Method of removing filling fluid and other soluble residues from the bore cavity of hollow fibres
Abstract
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Expired 3 June 2015, 11.3 years ago.
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12 claims: 12 independent, 0 dependent
- 1Process for removal of a lumen filler and/or other soluble residues from hollow filaments, whereby the hollow filaments of finite length are combined into bundles and the lumen filler is first roughly removed by means of centrifuging, the bundles are cleaned by feeding a solvent and centrifuging, and the solvent is then evaporated by means of a gas, characterized in that the cleaning with solvent is carried out by end spraying together with centrifuging of the hollow filament bundles, and spraying is carried out in at least two steps. Procédé permettant de débarrasser des fibres creuses de la substance médullaire et/ou d'autres résidus solubles, dans lequel des fibres creuses d'une longueur définie sont réunies par faisceaux et la substance médullaire est, dans un premier temps, éliminée grossièrement par centrifugation, les faisceaux sont ensuite nettoyés par passage d'un solvant et centrifugation, puis le solvant est évaporé à l'aide d'un gaz, lequel procédé est caractérisé par le fait que le nettoyage par un solvant se fait par aspersion frontale sous centrifugation des faisceaux de fibres, et par le fait que cette aspersion se fait en au moins deux étapes. Verfahren zur Entfernung eines Lumenfüllers und/oder anderer löslicher Rückstände aus Hohlfäden, bei dem die Hohlfäden endlicher Länge zu Bündeln zusammengefaßt werden, und der Lumenfüller zunächst grob durch Zentrifugieren entfernt wird, die Bündel durch Zuführen eines Lösemittels und Zentrifugieren gereinigt werden und anschließend das Lösemittel mit Hilfe eines Gases verdunstet wird, dadurch gekennzeichnet, daß die Reinigung mit Lösemittel durch stirnseitiges Besprühen bei gleichzeitigem Zentrifugieren der Hohlfadenbündel durchgeführt wird und das Besprühen in mindestens zwei Stufen erfolgt.
- 2Process according to Claim 1, characterized in that the spraying is carried out in at least three steps, whereby the first step is carried out in a pass-through mode and spraying in further steps is carried out in a recirculation process. Procédé selon la revendication 1, caractérisé en ce que l'aspersion se fait en au moins trois étapes, la première étape consistant en un passage unique du solvant et l'aspersion des étapes ultérieures étant réalisée en boucle. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Besprühen in mindestens drei Stufen erfolgt, wobei die erste Stufe im Durchlauf und die Besprühung der weiteren Stufen im Kreislaufverfahren erfolgt.
- 3Process according to Claim 2, characterized in that solvents containing lumen fillers and/or soluble residues are collected from each step separately, whereby the solvent of the first step is fed to the recovery process and the solvents of the further steps are used for spraying in a lower-order step. Procédé selon la revendication 2, caractérisé en ce que l'on recueille séparément les solvants contenant la substance médullaire et/ou les résidus solubles de chaque étape, le solvant de la première étape étant ensuite dirigé vers une étape de recyclage et les solvants des autres étapes étant utilisés pour l'aspersion dans une étape de rang inférieur. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß man die Lumenfüller und/oder lösliche Rückstände enthaltende Lösungsmittel von jeder Stufe für sich sammelt, wobei das Lösemittel der ersten Stufe der Rückgewinnung zugeführt wird und die Lösemittel der weiteren Stufen zum Besprühen in einer niederen Stufe verwendet werden.
- 4Process according to Claims 2 or 3, characterized in that the spraying of the hollow filament bundles takes place in up to eight steps, whereby the second and the subsequent steps are carried out under recirculation in such a way that the solvent applied is collected after the pass through the bundles and is redirected to the ends of the bundles until the content of lumen filler in the solvent remains approximately constant. Procédé selon la revendication 2 ou 3, caractérisé en ce que l'aspersion des faisceaux de fibres creuses se fait en jusqu'à huit étapes, la deuxième étape et les suivantes se faisant en boucle, à savoir par captage du solvant chargé ayant traversé les faisceaux et réintroduction frontale de celui-ci dans les faisceaux jusqu'à ce que la teneur en substance médullaire du solvant soit à peu près constante. Verfahren nach Anspruch 2 oder 3, dadurch gekennzeichnet, daß die Besprühung der Hohlfadenbündel in bis zu acht Stufen erfolgt, wobei die zweite und die folgenden Stufen im Kreislauf derart duchgeführt werden, daß das beaufschlagte Lösemittel nach dem Durchlauf durch die Bündel aufgefangen und den Bündeln wieder stirnseitig solange zugeführt wird, bis der Gehalt an Lumenfüller im Lösungsmittel in etwa konstant bleibt.
