WO2002040140A1 - Improvements to methods for repairing by sealing hollow fibres of membranes, in particular, ultrafiltration, nanofiltration, and hyperfiltration membranes - Google Patents

Improvements to methods for repairing by sealing hollow fibres of membranes, in particular, ultrafiltration, nanofiltration, and hyperfiltration membranes Download PDF

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Publication number
WO2002040140A1
WO2002040140A1 PCT/FR2001/003476 FR0103476W WO0240140A1 WO 2002040140 A1 WO2002040140 A1 WO 2002040140A1 FR 0103476 W FR0103476 W FR 0103476W WO 0240140 A1 WO0240140 A1 WO 0240140A1
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adhesive
fibers
membranes
fiber
plug
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PCT/FR2001/003476
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French (fr)
Inventor
Nouhad Abidine
Patrick Sauvade
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Aquasource
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Priority to AU2002223043A priority Critical patent/AU2002223043A1/en
Publication of WO2002040140A1 publication Critical patent/WO2002040140A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
    • B01D65/102—Detection of leaks in membranes

Definitions

  • the present invention relates to a method for repairing ultra-, nano- and hyper-filtration membranes, in particular in the configuration of hollow fibers, these membranes being used in particular in the separation operations implemented in particular in installations. treatment of liquids, for example aqueous effluents. These repairs can be carried out on new fibers, or on used fibers, the objective being to restore the integrity of the fibers, that is to say their total impermeability to compounds and particles of size greater than their cut-off thresholds. .
  • the invention also applies to the repair of microfiltration fibers, gas permeation, pervaporation etc.
  • microfiltration and ultrafiltration membranes make it possible, during permeation, to carry out the clarification and disinfection of the water passing through them in order to eliminate bacteria, viruses and other parasites.
  • the hollow fibers of such membranes have a geometry that is particularly suitable for ensuring good retention of dissolved and particulate species.
  • the hollow fibers are self-supporting, the bonding made at the two ends of a hollow fiber module ensures, on the one hand a perfect seal of the fibers with respect to each other and on the other hand a sealing between the entire bundle of fibers molded in a resin (constituting the head plate of a module, formed during the potting operation) and the external envelope of the module (casing or pressure tube).
  • a technique sometimes used consists, after potting, in strengthening the external protection of the hollow fibers, by brushing the fibers with a sufficiently fluid resin, this operation being sometimes called “varnishing". This varnishing then ensures perfect sealing of the porous section of the fibers, sections which could allow the migration of viruses, bacteria, microorganisms, macromolecules and other products and solutes of low mass found in water.
  • the hollow fibers of the membrane separation modules ensure good disinfection of water, or even other liquids or fluids.
  • the fibers break, particularly during bundling, potting or casing operations. These ruptures, more or less numerous, are linked to manufacturing defects or to natural or forced aging of the bran material. When such ruptures are noted, it becomes necessary to repair the broken fibers, failing which the module equipped with hollow fibers would no longer be able to fully ensure viral or bacteriological disinfection.
  • the first method consists in pushing into the damaged fiber a cylindrical obturator, also called "nail” having a dimension appropriate to the internal diameter of the fiber.
  • a cylindrical obturator also called "nail” having a dimension appropriate to the internal diameter of the fiber.
  • Some module manufacturers offer conical nails for this purpose, in order to facilitate their installation.
  • the quality of this repair can be further improved by brushing the fiber with a mono or two-component adhesive, in order to perfect and consolidate the sealing of the repair thus carried out.
  • the disadvantage of this technique lies in the frequency of defective adhesions between the two materials (nail and fiber) resulting from the small contact surface and / or possible crosslinking / polymerization defects of said adhesive.
  • the second method consists in injecting a two-component adhesive into the fiber identified as broken or "leaky". After injection of the adhesive using a needle, the latter is removed and the crosslinking of the adhesive is awaited.
  • the major drawback of this technique lies in the fact that, during the injection of small amounts of adhesive, cross-linking the product is time consuming. Therefore, before restarting the repaired module, there is a waiting period which can prove to be penalizing since it can reach 24 hours before complete crosslinking. It should also be mentioned that the crosslinking kinetics are linked to the ambient temperature prevailing on the site. Therefore, in cold weather, the crosslinking of the adhesive requires a longer duration and is sometimes even impossible. Thus, it is common to have to wait until the day after the repair before being able to reassemble the module, comprising the repaired defective fiber, on the filtration assembly.
