EP0034548B1 - Apparatus for obtaining dispersions - Google Patents

Apparatus for obtaining dispersions Download PDF

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Publication number
EP0034548B1
EP0034548B1 EP81420010A EP81420010A EP0034548B1 EP 0034548 B1 EP0034548 B1 EP 0034548B1 EP 81420010 A EP81420010 A EP 81420010A EP 81420010 A EP81420010 A EP 81420010A EP 0034548 B1 EP0034548 B1 EP 0034548B1
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EP
European Patent Office
Prior art keywords
turbine
dispersions
conduit
powder
blades
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Expired - Lifetime
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EP81420010A
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German (de)
French (fr)
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EP0034548A1 (en
Inventor
André Berchoux
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Rhone Poulenc Textile SA
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Rhone Poulenc Textile SA
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50Mixing liquids with solids
    • B01F23/53Mixing liquids with solids using driven stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/60Pump mixers, i.e. mixing within a pump
    • B01F25/64Pump mixers, i.e. mixing within a pump of the centrifugal-pump type, i.e. turbo-mixers

Definitions

  • the present invention relates to a device for continuously obtaining fine dispersions.
  • It relates to a device for obtaining dispersions of a divided product in the form of powder in a liquid.
  • the plane of the turbine is inclined to promote the flow of dispersions.
  • the conduit bringing the powder is inclined so that it arrives by gravity.
  • the powder and the liquid are brought into contact dynamically and at high speed. To do this, they must be brought to separate points and speeded up separately.
  • Such a device is suitable even in the case of liquid having a high solvating power with respect to the powder, intended to be dispersed in said liquid.
  • the contact time inside the device is as short as possible, of the order millisecond; this time must be all the lower, the higher the solvating power of the liquid vis-à-vis the powder.
  • the solvent and the powder are brought to respective temperatures such that the solvating power is as low as possible during the operation, to avoid the risks of clogging.
  • Such a device is particularly suitable for obtaining dispersions of polyvinyl chloride in a solvent such as the carbon sulfide / acetone mixture.
  • the dispersions thus obtained are fine and regular so that the resulting solutions can then be spun continuously without problem to give yarns and fibers also of regular composition. Furthermore, the actual dissolution can be carried out more quickly and more easily so that the energy required for obtaining the collodions is much less.
  • the concentration limit is determined by the viscosity of the products obtained beyond which they are no longer transportable.
  • the polyvinyl chloride powder is conveyed by gravity into the conduit (1) arriving at the center of the turbine (2) then immediately set in speed by centrifugal force by means of the blades (3).
  • the solvent is conveyed separately by means of a conduit (6) placed perpendicularly to the plane of the turbine and arrives on the series of outer blades (8) then is put into motion immediately, the powder and the solvent coming into contact. speed on the outer part of the turbine (2). This is inserted into a room (4) and actuated by means of the motor (5).
  • the turbine is inclined at 45 ° relative to the horizontal.
  • the dispersion leaves tangentially to the turbine (2) by means of the conduit (7) and the dispersion is collected by gravity.
  • FIG. 2 represents another embodiment of the device according to the invention. It includes a conduit (1) provided with an endless screw, placed horizontally bringing the polymer powder to the center of the turbine (2) provided with blades (3) allowing the polymer powder to speed up in the external part the turbine; the conduit (6) allows the direct introduction of the solvent on the blades (8) outside the turbine, the two products being dispersed instantly by the turbine (2) actuated by the motor (5). The dispersion obtained leaves by gravity by means of the conduit (7) tangential to the turbine.
  • the device according to the present application makes it possible to obtain, in a very short period of time, which may be as low as a few milliseconds, fine and regular dispersions of variable concentration depending on the viscosity of said dispersions and on their ability to be conveyed.
  • dispersions of polyvinyl chloride powder in the solvent mixture of carbon sulfide / acetone (50/50 by volume) with a concentration of 28 to 30% by weight it even turns out to be possible to obtain dispersions by introducing the solvent-mixture at room temperature, which is of significant economic interest.
  • the device as shown in FIG. 2 is used, which has been continuously rotated for 100 hours, while introducing polyvinyl chloride powder with a flow rate of 45 kg / hour into the center of the turbine, by l 'Intermediate of a dosing screw and the solvent mixture carbon sulfide / acetone (50/50 by volume) maintained at around 20C at a rate of 115 l / hour on the outside of the turbine.
  • the device with an internal diameter of 12 cm has an outer row of 12 blades (8) inclined at 30 °; the central blades (3) are simply constituted by a butterfly screw, the speed of rotation of the turbine is 3,000 rpm and the dispersion is produced in a period of about 5 milliseconds at the rate of 160 kg / hour.
  • the dispersion thus obtained is taken up in a tank and can be used continuously in later stages of treatment.
  • polyvinyl chloride powder is introduced separately at a rate of 60 kg / hour and the solvent mixture of carbon sulfide / acetone at a rate of 160 kg / hour at room temperature, the dispersion has was produced continuously with a flow rate of 220 kg / hour for 5 hours directly at room temperature.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Description