- 5Process according to one of Claims 2 to 4, characterized in that the last step is carried out under recirculation until a constant concentration of at most 400, preferably at most 250 or 200 ppm of lumen filler or soluble residues, respectively, has been attained. Procédé selon une des revendications 2 à 4, caractérisé en ce que la dernière étape est réalisée en boucle jusqu'à obtention d'une concentration constante en substance médullaire et/ou en résidus solubles, qui est au plus égale à 400 ppm, et de préférence au plus égale à 250 ou 200 ppm. Verfahren nach einem der Ansprüche 2 bis 4, dadurch gekennzeichnet, daß die letzte Stufe im Kreislauf durchgeführt wird, bis eine konstante Konzentration von höchstens 400, vorzugsweise höchstens 250 bzw. 200 ppm an Lumenfüller und/oder löslicher Reste sich eingestellt hat.
- 6Process according to Claim 5, characterized in that in the last step fresh solvent containing at most 20 ppm of lumen filler is used. Procédé selon la revendication 5, caractérisé en ce que l'on utilise pour la dernière étape du solvant frais contenant au plus 20 ppm de substance médullaire. Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß man für die letzte Stufe frisches Lösemittel mit einem Gehalt von höchstens 20 ppm an Lumenfüller verwendet.
- 7Process according to Claim 6, characterized in that in the last step solvents containing at most 5 ppm of lumen filler are used. Procédé selon la revendication 6, caractérisé en ce que l'on utilise pour la dernière étape du solvant contenant au plus 5 ppm de substance médullaire. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß in der letzten Stufe Lösemittel mit einem Gehalt von höchstens 5 ppm an Lumenfüller verwendet werden.
- 8Process according to one of Claims 1 to 7, characterized in that the hollow filament bundles are radially arranged in groups in the centrifuge. Procédé selon l'une quelconque des revendications 1 à 7, caractérisé en ce que les faisceaux de libres creuses sont disposés radialement, par groupes, dans la centrifugeuse. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß die Hohlfadenbündel in Gruppen in der Zentrifuge radial angeordnet werden.
- 9Process according to one or more of Claims 1 to 8, characterized in that the lumen filler and solvent are recovered from the solvent collected in the first step, which has a high content of lumen filler. Procédé selon une ou plusieurs des revendications 1 à 8, caractérisé en ce que l'on récupère la substance médullaire et le solvant à partir du solvant provenant de la première étape, fortement enrichi en substance médullaire. Verfahren nach einem oder mehreren der Ansprüche 1 bis 8, dadurch gekennzeichnet, daß aus dem in der ersten Stufe gesammelten, stark mit Lumenfüller angereicherten Lösemittel der Lumenfüller und das Lösemittel wiedergewonnen wird.
- 10Process according to one or more of Claims 1 to 9, characterized in that solvent 0.3 to 10 times the hollow filament volume is employed for the individual steps. Procédé selon une ou plusieurs des revendications 1 à 9, caractérisé en ce que l'on utilise pour les différentes étapes une quantité de solvant équivalente à 0,3 - 10 fois le volume de la fibre creuse. Verfahren nach einem oder mehreren der Ansprüche 1 bis 9, dadurch gekennzeichnet, daß für die einzelnen Stufen das 0,3 bis 10-fache des Hohlfadenvolumens an Lösungsmittel eingesetzt wird.