  • the present invention has set itself the objective of providing a simple method, easy to implement and with immediate results, that is to say a method according to which in particular the duration of repair no longer constitutes a limit to the operation of the membranes and thanks to which the duration and the quality of the repair no longer depend on the ambient temperature, nor on the quality or history of the fibers to be repaired . Furthermore, thanks to the invention, the separation and permeability performance of the membranes are immediately and fully restored.
  • this invention relates to a method for repairing ultra-, nano- and hyper-filtration membranes, in particular in fiber configuration.
  • tubular hollow which consists, after detection and localization of a leak in a damaged fiber, in injecting a crosslinkable adhesive therein, this process being characterized in that a plug of a precisely dosed amount of is injected into the damaged fiber a mono-component synthetic adhesive and the curing of said adhesive plug is carried out by crosslinking / polymerization under ultraviolet radiation with a focusing of this radiation on the section of the fiber to be repaired, under a high flux density in the form of a beam parallel, via a waveguide.
  • an adhesive which is a synthetic resin and the height of the adhesive plug injected is of the order of 6 +/- 1 mm.
  • an adhesive stopper with the height mentioned above close to 5 to 7 mm, by injection either manually or using conventional apparatuses injection of adhesive fitted with precise dosers and pistons driven by a controlled pressure of compressed air; - that the adhesive thus injected did not flow after its installation;
  • the injected adhesive could be crosslinked over its entire height; that the crosslinking / polyerization time of the adhesive was approximately 30 seconds under intense ultraviolet radiation whose parallel beam was focused on the section of the fiber to be repaired using a waveguide.
  • adhesives crosslinkable under ultraviolet radiation and having a fairly wide viscosity range can be used. It is then possible to repair hollow fibers having internal diameters of, for example, between 0.3 and 2.0 mm.
  • adhesives which can be used according to the invention, mention may in particular be made of glues sold commercially by the companies PERMABOND (adhesive UN 9110) and HERAEUS (adhesive FLOWLI ⁇ E).
  • glues sold commercially by the companies PERMABOND (adhesive UN 9110) and HERAEUS (adhesive FLOWLI ⁇ E).
  • any system can be used to focus the UV radiation on the section of the fiber to be repaired, for example the device “Translux CL. »Marketed by the firm HERAEUS.
  • the new fibers are immersed in a solution containing hydrochloric acid at pH 1 for two consecutive days;
  • the new fibers are immersed in an aqueous sodium hydroxide solution at pH 10, for 24 hours;
  • the new fibers are immersed in a solution containing citric acid at a pH close to 3, for 24 hours;
  • the new fibers are immersed in a chlorine solution containing 500 ppm of active chlorine, for 24 hours.
  • the present invention is not limited to the examples of implementation described above, but that it encompasses all variants thereof, in particular, as already mentioned, the invention is not limited to the repair of only ultra-, nano and hyper-filtration fibers, but it can also be applied to the repair in particular of microfiltration fibers of gas permeation, of pervaporation etc ...

Abstract

The invention concerns a method for repairing membranes, such as ultrafiltration, nanofiltration and hyperfiltration membranes, in particular shaped like tubular hollow fibres, which consists, after detecting and locating a leak in a damaged fibre, in injecting therein a crosslinkable adhesive. Said method is characterised in that it consists in injecting into the damaged fibre a plug of an accurately measured amount of a single-constituent synthetic adhesive and in hardening said adhesive plug by crosslinking/polymerisation under ultraviolet radiation focusing said radiation on the fibre section to be repaired, under high flux density in the form of parallel beam, via a waveguide.

Description

Perfectionnements apportés aux procédés de réparation par obturation des fibres creuses des membranes, notamment d'ultra-, nano- et hyper-filtration Improvements brought to repair processes by filling the hollow fibers of the membranes, in particular of ultra-, nano- and hyper-filtration
La présente invention est relative à un procédé de réparation des membranes d'ultra-, nano- et hyper- filtration, en particulier en configuration de fibres creuses, ces membranes étant utilisées notamment dans les opérations de séparation mises en œuvre en particulier dans les installations de traitement de liquides, par exemple d'effluents aqueux. Ces réparations peuvent être effectuées sur des fibres neuves, ou sur des fibres usagées, l'objectif étant de restaurer l'intégrité des fibres, c'est-à-dire leur imperméabilité totale aux composés et particules de taille supérieure à leurs seuils de coupure.The present invention relates to a method for repairing ultra-, nano- and hyper-filtration membranes, in particular in the configuration of hollow fibers, these membranes being used in particular in the separation operations implemented in particular in installations. treatment of liquids, for example aqueous effluents. These repairs can be carried out on new fibers, or on used fibers, the objective being to restore the integrity of the fibers, that is to say their total impermeability to compounds and particles of size greater than their cut-off thresholds. .