La présente invention concerne un dispositif pour l'obtention continue de dispersions fines.The present invention relates to a device for continuously obtaining fine dispersions.

Elle concerne un dispositif pour l'obtention de dispersions d'un produit divisé sous forme de poudre dans un liquide.It relates to a device for obtaining dispersions of a divided product in the form of powder in a liquid.

Elle s'applique particulièrement aux liquides présentant un pouvoir de solvatation important vis-à-vis des poudres avec lesquelles ils doivent être mélangés, par exemple des polymères sous forme de poudre.It is particularly applicable to liquids having a high solvating power with respect to the powders with which they are to be mixed, for example polymers in powder form.

En effet, la dissolution de certains polymères filables en solution présente de grosses difficultés, c'est pourquoi il est plus facile dans un premier temps de les disperser dans des conditions où la dissolution ne se produit pas avant de les dissoudre : cela permet d'éviter la formation de grumeaux voire même la prise en masse de la poudre et du liquide.Indeed, the dissolution of certain spinnable polymers in solution presents great difficulties, this is why it is easier at first to disperse them under conditions where the dissolution does not occur before dissolving them: this makes it possible to avoid the formation of lumps or even the solidification of the powder and the liquid.

Ainsi, jusqu'à présent, la dissolution du chlorure de polyvinyle en poudre dans le mélange solvant acétone/sulfure de carbone nécessitait un malaxage de plusieurs heures dans un malaxeur et devait se faire nécessairement en discontinu ; de surcroit, le mélange obtenu manquait d'homogénéité, inconvénient qui se répercutait sur la qualité des fils obtenus.Thus, until now, the dissolution of the polyvinyl chloride powder in the acetone / carbon sulphide solvent mixture required kneading for several hours in a kneader and had to be done batchwise; moreover, the mixture obtained lacked homogeneity, a disadvantage which had repercussions on the quality of the wires obtained.

On a essayé également de préparer des dispersions selon le dispositif décrit dans la demande française n* 2 250 564 en formant d'abord un conduit liquide dans le liquide dans lequel la poudre doit être dispersée, en introduisant la poudre dans le conduit liquide puis en pulvérisant le conduit liquide contenant la poudre.We have also tried to prepare dispersions according to the device described in French application No. 2,250,564 by first forming a liquid conduit in the liquid in which the powder is to be dispersed, by introducing the powder into the liquid conduit and then by spraying the liquid conduit containing the powder.

