase solide est amenée par le conduit 25'' au bac 26.The reaction product is then transferred in a second centrifuge 22 '' through the conduit 17 '', passing through a cooling device 70. Here, the temperature of the product from the 1 '' reactor is dropped below the temperature at which the soda vaporizes, i.e. around 180 ° C. In this centrifuge there is phase separation liquid and solid phase. The liquid phase is recycled through the 24 '' pipe to the preparation tanks and / or equalization of the basic attack solution and the solid phase is brought through the 25 '' conduit to the tray 26.

    Les conduits 16' et 16'', peuvent, comme le conduit 16 sur la figure 2, servir de moyens de recyclage du milieu gazeux issu du réacteur respectif vers la source de solution basique d'attaque.The 16 'and 16' 'conduits can, like the conduit 16 in FIG. 2, serve as recycling means gaseous medium from the respective reactor to the source of basic attack solution.

    En résumé, on peut énumérer quelques avantages principaux du procédé et de l'installation suivant l'invention :

    • La sécurité est augmentée par la suppression du transport entre site générateur et usine de traitement et par l'absence de tout emballage des déchets ce qui évite tout risque dû à un déchirement des sacs,
    • La fermeture et le lavage des réacteurs avant leur sortie des sites générateurs d'amiante et l'absence de réouverture des réacteurs avant destruction de l'amiante.
    • La simplicité d'emploi.
    • L'absence de la nécessité de trier, de broyer ou de concasser les gravats à introduire dans les réacteurs.
    • La destruction totale des fibres d'amiante à un coût relativement bas.
    • La revalorisation de matières qui deviendront commercialisables et le recyclage des liquides et des gaz, ce qui évite tout rejet dans l'air ou toute évacuation dans les égouts ou le sol.
    In summary, some main advantages of the process and the installation according to the invention can be listed:
    • Safety is increased by the elimination of transport between the generator site and the treatment plant and by the absence of any packaging of the waste, which avoids any risk due to tearing of the bags,
    • The closure and washing of the reactors before they leave asbestos-generating sites and the absence of reopening of the reactors before destruction of the asbestos.
    • Ease of use.
    • The absence of the need to sort, grind or crush the rubble to be introduced into the reactors.
    • Total destruction of asbestos fibers at a relatively low cost.
    • The revalorization of materials which will become marketable and the recycling of liquids and gases, which avoids any release into the air or any evacuation in the sewers or the ground.

    Claims (26)