L'invention s'applique également à la réparation des fibres de microfiltration, de permëation de gaz, de pervaporation etc..The invention also applies to the repair of microfiltration fibers, gas permeation, pervaporation etc.
On sait que les membranes de microfiltration et d'ultrafiltration permettent, au cours de la perméation, d'effectuer la clarification et la désinfection des eaux qui les traverse afin d'éliminer les bactéries, virus et autres parasites.It is known that microfiltration and ultrafiltration membranes make it possible, during permeation, to carry out the clarification and disinfection of the water passing through them in order to eliminate bacteria, viruses and other parasites.
On sait également que les fibres creuses de telles membranes possèdent une géométrie particulièrement adaptée en vue d'assurer une bonne rétention des espèces dissoutes et particulaires . Les fibres creuses sont auto-supportées, les collages faits aux deux extrémités d'un module à fibres creuses assurent, d'une part une étanchéité parfaite des fibres les unes par rapport aux autres et d'autre part une étanchéité entre l'ensemble du faisceau de fibres moulées dans une résine (constituant la plaque de tête d'un module, formé lors de l'opération d'empotage) et l'enveloppe externe du module (carter ou tube de pression) .It is also known that the hollow fibers of such membranes have a geometry that is particularly suitable for ensuring good retention of dissolved and particulate species. The hollow fibers are self-supporting, the bonding made at the two ends of a hollow fiber module ensures, on the one hand a perfect seal of the fibers with respect to each other and on the other hand a sealing between the entire bundle of fibers molded in a resin (constituting the head plate of a module, formed during the potting operation) and the external envelope of the module (casing or pressure tube).
En ce qui concerne la réalisation de tels modules à fibres creuses, on peut se reporter par exemple au Mémento Technique de l'Eau, 1989, Tome 2, Chapitre 15, édité par DEGREMONT .With regard to the production of such hollow fiber modules, reference may be made, for example, to the Water Technical Memento, 1989, Volume 2, Chapter 15, edited by DEGREMONT.
Une technique parfois utilisée consiste, après l'empotage, à renforcer la protection externe des fibres creuses, en badigeonnant les fibres avec une résine suffisamment fluide, cette opération étant parfois appelée « vernissage ». Ce vernissage assure par la suite un bouchage parfait de la section poreuse des fibres, sections qui pourraient permettre la migration des virus, bactéries, microorganismes, macromolécules et autres produits et solutés de faible masse se trouvant dans l'eau.A technique sometimes used consists, after potting, in strengthening the external protection of the hollow fibers, by brushing the fibers with a sufficiently fluid resin, this operation being sometimes called "varnishing". This varnishing then ensures perfect sealing of the porous section of the fibers, sections which could allow the migration of viruses, bacteria, microorganisms, macromolecules and other products and solutes of low mass found in water.
Normalement, lorsqu'elles sont fabriquées selon les règles de l'art, les fibres creuses des modules de séparation par membranes assurent une bonne désinfection des eaux, voire d'autres liquides ou fluides. Cependant, malgré tous les soins apportés à leur fabrication, il peut survenir des ruptures de fibres, notamment lors des opérations de mise en faisceau, d'empotage ou de mise en carter. Ces ruptures, plus ou moins nombreuses, sont liées aux défauts de fabrication ou au vieillissement naturel ou forcé du matériau me branaire. Lorsque de telles ruptures sont constatées, il devient nécessaire de réparer les fibres cassées, faute de quoi le module équipé de fibres creuses ne serait plus en mesure d'assurer pleinement la désinfection virale ou bactériologique. Il existe dans l'état actuel de la technique de nombreux procédés pouvant être utilisés pour détecter la présence des fibres cassées ou qui fuient . On peut par exemple se référer à FR-A-2 775 440. Une fois identifiée, une fibre endommagée doit être réparée le plus rapidement possible afin de ne pas endommager les fibres auxquelles elle est intégrée, ces dommages pouvant résulter notamment d'une pollution du compartiment perméat .Normally, when manufactured according to the rules of the art, the hollow fibers of the membrane separation modules ensure good disinfection of water, or even other liquids or fluids. However, despite all the care taken in their manufacture, it may occur that the fibers break, particularly during bundling, potting or casing operations. These ruptures, more or less numerous, are linked to manufacturing defects or to natural or forced aging of the bran material. When such ruptures are noted, it becomes necessary to repair the broken fibers, failing which the module equipped with hollow fibers would no longer be able to fully ensure viral or bacteriological disinfection. There are many methods available in the state of the art that can be used to detect the presence of broken or leaking fibers. One can for example refer to FR-A-2 775 440. Once identified, a damaged fiber must be repaired as quickly as possible in order not to damage the fibers in which it is integrated, this damage being able to result in particular from pollution permeate compartment.