Mais un tel dispositif ne convient pas pour l'obtention de dispersions de certains polymères telles que celles de polychlorure de vinyle dans le mélange solvant acétone/sulfure de carbone : le polymère et le solvant se prennent en masse en bloquant totalement l'appareil. ,However, such a device is not suitable for obtaining dispersions of certain polymers such as those of polyvinyl chloride in the acetone / carbon sulfide solvent mixture: the polymer and the solvent solidify, completely blocking the device. ,

Il est connu selon l'US-A-3423075 de mélanger des produits humides et secs au moyen d'un dispositif horizontal comportant une seule série de pales pour le mélange des produits, le produit sec étant amené par une ouverture centrale et le produit humide au moyen de plusieurs tuyaux placés circonférentiellement par rapport à l'arrivée centrale.It is known according to US-A-3423075 to mix wet and dry products by means of a horizontal device comprising a single series of blades for mixing the products, the dry product being brought in through a central opening and the wet product by means of several pipes placed circumferentially with respect to the central inlet.

Il est également connu selon l'US-A-4176972 un dispositif pour mélanger des boues de gypse comportant un disque rotatif plat et un boîtier fixe déterminant une chambre circulaire creuse divisée en trois zones annulaires séparées les unes des autres sur une grande partie de leur périphérie, les 2 premières zones comportant des lames et des dents tournant avec le disque pour assurer le mélange.It is also known according to US-A-4176972 a device for mixing gypsum sludge comprising a flat rotating disc and a fixed housing defining a hollow circular chamber divided into three annular zones separated from each other over a large part of their periphery, the first 2 zones comprising blades and teeth rotating with the disc to ensure mixing.

La présente invention concerne un dispositif pour la préparation en continu et pratiquement instantanée de dispersions fines et régulières de polymères en poudre dans leur solvant liquide, comprenant :

  • une turbine actionnée par un moteur sur laquelle sont fixées seulement deux rangées de pales ne permettant pas le retour des produits au centre de la turbine, une rangée située concentriquement au centre, l'autre rangée placée concentriquement à la rangée sur la partie extérieure de la turbine, le passage des matériaux étant effectué de manière libre et continue, sans rencontrer d'obstacle autre que les pales,
  • un seul conduit permettant l'alimentation du polymère en poudre au centre de la turbine,
  • un seul conduit permettant d'introduire du liquide sur les pales extérieures,
  • un conduit d'évacuation des dispersions obtenues, tangentiellement à la turbine et situé dans le même plan que celle-ci.
The present invention relates to a device for the continuous and practically instantaneous preparation of fine and regular dispersions of powdered polymers in their liquid solvent, comprising:
  • a turbine powered by a motor on which are fixed only two rows of blades not allowing the return of the products in the center of the turbine, one row located concentrically in the center, the other row placed concentrically with the row on the outside of the turbine, the passage of the materials being carried out in a free and continuous manner, without encountering any obstacle other than the blades,
  • a single duct allowing the polymer powder to be fed to the center of the turbine,
  • a single conduit for introducing liquid onto the outer blades,
  • a discharge pipe for the dispersions obtained, tangential to the turbine and located in the same plane as the latter.

De préférence, le plan de la turbine est incliné pour favoriser l'écoulement des dispersions.Preferably, the plane of the turbine is inclined to promote the flow of dispersions.

De manière préférentielle également, le conduit amenant la poudre est incliné de telle sorte que celle-ci arrive par gravité.Also preferably, the conduit bringing the powder is inclined so that it arrives by gravity.

La poudre et le liquide sont mis en contact de manière dynamique et à grande vitesse. Pour ce faire, ils doivent être amenés en des points séparés et mis en vitesse séparément.The powder and the liquid are brought into contact dynamically and at high speed. To do this, they must be brought to separate points and speeded up separately.

Un tel dispositif convient même dans le cas de liquide présentant un pouvoir de solvatation élevé vis-à-vis de la poudre, destinée à être dispersée dans ledit liquide.Such a device is suitable even in the case of liquid having a high solvating power with respect to the powder, intended to be dispersed in said liquid.