    1. Process for the treatment of waste containing asbestos, originating from a site generating such waste, including a reaction by digestion of the said waste with a basic solution until a reaction product without asbestos fibres is obtained,
      characterized in that it includes
      a transfer of the waste containing asbestos from the generating site to the interior of a treatment reactor, without the waste being in contact with an external medium,
      feeding the reactor with basic digestion solution,
      the abovementioned digestion until the said reaction product is obtained without fibres,
      separation of the reaction product into a solid phase and a liquid phase,
      recycling of the liquid phase resulting from the separation and optionally of a gaseous mixture drawn off from the reactor after digestion, in order to form the basic digestion solution,
      recovery of the solid phase resulting from the separation with a view to an optional reclaiming, and
      discharge out of the reactor of a small quantity of a irrecoverable waste containing no asbestos fibres,
      the abovementioned stages being carried out in a circuit without any possible outward release of asbestos fibres, any product resulting from this circuit being devoid of any asbestos fibre.
    2. Process in accordance with Claim 1, characterized in that the transfer takes place in a dosed, removable receptacle and in that the process additionally includes, during or after the transfer, an external washing of the receptacle with a washing liquid.
    3. Process in accordance with either of Claims 1 and 2, characterized in that the transfer takes place in the said reactor, as a removable receptacle.
    4. Process in accordance with either of Claims 2 and 3, characterized in that it includes a recovery of the said washing liquid and its recycling for the said formation of the basic digestion solution.
    5. Process in accordance with any one of Claims 1 to 4, characterized in that, during the said digestion, it includes an agitation of the waste in the reactor and optionally a simultaneous shredding thereof.
    6. Process in accordance with any one of Claims 1 to 5, characterized in that the said separation includes, in a manner which is leakproof with regard to the outside, a removal of the reaction product out of the reactor and centrifuging of the removed product, as well as optionally an internal rinsing of the reactor with a rinsing liquid which is then brought to the centrifuging of directly to the formation of the basic digestion solution.
    7. Process in accordance with any one of Claims 1 to 6, characterized in that the basic digestion solution contains water as solvent and a water-soluble agent generating OH- ions, especially an alkaline or alkaline-earth base, preferably NaOH or KOH.
    8. Process in accordance with claim 7, characterized in that the formation of basic digestion solution includes dissolving the agent generating OH- ions in water at a temperature of the order of 100 to 130°C, preferably at 120°C.
    9. Process in accordance with claim 8, characterized in that the formation of basic digestion solution additionally includes dissolving the agent generating OH- ions in cold or lukewarm water to form an equalizing solution which is then brought to the said dissolving at a temperature of the order of 100 to 130°C.
    10. Process in accordance with any one of Claims 1 to 9, characterized in that the digestion reaction is performed with an aqueous digestion solution of NaOH at a temperature of the order of 175 to 190°C and at a pressure of approximately 8 to 10 kg/cm2.
    11. Process in accordance with any one of Claims 1 to 9, characterized in that the digestion includes
      a first digestion in the reactor with the basic digestion solution at a temperature and a pressure which make it possible to obtain a product of disassociation of the asbestos fibres from the other waste,
      a separation of the abovementioned product of disassociation into a solid phase which is concentrated in volume in relation to the waste containing asbestos and transferred into the reactor and a liquid phase,
      recycling of this liquid phase for the formation of the basic digestion solution,
      introduction of the solid phase concentrated in volume, originating from the product of disassociation, into an additional reactor,
      a second digestion, in the additional reactor, of this solid phase concentrated in volume with the basic digestion solution at a temperature and a pressure which are sufficiently raised to obtain the said reaction product without fibres,
      the temperature and the pressure during the first digestion having lower values than the temperature and pressure values applied during the second digestion, and
      cooling of the said reaction product before its abovementioned separation.
    12. Process in accordance with Claim 11, characterized in that the first digestion is performed with an aqueous digestion solution of NaOH at a temperature lower than 180°C, preferably of the order of 160 to 175°C, advantageously of approximately 170°C, in that the second digestion is performed with an aqueous digestion solution of NaOH at a temperature higher than 180°C, preferably of the oder of 190° to 210°C, advantageously of approximately 200°C, at a pressure of 2 to 10 kg/cm2, preferably of 2.5 to 5 kg/cm2, and in that the cooling is performed to a temperature lower than 180°C.
    13. Process in accordance with one of Claims 1 to 12, characterized in that the liquid phase resulting from the separation, the gas mixture drawn from the reactor, a liquid from external washing of the reactor and optionally a liquid from internal rinsing of the reactor and a liquid phase resulting from a separation of a product of disassociation of the asbestos fibres from the other waster, are brought to a dissolving of an agent generating OH- ions in cold or lukewarm water, in order to form the basic digestion solution.
    14. Plant for implementing a process in accordance with any one of Claims 1 to 13,
      characterized in that it includes
      a reactor (1; 1', 1''),