II existe divers procédés permettant de réparer les fibres endommagées. A titre d'exemples, on en décrira ci- après deux qui sont les plus particulièrement représentatifs et les plus largement utilisés à l'heure actuelle.There are various methods for repairing damaged fibers. By way of examples, two will be described below which are the most particularly representative and the most widely used at present.
Le premier procédé consiste à pousser dans la fibre endommagée un obturateur cylindrique, encore appelé « clou » présentant une dimension appropriée au diamètre interne de la fibre. Certains fabricants de modules proposent à cet effet des clous de forme conique, de manière à faciliter leur mise en place. De plus, on peut encore améliorer la qualité de cette réparation en badigeonnant la fibre avec un adhésif mono ou bi-composant , afin de parfaire et de consolider l'étanchéité de la réparation ainsi effectuée. L'inconvénient de cette technique réside dans la fréquence des adhérences défectueuses entre les deux matériaux (clou et fibre) résultant de la faible surface de contact et/ou d'éventuels défauts de réticulation/polymérisation dudit adhésif.The first method consists in pushing into the damaged fiber a cylindrical obturator, also called "nail" having a dimension appropriate to the internal diameter of the fiber. Some module manufacturers offer conical nails for this purpose, in order to facilitate their installation. In addition, the quality of this repair can be further improved by brushing the fiber with a mono or two-component adhesive, in order to perfect and consolidate the sealing of the repair thus carried out. The disadvantage of this technique lies in the frequency of defective adhesions between the two materials (nail and fiber) resulting from the small contact surface and / or possible crosslinking / polymerization defects of said adhesive.
Le deuxième procédé consiste à injecter un adhésif bi- composant dans la fibre identifiée comme rompue ou « fuyarde ». Après injection de l'adhésif à l'aide d'une aiguille, on retire cette dernière et on attend la reticulation de l'adhésif. L'inconvénient majeur de cette technique réside dans le fait que, lors de l'injection de petites quantités d'adhésif, la reticulation du produit exige beaucoup de temps. De ce fait, avant remise en route du module réparé, il existe un délai d'attente qui peut se révéler pénalisant étant donné qu' il peut atteindre 24 heures avant reticulation complète. Il convient également de mentionner que la cinétique de reticulation est liée à la température ambiante régnant sur le site. De ce fait, par temps froid, la reticulation de l'adhésif exige une durée plus longue et elle est même parfois impossible. Ainsi, il est courant de devoir attendre le lendemain de la réparation avant de pouvoir remonter le module, comportant la fibre défectueuse réparée, sur l'ensemble de filtration.The second method consists in injecting a two-component adhesive into the fiber identified as broken or "leaky". After injection of the adhesive using a needle, the latter is removed and the crosslinking of the adhesive is awaited. The major drawback of this technique lies in the fact that, during the injection of small amounts of adhesive, cross-linking the product is time consuming. Therefore, before restarting the repaired module, there is a waiting period which can prove to be penalizing since it can reach 24 hours before complete crosslinking. It should also be mentioned that the crosslinking kinetics are linked to the ambient temperature prevailing on the site. Therefore, in cold weather, the crosslinking of the adhesive requires a longer duration and is sometimes even impossible. Thus, it is common to have to wait until the day after the repair before being able to reassemble the module, comprising the repaired defective fiber, on the filtration assembly.
Les autres procédés actuellement disponibles sont dans l'ensemble plus adaptés aux réparations effectuées en usine par les fabricants de modules eux-mêmes et ils sont trop difficiles à mettre en œuvre sur un module équipé de fibres, éventuellement humides, par des opérateurs peu expérimentés .The other methods currently available are on the whole more suitable for repairs carried out in the factory by the module manufacturers themselves and they are too difficult to implement on a module equipped with fibers, possibly wet, by inexperienced operators.