Pour l'obtention de dispersion de poudre dans un liquide ayant un pouvoir de solvatation important vis-à-vis de la poudre, il est préférable que la durée de contact à l'intérieur du dispositif soit aussi faible que possible, de l'ordre de la millise- conde; ce temps doit être d'autant plus faible, que le pouvoir de solvatation du liquide est élevé vis-à-vis de la poudre.To obtain powder dispersion in a liquid having a high solvating power with respect to the powder, it is preferable that the contact time inside the device is as short as possible, of the order millisecond; this time must be all the lower, the higher the solvating power of the liquid vis-à-vis the powder.

De la même manière, il est également préférable que le solvant et la poudre soient amenés à des températures respectives telles que le pouvoir de solvatation soit le plus faible possible au cours de l'opération, pour éviter les risques de colmatage.In the same way, it is also preferable that the solvent and the powder are brought to respective temperatures such that the solvating power is as low as possible during the operation, to avoid the risks of clogging.

Un tel dispositif convient particulièrement pour l'obtention de dispersions de polychlorure de vinyle dans un solvant tel que le mélange sulfure de carbone/acétone. Les dispersions ainsi obtenues sont fines et régulières si bien que les solutions en résultant peuvent ensuite être filées en continu sans problème pour donner des fils et fibres également de composition régulière. Par ailleurs, la dissolution proprement dite peut être réalisée plus rapidement et plus facilement si bien que l'énergie nécessitée pour l'obtention des collodions est bien moindre.Such a device is particularly suitable for obtaining dispersions of polyvinyl chloride in a solvent such as the carbon sulfide / acetone mixture. The dispersions thus obtained are fine and regular so that the resulting solutions can then be spun continuously without problem to give yarns and fibers also of regular composition. Furthermore, the actual dissolution can be carried out more quickly and more easily so that the energy required for obtaining the collodions is much less.

Enfin, il est possible selon ce dispositif d'obtenir des dispersions plus concentrées que celles utilisées habituellement permettant de réaliser aussi une économie sur la quantité de solvant utilisé. La limite de concentration est déterminée par la viscosité des produits obtenus au-delà de laquelle ils ne sont plus véhiculables.Finally, it is possible according to this device to obtain more concentrated dispersions than those usually used, also making it possible to save on the amount of solvent used. The concentration limit is determined by the viscosity of the products obtained beyond which they are no longer transportable.

La mise en oeuvre du dispositif selon l'invention sera mieux comprise à l'aide des figures 1 et 2 qui constituent des exemples de réalisation du dispositif selon l'invention à titre illustratif mais non limitatif.The implementation of the device according to the invention will be better understood with the aid of Figures 1 and 2 which constitute exemplary embodiments of the device according to the invention by way of illustration but not limitation.

Selon la figure 1, la poudre de polychlorure de vinyle est véhiculée par gravité dans le conduit (1) arrivant au centre de la turbine (2) puis immédiatement mise en vitesse par force centrifuge au moyen des pales (3). Le solvant est véhiculé séparément au moyen d'un conduit (6) placé perpendiculairement par rapport au plan de la turbine et arrive sur la série de pales (8) extérieures puis est mis en mouvement aussitôt, la poudre et le solvant entrant en contact en vitesse sur la partie extérieure de la turbine (2). Celle-ci est insérée dans une pièce (4) et actionnée au moyen du moteur (5). La turbine est inclinée à 45° par rapport à l'horizontale. La dispersion sort tangentiellement à la turbine (2) au moyen du conduit (7) et la dispersion est recueillie par gravité.According to FIG. 1, the polyvinyl chloride powder is conveyed by gravity into the conduit (1) arriving at the center of the turbine (2) then immediately set in speed by centrifugal force by means of the blades (3). The solvent is conveyed separately by means of a conduit (6) placed perpendicularly to the plane of the turbine and arrives on the series of outer blades (8) then is put into motion immediately, the powder and the solvent coming into contact. speed on the outer part of the turbine (2). This is inserted into a room (4) and actuated by means of the motor (5). The turbine is inclined at 45 ° relative to the horizontal. The dispersion leaves tangentially to the turbine (2) by means of the conduit (7) and the dispersion is collected by gravity.