      a transfer unit (1, 1', 62) permitting the said transfer of the waste within the reactor (1; 1', 1'') without the waste being in contact with the outside medium,
      a source (29, 42) of the basic digestion solution, connected to the reactor (1; 1', 1''),
      a separator (22; 22', 22'') connected to the reactor (1; 1', 1'') and capable of separating the reaction product into a solid phase and a liquid phase,
      a conduit for recycling (24; 24', 24'') the liquid phase resulting from the separator towards the source (29, 42) of the basic digestion solution,
      optionally means for recycling (16; 16', 16'', 27, 28) the gas mixture from the reactor (1; 1', 1'') towards the source (29, 42) of basic digestion solution, and
      an exit (25; 25', 25'', 26) for the solid phase resulting from the separator (22; 22', 22'').
    15. Plant in accordance with Claim 14, characterized in that the transfer unit is a removable trough (62) which is filled with waste at the generating site and in that the reactor (1) includes an opening through which the waste containing asbestos from the removable trough (62) can be introduced in a leakproof manner into the reactor (1) without the waste coming into contact with the external medium, and a lid (2) capable of closing this opening.
    16. Plant in accordance with Claim 14, characterized in that the transfer unit is the reactor (1, 1'), which is arranged in a removable manner, and in that the reactor (1, 1') includes an opening through which the waste contaning asbestos can be introduced into the reactor at the generating site and a lid (2) capable of dosing this opening.
    17. Plant in accordance with one of Claims 14 to 16, characterized in that it additionally includes a device for external washing (5) of the transfer unit (1,1', 62) and a device for collecting (7, 8, 9) the aqueous wash, connected to the source (29, 42) of basic digestion solution so as to recycle thereto the said aqueous wash.
    18. Plant in accordance with any one of Claims 14 to 17, characterized in that, during the digestion, the reactor is supported on a framework so as to be capable of being subjected to an agitating motion.
    19. Plant in accordance with any one of Claims 14 to 18, characterized in that it includes a source of heat (21, 59) capable of heating the basic digestion solution in the reactor to a temperature of the order of 175 to 190°C and in that the reactor (1) is capable of withstanding a pressure of the order of 10 kg/cm2.
    20. Plant in accordance with any one of Claims 14 to 18, characterized in that it includes a source of heat (21') capable of heating the basic digestion solution in the reactor (1') in such a manner that a temperature and a pressure are obtained which make it possible to obtain a product of disassociation of the asbestos fibres from the other waste, an intermediate separator (22') separating said product of disassociation in a solid phase which is concentrated in volume in relation to the waste containing asbestos and transferred into the reactor (1') and a liquid phase, a conduit for additional recycling (24') of the liquid phase obtained towards the source of basic digestion solution, an additional reactor (1'') into which the solid phase concentrated in volume is introduced, an additional source of heat (21'') capable of heating the basic digestion solution in the additional reactor (1'') in such a manner that a temperature and a pressure are obtained which are sufficient to obtain a reaction product without fibres, the temperature and the pressure in the reactor (1') having values lower than the temperature and pressure values applied within the additional reactor (1''), the abovementioned separator (22'') being connected to the reactor (1') through the intermediacy of the intermediate separator (22') and of the additional reactor (1''), and a device for cooling (70) the said reaction product leaving the additional reactor (1'').
    21. Plant in accordance with Claim 20, characterized in that the source of heat (21') is capable of heating the basic digestion solution in the reactor (1') to a temperature lower than 180°C, preferably of the order of 160 to 175°C, advantageously of approximately 170°C, and in that the additional source of heat (21'') is capable of heating the basic digestion solution in the additional reactor (1'') to a temperature higher than 180°C, preferably of the order of 190 to 210°C, advantageously of approximately 200°C, the additional reactor (1'') being capable of withstanding a pressure of 2 to 10 kg/cm2, preferably of 2.5 to 5 kg/cm2.
    22. Plant in accordance with Claim 19, characterized in that the source of heat includes a circulation of hot oil in a jacket enclosure (59) surrounding the reactor.
    23. Plant in accordance with any one of Claims 14 to 22, characterized in that the source of basic digestion solution includes a preparation vessel (29) into which the agent generating OH- ions, and a solvent, preferably water, are introduced, and a source of heat (30) enabling this solution to be heated to a temperature of the order of 100 to 120°C.
    24. Plant in accordance with Claim 23, characterized in that the source of basic solution additionally includes an equalizing vessel (42) into which are introduced the agent generating OH- ions, and a solvent, preferably water, as well as the liquid phase resulting from the separator (22), the gas mixture taken from the reactor (1; 1', 1'') after the digestion, a liquid from external washing of the reactor and optionally a liquid from internal rinsing of the reactor, as well as a liquid phase resulting from a separation of a product of disassociation of the asbestos fibres in relation to other waste.
    25. Plant in accordance with any one of Claims 14 to 24, characterized in that the separator (22; 22', 22'') is a centrifuge.
    26. Plant in accordance with any one of Claims 14 to 25, characterized in that it is supported on one of more base plates (56, 64) capable of movement by road.
    EP96915921A 1995-06-16 1996-06-10 Method and plant for processing asbestos-containing waste Expired - Lifetime EP0846016B1 (en)