Afin de pallier les inconvénients des procédés de réparation mentionnés ci-dessus, la présente invention s'est fixé pour objectif d'apporter un procédé simple, facile à mettre en œuvre et aux résultats immédiats, c'est- à-dire un procédé selon lequel notamment la durée de réparation ne constitue plus une limite à l'exploitation des membranes et grâce auquel la durée et la qualité de la réparation ne dépendent plus de la température ambiante, ni de la qualité ou de l'historique des fibres devant être réparées. En outre, grâce à l'invention, les performances de séparation et de perméabilité des membranes sont immédiatement et intégralement restaurées .In order to overcome the drawbacks of the repair methods mentioned above, the present invention has set itself the objective of providing a simple method, easy to implement and with immediate results, that is to say a method according to which in particular the duration of repair no longer constitutes a limit to the operation of the membranes and thanks to which the duration and the quality of the repair no longer depend on the ambient temperature, nor on the quality or history of the fibers to be repaired . Furthermore, thanks to the invention, the separation and permeability performance of the membranes are immediately and fully restored.
En conséquence, cette invention concerne un procédé de réparation de membranes d'ultra-, nano- et hyper- filtration, en particulier en configuration de fibres creuses tubulaires qui consiste, après détection et localisation d'une fuite dans une fibre endommagée, à y injecter un adhésif réticulable, ce procédé étant caractérisé en ce que l'on injecte dans la fibre endommagée un bouchon d'une quantité précisément dosée d'un adhésif synthétique mono-composant et on effectue le durcissement dudit bouchon d'adhésif par réticulation/polymérisation sous rayonnement ultra-violet avec une focalisation de ce rayonnement sur la section de la fibre à réparer, sous une forte densité de flux sous forme de faisceau parallèle, par l'intermédiaire d'un guide d'onde.Consequently, this invention relates to a method for repairing ultra-, nano- and hyper-filtration membranes, in particular in fiber configuration. tubular hollow which consists, after detection and localization of a leak in a damaged fiber, in injecting a crosslinkable adhesive therein, this process being characterized in that a plug of a precisely dosed amount of is injected into the damaged fiber a mono-component synthetic adhesive and the curing of said adhesive plug is carried out by crosslinking / polymerization under ultraviolet radiation with a focusing of this radiation on the section of the fiber to be repaired, under a high flux density in the form of a beam parallel, via a waveguide.
Selon un mode de mise en œuvre de la présente invention, on utilise un adhésif qui est une résine synthétique et la hauteur du bouchon d'adhésif injecté est de l'ordre de 6 +/- 1 mm.According to an embodiment of the present invention, an adhesive is used which is a synthetic resin and the height of the adhesive plug injected is of the order of 6 +/- 1 mm.
Pour la mise au point de cette nouvelle technique, il a fallu vaincre deux préjugés résultant des phénomènes décrits ci-dessus dont les conséquences pouvaient être cumulatives :For the development of this new technique, it was necessary to overcome two prejudices resulting from the phenomena described above whose consequences could be cumulative:
- tout d'abord, l'Homme de l'art sait, notamment par la littérature disponible que la reticulation sous rayonnement ultra-violet des polymères et monomères ne peut se faire que sous des épaisseurs assez faibles. Il est donc généralement admis que, pour réaliser un bouchon d'adhésif, par exemple pour réparer une fibre creuse, il n'est pas possible d'obtenir une reticulation complète sur une épaisseur supérieure à 1 mm, ce qui n'est ni suffisant, ni sécurisant pour l'Homme de l'art ;- First of all, those skilled in the art know, in particular from the available literature that the crosslinking under ultraviolet radiation of the polymers and monomers can only be done at fairly small thicknesses. It is therefore generally accepted that, to make an adhesive plug, for example to repair a hollow fiber, it is not possible to obtain complete crosslinking over a thickness greater than 1 mm, which is neither sufficient , nor reassuring for those skilled in the art;
- ensuite, le fait d'injecter un adhésif dans une fibre creuse sur une hauteur inférieure à 1 mm est techniquement très difficile et la question reste posée du devenir de l'excès d'adhésif non polymérisé/réticulé, donc instable. Ces considérations démontrent que l'Homme de l'art était détourné par ses connaissances de l'état de la technique d'envisager une réparation des fibres creuses par injection d'un bouchon d'adhésif d'épaisseur relativement importante .- Then, the fact of injecting an adhesive into a hollow fiber over a height of less than 1 mm is technically very difficult and the question remains of the fate of the excess of non-polymerized / crosslinked adhesive, therefore unstable. These considerations demonstrate that those skilled in the art were diverted by their knowledge of the state of the art to envisage repairing the hollow fibers by injecting a plug of adhesive of relatively large thickness.