La figure 2 représente un autre mode de réalisation du dispositif selon l'invention. Il comprend un conduit (1) muni d'une vis sans fin, placé horizontalement amenant la poudre de polymère au centre de la turbine (2) munie de pales (3) permettant la mise en vitesse de la poudre de polymère dans la partie extérieure de la turbine ; le conduit (6) permet l'introduction directe du solvant sur les pales (8) extérieures de la turbine, les deux produits étant dispersés instantanément par la turbine (2) actionnée par le moteur (5). La dispersion obtenue sort par gravité au moyen du conduit (7) tangentiellement à la turbine.FIG. 2 represents another embodiment of the device according to the invention. It includes a conduit (1) provided with an endless screw, placed horizontally bringing the polymer powder to the center of the turbine (2) provided with blades (3) allowing the polymer powder to speed up in the external part the turbine; the conduit (6) allows the direct introduction of the solvent on the blades (8) outside the turbine, the two products being dispersed instantly by the turbine (2) actuated by the motor (5). The dispersion obtained leaves by gravity by means of the conduit (7) tangential to the turbine.

Le dispositif selon la présente demande permet d'obtenir, en un laps de temps très court, pouvant être aussi faible que quelques millisecondes, des dispersions fines et régulières de concentration variable dépendant de la viscosité desdites dispersions et de leur aptitude à être véhiculées. Pour le cas particulier des dispersions de polychlorure de vinyle en poudre dans le mélange solvant sulfure de carbone/acétone (50/50 en volume) de concentration 28 à 30 % en poids, il s'avère même possible d'obtenir des dispersions en introduisant le mélange-solvant à température ambiante ce qui présente un intérêt économique important.The device according to the present application makes it possible to obtain, in a very short period of time, which may be as low as a few milliseconds, fine and regular dispersions of variable concentration depending on the viscosity of said dispersions and on their ability to be conveyed. For the specific case of dispersions of polyvinyl chloride powder in the solvent mixture of carbon sulfide / acetone (50/50 by volume) with a concentration of 28 to 30% by weight, it even turns out to be possible to obtain dispersions by introducing the solvent-mixture at room temperature, which is of significant economic interest.

Les exemples qui suivent sont donnés à titre indicatif pour illustrer l'invention.The examples which follow are given by way of illustration to illustrate the invention.

Exemple 1Example 1

On utilise le dispositif tel que représenté sur la figure 2 que l'on a fait tourner en continu pendant 100 heures, tout en introduisant de la poudre de polychlorure de vinyle avec un débit de 45 kg/heure au centre de la turbine, par l'intermédiaire d'une vis doseuse et le mélange solvant sulfure de carbone/acétone (50/50 en volume) maintenu à environ 20C à raison de 115 1/heure sur l'extérieur de la turbine.The device as shown in FIG. 2 is used, which has been continuously rotated for 100 hours, while introducing polyvinyl chloride powder with a flow rate of 45 kg / hour into the center of the turbine, by l 'Intermediate of a dosing screw and the solvent mixture carbon sulfide / acetone (50/50 by volume) maintained at around 20C at a rate of 115 l / hour on the outside of the turbine.

L'appareil de diamètre intérieur de 12 cm comporte une rangée extérieure de 12 pales (8) inclinées à 30° ; les pales centrales (3) sont simplement constituées par une vis papillon, la vitesse de rotation de la turbine est de 3 000 t/minute et la dispersion est produite en un laps de temps de 5 millisecondes environ à raison de 160 kg/heure.The device with an internal diameter of 12 cm has an outer row of 12 blades (8) inclined at 30 °; the central blades (3) are simply constituted by a butterfly screw, the speed of rotation of the turbine is 3,000 rpm and the dispersion is produced in a period of about 5 milliseconds at the rate of 160 kg / hour.