- 11Process according to Claim 10, characterized in that solvent 0.6 to 5 times the hollow filament volume is employed for the individual steps. Procédé selon la revendication 10, caractérisé en ce que l'on utilise pour les différentes étapes une quantité de solvant équivalente à 0,6 - 5 fois le volume de la fibre creuse. Verfahren nach Anspruch 10, dadurch gekennzeichnet, daß für die einzelnen Stufen das 0,6 bis 5 fache des Hohlfadenvolumens an Lösungsmittel eingesetzt wird.
- 12Apparatus for carrying out a process for removal of a lumen filler and/or other soluble residues from hollow filament bundles by means of centrifuging and flushing with a solvent or cleaning agent, consisting of means for introducing and draining lumen filler and flushing agent as well as for operating the centrifuge, and common centrifuge accessories, characterized in that an extractor basket (4) with receptacles (15) for radial insertion of hollow filament bundles, spacers (16) for securing the receptables (15) and a distributor (7) with spraying nozzles (8) for end spraying of the hollow filament bundles. Dispositif pour réaliser un procédé permettant de débarrasser des faisceaux de fibres creuses de la substance médullaire et/ou d'autres résidus solubles par centrifugation et rinçage avec un solvant ou un agent de nettoyage, lequel dispositif comprend des moyens d'arrivée et de sortie de la substance médullaire et de l'agent de rinçage, des moyens permettant de faire fonctionner une centrifugeuse ainsi que des accessoires de centrifugation habituels, caractérisé par un panier d'essorage perforé en fil (4) pour centrifugeuse comportant des emplacements (15) pour l'insertion radiale de faisceaux de fibres creuses. des dispositifs d'espacement (16) permettant de bloquer les emplacements (15), et par un distributeur (7) comportant des buses d'aspersion (8) pour l'aspersion frontale des faisceaux de fibres creuses. Vorrichtung zur Durchführung eines Verfahrens zum Entfernen eines Lumenfüllers und/oder anderer löslicher Rückstände aus Hohlfadenbündeln mittels Zentrifugieren und Spülen mit einem Lösungsmittel bzw. Reinigungsmittel bestehend aus Mitteln zum Zu- und Ableiten von Lumenfüller und Spülmittel sowie zum Betreiben der Zentrifuge und üblichem Zentrifugenzubehör, gekennzeichenet durch einen Zentrifugensiebkorb (4) mit Plätzen (15) zur radialen Einlage von Hohlfadenbündeln, Abstandshaltern (16) zur Sicherung der Plätze (15) und einen Verteiler (7) mit Sprühdüsen (8) zum stirnseitigen Besprühen der Hohlfadenbündel.
Independent claims12
29 paragraphs, as filed
The invention relates to the removal of a lumen filler And / or other soluble residues from hollow fibers.
The production of hollow fibers, in particular of hollow-fiber membranes, From various organic or synthetic Polymers is widely known. In extrusion Of the spinning solution required for the production of hollow fibers Is used to ensure the lumen (inner cavity of the hollow thread) Usually a liquid (lumen filler) into the From a ring spinning nozzle. Only fluids can be used for the lumen filler Neither change the polymer of the hollow filament, Production of the hollow filament.
Thus, for example, for the production of cellulosic Hollow thread membranes Isopropyl myristate as lumen filler Is used. This lumen filler can be used with Fluorocarbons (CFCs) from the membrane But this creates the problem that then Also the cleaning agent completely, for example By rinsing with a gas, from the membrane have to be. In addition, the use of CFCs due to the very Negative environmental influences.
For other polymers, such as, for example, polyamides, Polyacrylonitrile or polyethersulfone are each specific Lumen filler required, which can only be used with specific Remove solvents from the membrane. Also In this case, solvents which have a Significant environmental pollution and / or only with Can be removed.
There are already various methods for removing Lumen fillers made of hollow fibers. For example Are easily volatilized in the production of hollow fibers Lumen filler used by gassing under pressure easily Can be removed again from the hollow threads. For the production Of cellulosic hollow fibers is however a more volatile one Lumen Filler has not been found so far. Also For other hollow filaments in which higher-boiling lumen fillers Must be used, a direct removal of the Lumen filler by a gas, if appropriate under the action Of heat, not possible or only with very high time.