Dans le cadre de la présente invention, on a pu vérifier :In the context of the present invention, it has been possible to verify:
- qu'il était possible de mettre en place, par un geste simple, un bouchon d'adhésif présentant la hauteur mentionnée ci-dessus voisine de 5 à 7 mm, par injection soit manuellement, soit à l'aide des appareils classiques d'injection d'adhésif équipés de doseurs précis et de pistons mus par une pression contrôlée d'air comprimé ; - que l'adhésif ainsi injecté ne coulait pas après sa mise en place ;- that it was possible to put in place, with a simple gesture, an adhesive stopper with the height mentioned above close to 5 to 7 mm, by injection either manually or using conventional apparatuses injection of adhesive fitted with precise dosers and pistons driven by a controlled pressure of compressed air; - that the adhesive thus injected did not flow after its installation;
- que l'adhésif injecté pouvait être réticulé sur toute sa hauteur ; que le temps de réticulation/poly érisation de l'adhésif était d'environ 30 secondes sous un rayonnement ultra-violet intense dont le faisceau parallèle était focalisé sur la section de la fibre à réparer en utilisant un guide d'onde.- that the injected adhesive could be crosslinked over its entire height; that the crosslinking / polyerization time of the adhesive was approximately 30 seconds under intense ultraviolet radiation whose parallel beam was focused on the section of the fiber to be repaired using a waveguide.
Pour la mise en œuvre de la présente invention, on peut utiliser plusieurs adhésifs réticulables sous rayonnement ultra-violet et présentant une gamme de viscosité assez large. Il est alors possible de réparer des fibres creuses présentant des diamètres internes compris par exemple entre 0,3 et 2,0 mm. A titre d'exemples d'adhésifs utilisables selon l'invention, on peut citer notamment des colles vendues dans le commerce par les sociétés PERMABOND (adhésif UN 9110) et HERAEUS (adhésif FLOWLIΝE) . En ce qui concerne le dispositif permettant d'assurer la reticulation de l'adhésif, on peut utiliser tout système permettant de focaliser le rayonnement UV sur la section de la fibre à réparer, par exemple le dispositif « Translux CL. » commercialisé par la firme HERAEUS .For the implementation of the present invention, several adhesives crosslinkable under ultraviolet radiation and having a fairly wide viscosity range can be used. It is then possible to repair hollow fibers having internal diameters of, for example, between 0.3 and 2.0 mm. As examples of adhesives which can be used according to the invention, mention may in particular be made of glues sold commercially by the companies PERMABOND (adhesive UN 9110) and HERAEUS (adhesive FLOWLIΝE). With regard to the device for ensuring the crosslinking of the adhesive, any system can be used to focus the UV radiation on the section of the fiber to be repaired, for example the device “Translux CL. »Marketed by the firm HERAEUS.
Afin de vérifier la tenue des réparations effectuées selon l'invention, sur des fibres à base d'acétate de cellulose, on a effectué sur ces dernières divers prétraitements :In order to verify the performance of the repairs carried out according to the invention, on fibers based on cellulose acetate, various pretreatments were carried out on them:
- les fibres sont neuves, propres et exemptes de tous résidus de fabrication ;- the fibers are new, clean and free from all manufacturing residues;
- les fibres neuves sont plongées dans une solution contenant de l'acide chlorhydrique à pH 1 et ce durant deux jours consécutifs ;- the new fibers are immersed in a solution containing hydrochloric acid at pH 1 for two consecutive days;
- les fibres neuves sont plongées dans une solution aqueuse de soude à pH 10, durant 24 heures ;- the new fibers are immersed in an aqueous sodium hydroxide solution at pH 10, for 24 hours;
- les fibres neuves sont plongées dans une solution contenant de l'acide citrique à pH voisin de 3, durant 24 heures ;- the new fibers are immersed in a solution containing citric acid at a pH close to 3, for 24 hours;
- les fibres neuves sont plongées dans une solution de chlore à 500 ppm de chlore actif, durant 24 heures.- the new fibers are immersed in a chlorine solution containing 500 ppm of active chlorine, for 24 hours.
On a effectué d'autres trempages qui concernaient des fibres neuves et des fibres usagées prélevées sur un module expertisé ayant cinq années de service, les trempages étant effectués dans des lessives potentiellement utilisables au contact des fibres en acétate de cellulose. Il s'agissait de lessives de la gamme « Ultrasil » de la Sté ECOLAB et de la gamme « Permaclean » commercialisée par la Sté AQUAZUR.Other soaking operations were carried out which concerned new fibers and used fibers taken from an expert module having five years of service, the soaking operations being carried out in potentially usable detergents in contact with the cellulose acetate fibers. These were detergents from the “Ultrasil” range of the ECOLAB Company and the “Permaclean” range marketed by the AQUAZUR Company.