La dispersion ainsi obtenue est reprise dans un réservoir et peut être utilisée de manière continue dans des stades ultérieurs de traitement.The dispersion thus obtained is taken up in a tank and can be used continuously in later stages of treatment.

Exemple 2Example 2

Dans la turbine utilisée dans l'exemple 1, on introduit séparément de la poudre de polychlorure de vinyle à raison de 60 kg/heure et le mélange solvant sulfure de carbone/acétone à raison de 160 kg/heure à température ambiante, la dispersion a été produite en continu avec un débit de 220 kg/heure pendant 5 heures directement à température ambiante.In the turbine used in Example 1, polyvinyl chloride powder is introduced separately at a rate of 60 kg / hour and the solvent mixture of carbon sulfide / acetone at a rate of 160 kg / hour at room temperature, the dispersion has was produced continuously with a flow rate of 220 kg / hour for 5 hours directly at room temperature.

Claims (3)

1. Device for the continuous and virtually instantaneous preparation of fine and uniform dispersions of powdered polymers in their liquid solvent, characterized in that it comprises :
a turbine (2) activated by a motor (5), on which turbine are fixed only two rows of blades (3 and 8) which do not permit the return of the products to the centre of the turbine, a row (3) located concentrically with the centre, the other row (8) placed concentrically to the row (3) on the outer part of the turbine (2), the passage of the materials being effected freely and continuously without encountering any obstacle other than the blades (3 and 8),
a single conduit (1) permitting the supply of powdered polymer to the centre of the turbine,
a single conduit (6) permitting the introduction of the liquid over the outer blades (8),
a conduit (7), for removing the dispersions obtained, which is tangential to the turbine and located in the same plane as the latter.
2. Device according to Claim 1, characterized in that the plane of the turbine is tilted in order to favour the flow of the dispersions.
3. Device according to Claim 1, characterized in that the conduit (1) supplying the powder is tilted with respect to the overall apparatus such that the powder arrives by means of gravity.
EP81420010A 1980-02-13 1981-02-11 Apparatus for obtaining dispersions Expired - Lifetime EP0034548B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8003217A FR2475418A1 (en) 1980-02-13 1980-02-13 METHOD AND DEVICE FOR OBTAINING DISPERSIONS
FR8003217 1980-02-13

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EP0034548A1 EP0034548A1 (en) 1981-08-26
EP0034548B1 true EP0034548B1 (en) 1990-01-03

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US (1) US4529321A (en)
EP (1) EP0034548B1 (en)
JP (1) JPS56152840A (en)
BR (1) BR8100929A (en)
CA (1) CA1160937A (en)
DE (1) DE3177138D1 (en)
ES (1) ES499364A0 (en)
FR (1) FR2475418A1 (en)
SU (1) SU1276250A3 (en)

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Publication number Priority date Publication date Assignee Title
US3423075A (en) * 1967-01-31 1969-01-21 Nat Lead Co Mixing device
US3923289A (en) * 1971-12-13 1975-12-02 Victor Danberg Method of mixing solids and liquids on a continuous basis
US4176972A (en) * 1978-08-09 1979-12-04 National Gypsum Company Coaxial pump mixer

Also Published As

Publication number Publication date
FR2475418B1 (en) 1984-12-21
DE3177138D1 (en) 1990-02-08
US4529321A (en) 1985-07-16
ES8201438A1 (en) 1981-12-16
SU1276250A3 (en) 1986-12-07
JPS56152840A (en) 1981-11-26
BR8100929A (en) 1981-08-25
ES499364A0 (en) 1981-12-16
CA1160937A (en) 1984-01-24
EP0034548A1 (en) 1981-08-26
FR2475418A1 (en) 1981-08-14
JPH059456B2 (en) 1993-02-05

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