    Applications Claiming Priority (5)

    Application Number Priority Date Filing Date Title
    BE9500536A BE1009413A6 (en) 1995-06-16 1995-06-16 Elimination of asbestos fibres - economical, ecological, recycling method
    BE9500536 1995-06-16
    BE9500911 1995-11-06
    BE9500911A BE1009724A6 (en) 1995-11-06 1995-11-06 Method and installation to treat waste containing asbestos
    PCT/BE1996/000056 WO1997000099A1 (en) 1995-06-16 1996-06-10 Method and plant for processing asbestos-containing waste

    Publications (2)

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    EP0846016A1 EP0846016A1 (en) 1998-06-10
    EP0846016B1 true EP0846016B1 (en) 1999-12-29

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    EP96915921A Expired - Lifetime EP0846016B1 (en) 1995-06-16 1996-06-10 Method and plant for processing asbestos-containing waste

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    EP (1) EP0846016B1 (en)
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    EA (1) EA199800066A1 (en)
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    JP5192649B2 (en) * 2006-02-23 2013-05-08 一般財団法人ファインセラミックスセンター Asbestos processing method, recycled material derived from asbestos, and manufacturing method thereof
    JP6224376B2 (en) * 2012-08-16 2017-11-01 学校法人北里研究所 Asbestos detoxification treatment method
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    FR3026032B1 (en) * 2014-09-22 2020-10-30 Paul Poggi MOBILE ASBESTOS NEUTRALIZATION UNIT
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    FR3070282B1 (en) * 2017-08-24 2019-09-06 Universite De Montpellier METHOD FOR DESTRUCTION AND VALORIZATION OF AMIANT WASTE
    CN109553385B (en) * 2018-12-19 2021-09-21 西南科技大学 Chrysotile tailing ceramsite and preparation method thereof

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    EP0846016A1 (en) 1998-06-10
    AU704269B2 (en) 1999-04-15
    GR3032632T3 (en) 2000-05-31
    DE69605927T2 (en) 2000-06-15
    PL324011A1 (en) 1998-04-27
    WO1997000099A1 (en) 1997-01-03
    JP3776935B2 (en) 2006-05-24
    CA2225523C (en) 2011-03-01
    PL182770B1 (en) 2002-02-28
    ES2142064T3 (en) 2000-04-01
    IL122613A0 (en) 1998-08-16
    CZ290478B6 (en) 2002-07-17
    HU225596B1 (en) 2007-05-02
    CA2225523A1 (en) 1997-01-03
    JPH11507585A (en) 1999-07-06
    ATE188134T1 (en) 2000-01-15
    AU5888696A (en) 1997-01-15
    DK0846016T3 (en) 2000-05-15
    CZ403497A3 (en) 1998-07-15
    EA199800066A1 (en) 1998-08-27
    DE69605927D1 (en) 2000-02-03
    HUP9901933A2 (en) 1999-09-28
    IL122613A (en) 2001-08-26
    US6391271B1 (en) 2002-05-21
    PT846016E (en) 2000-06-30
    NZ308981A (en) 1999-01-28
    HUP9901933A3 (en) 2001-04-28

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