Dans tous les cas mentionnés ci-dessus, toutes les réparations ont tenu et il ne s'est produit aucun incident.In all of the above-mentioned cases, all repairs were successful and no incidents occurred.
Sur toutes les fibres ainsi réparées, il est arrivé que certaines finissent par éclater, par mise sous pression croissante, mais loin de la zone réparée et sans que la réparation soit endommagée. On notera que dans le cas des fibres à base d'acétate de cellulose, de tels éclatements se produisent lorsqu'on atteint des pressions appliquées comprises entre 15 et 24.105 Pa., suivant que les fibres aient été vieillies, attaquées par des acides, des bases, des oxydants ou qu'elles étaient neuves.On all the fibers thus repaired, it has happened that some end up bursting, by increasing pressure, but far from the repaired area and without the repair is damaged. It will be noted that in the case of fibers based on cellulose acetate, such splitting occurs when an applied pressure of between 15 and 24 × 10 5 Pa is reached, depending on whether the fibers have been aged, attacked by acids, bases, oxidants or that they were new.
Il a également été possible de vérifier que le procédé de l'invention s'appliquait à des fibres à base d'autres matériaux que l'acétate de cellulose. Ainsi, on a pu faire des essais sur des fibres creuses à base de polysulfone naturel, de polyéthersulfone, d' éthylcellulose, ainsi que de polysulfone modifié par addition d'un polymère hydrophile que l'on a pris le soin de réticuler. Dans tous les cas, les fibres avaient des diamètres internes différents, sensiblement proches de 0,5 à 1,2 mm. Toutes les réparations ont été réussies et elles ont tenu.It was also possible to verify that the process of the invention applied to fibers based on materials other than cellulose acetate. Thus, it was possible to carry out tests on hollow fibers based on natural polysulfone, polyethersulfone, ethylcellulose, as well as polysulfone modified by the addition of a hydrophilic polymer which care was taken to crosslink. In all cases, the fibers had different internal diameters, substantially close to 0.5 to 1.2 mm. All the repairs were successful and they held up.
Enfin, on a effectué des tests afin de vérifier la tenue dans le temps des réparations effectuées selon l'invention. En effet, il aurait pu se produire des endommagements probablement en raison d'un interface pouvant se trouver sur le pourtour interne des fibres qui n'aurait pas suffisamment réticulé. Dans ce but, on a procédé à la réparation, selon le procédé objet de l'invention, des fibres neuves et des fibres colmatées en y implantant des bouchons d'adhésif. Après reticulation, tous les échantillons ont été testés sur un banc de vieillissement mécanique dans les conditions suivantes : durée de filtration égale à 30 secondes = durée de rétrolavage ; pression de filtration interne égale à X ; pression de rétrolavage externe égale à Y. Durant ce test, on a appliqué les valeurs suivantes pour X et Y :Finally, tests were carried out in order to verify the resistance over time of the repairs carried out according to the invention. Indeed, there could have been damage, probably due to an interface which may be on the internal periphery of the fibers which would not have sufficiently crosslinked. For this purpose, we proceeded to repair, according to the process which is the subject of the invention, new fibers and clogged fibers by implanting adhesive plugs therein. After crosslinking, all the samples were tested on a mechanical aging bench under the following conditions: filtration time equal to 30 seconds = backwashing time; internal filtration pressure equal to X; external backwashing pressure equal to Y. During this test, the following values were applied for X and Y:
X = Y = 3.105 Pa. puis 4.105 Pa. X ≈ 3.105 Pa. et Y = 4.105 Pa .X = Y = 3.10 5 Pa. Then 4.10 5 Pa. X ≈ 3.10 5 Pa. And Y = 4.10 5 Pa.
X = 4.10 Pa. et Y = 3.10b Pa .X = 4.10 Pa. And Y = 3.10 b Pa.
Les essais ont été poursuivis jusqu'à l'obtention d'un nombre de cycles supérieur à 100.000 sans qu'il soit constaté d' endommagement des bouchons d'adhésif. Il se confirme donc que ces bouchons ont une excellente tenue dans le temps et qu'ils n'altèrent pas la durée de vie potentielle des fibres objet des tests, laquelle est supérieure à douze années hors vieillissement chimique.The tests were continued until a number of cycles greater than 100,000 was obtained without any damage to the adhesive plugs being observed. It is therefore confirmed that these plugs have excellent resistance over time and that they do not alter the potential lifespan of the fibers under test, which is more than twelve years excluding chemical aging.
Il ressort donc des résultats des tests effectués sur des fibres réparées en mettant en œuvre le procédé de l'invention, que celles-ci retrouvent immédiatement leurs performances mécaniques et séparatives d'origine. En effet, quel que soit le type de « fatigue » que les fibres aient subi (attaque acide, basique, bactériologique ou par des détergents) les bouchons d'adhésif formés selon l'invention adhèrent, de façon irréversible, à la membrane et ne se décollent plus de la fibre réparée. Par ailleurs, le fait que l'on ait observé, après réparation, que les fibres soumises à une pression interne croissante éclatent toujours en dehors des emplacements comportant des bouchons d'adhésif, démontre bien la très grande fiabilité des réparations effectuées par la mise en œuvre du procédé objet de l'invention.It therefore appears from the results of the tests carried out on fibers repaired by implementing the method of the invention, that these immediately recover their original mechanical and separating performance. Indeed, whatever the type of “fatigue” that the fibers have undergone (acid, basic, bacteriological attack or by detergents) the adhesive plugs formed according to the invention adhere, in an irreversible manner, to the membrane and do not more of the repaired fiber comes off. Furthermore, the fact that it has been observed, after repair, that the fibers subjected to increasing internal pressure always burst outside the locations comprising adhesive plugs, clearly demonstrates the very high reliability of the repairs carried out by placing work of the process which is the subject of the invention.
Il demeure bien entendu que la présente invention n'est pas limitée aux exemples de mise en oeuvre décrits ci-dessus, mais qu'elle en englobe toutes les variantes, en particulier, ainsi qu'on l'a déjà mentionné, l'invention n'est pas limitée à la réparation des seules fibres d'ultra-, nano et hyper-filtration, mais elle peut également s'appliquer à la réparation notamment de fibres de microfiltration de perméation de gaz, de pervaporation etc.... It remains to be understood that the present invention is not limited to the examples of implementation described above, but that it encompasses all variants thereof, in particular, as already mentioned, the invention is not limited to the repair of only ultra-, nano and hyper-filtration fibers, but it can also be applied to the repair in particular of microfiltration fibers of gas permeation, of pervaporation etc ...

Claims

REVENDICATIONS
1 - Procédé de réparation de membranes, notamment d'ultra-, nano- et hyper-filtration, en particulier en configuration de fibres creuses tubulaires qui consiste, après détection et localisation d'une fuite dans une fibre endommagée, à y injecter un adhésif réticulable, ce procédé étant caractérisé en ce que l'on injecte dans la fibre endommagée un bouchon d'une quantité précisément dosée d'un adhésif synthétique mono-composant et on effectue le durcissement dudit bouchon d'adhésif par réticulation/polymérisation sous rayonnement ultra-violet avec une focalisation de ce rayonnement sur la section de la fibre à réparer, sous une forte densité de flux sous forme de faisceau parallèle, par l'intermédiaire d'un guide d' onde .1 - Method for repairing membranes, in particular of ultra-, nano- and hyper-filtration, in particular in configuration of hollow tubular fibers which consists, after detection and localization of a leak in a damaged fiber, in injecting an adhesive therein crosslinkable, this process being characterized in that a plug of a precisely dosed amount of a mono-component synthetic adhesive is injected into the damaged fiber and the curing of said adhesive plug is carried out by crosslinking / polymerization under ultra radiation -violet with a focusing of this radiation on the section of the fiber to be repaired, under a high flux density in the form of a parallel beam, by means of a waveguide.
2 - Procédé selon la revendication 1, caractérisé en ce que l'on utilise un adhésif qui est une résine synthétique.2 - Method according to claim 1, characterized in that an adhesive is used which is a synthetic resin.
3 - Procédé selon la revendication 1, caractérisé en ce que la hauteur du bouchon d'adhésif injecté est de l'ordre de 6 +/- 1 mm. 3 - Method according to claim 1, characterized in that the height of the injected adhesive plug is of the order of 6 +/- 1 mm.
PCT/FR2001/003476 2000-11-20 2001-11-08 Improvements to methods for repairing by sealing hollow fibres of membranes, in particular, ultrafiltration, nanofiltration, and hyperfiltration membranes WO2002040140A1 (en)

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AU2002223043A1 (en) 2002-05-27

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