DD-A-224 343 discloses a device for removing Lumen fillers made of hollow fibers, in which Hollow fiber bundles are arranged radially in a centrifuge, In order to initially expel the largest proportion of lumen fillers. Thereafter, the discharge side of the hollow-fiber bundle becomes And the hollow-fiber bundles with solvent Flooded so that it is completely immersed in solvent are. The solvent containing lumen filler is then spun off (Microbial cleaning). Then a fine cleaning Carried out by constantly supplying new solvents and Is thrown off. Subsequently, the solvent is mixed with Aid of a gas evaporates, whereby the centrifuge further in Operation. The described working procedure with the help of Of the known device requires considerable amounts Solvent and cleaning gas, so that this process can be carried out as Uneconomical.
Further, in DD-A-219804, a method for removing Of lumen fillers from hollow fibers, in which the lumen filler First roughly removed, the bundle with a A rinsing agent, which is a solvent for the lumen filler, Can be cleaned in two stages by means of end-face flooding And then removing the solvent by means of a gas becomes. This method is used for rolled hollow filament mats applied. In this case as well, enormous amounts are generated Solvent and gas.
The last two procedures must also be uneconomical Because a considerable energy expenditure Is required, the lumen filler, the solvent And the gas exiting from the centrifuges emerging from the centrifuge Considerable solvent quantities or gas quantities. The reason for the present invention The problem is therefore a method for removing A lumen filler and / or other soluble residues Hollow filaments, in which the hollow filaments of finite length become bundles And the lumen filler is initially coarse Is removed by centrifugation, the bundles with one Solvent by feeding detergent and Centrifugation, and then the Solvent is removed with the aid of a gas Where the environmentally harmful Influences are minimized, and in which a more economical Use of solvents and gas is possible.
According to the invention, this problem is solved in that the Cleaning with solvent by spraying on the front side Hollow fiber bundle is carried out and the spraying in At least two stages. Preferably, Spraying in at least three stages, the first stage In the passage and the spraying of the further steps in the Cycle. It is advantageous Lumen fillers and / or soluble residues Dissolve solvent from each stage separately, and then The solvent of the first stage is recycled And the solvents of the further stages for spraying In a lower step.
For the purposes of the present invention, Spray any solvent on the face Simultaneous centrifugation, as a result of which The solvent passes the bundle due to the centrifugal force Flows through the entire cross-section such that the solvent Without any significant impairment both outside the Along the hollow fibers as well as inside through the hollow threads . For this purpose, the bundles are arranged in the direction, In which direction the centrifugal force acts, Namely in such a way that the longitudinal axis of the bundles, Predominantly radially outwards in the centrifuge chamber are.
Due to the fact that during a further removal of the lumen filler The solvent containing a lumen filler Previous higher level Saves considerable amounts of solvents.
The process according to the invention is particularly successful when the Spraying of the hollow-fiber bundles takes place in up to eight stages, Wherein, after the first stage, spraying in the circuit takes place in such a way That the solvent applied is, according to The passage through the bundles and the bundles Is applied again on the end face until the content of Lumen fillers and / or soluble residues in the solvent At least approximately constant. To that extent is in everyone Effective control over what is still available Residual content of lumen fillers in the hollow filament.
In order to maintain a consistently low content of lumen fillers in the hollow thread, Which is clearly below the permissible content, In particular, a method is preferred, In which the last stage in the circuit is also carried out becomes. In this case, it has proven to be particularly useful when for last Stage with a rinsing agent with as low as possible Content of lumen fillers or soluble residues, eg at most 20 ppm. Preferably at most 5 ppm. Is started. By the salary in the highest and last stage of the The residual content of lumen fillers can be determined by spraying on the face In the hollow thread.
It is advantageous to drive the last cleaning stage, That the constant concentration in the circuit At lumen fillers or soluble residues as far as possible Is low because this concentration is also a measure of the Purity of the finished membrane. It is advantageous when This concentration is not higher than 300-400, preferably Is not higher than 250 and 200 ppm, respectively. Is the same Concentration does not meet the quality requirements, It may be necessary eg another or Several spraying stages or the amount of detergent Per step.
It is beneficial if one is between the individual Spraying stages after completion of a cleaning step Centrifuge after a time without feeding detergent Continued as much as possible of liquid .
In the process according to the invention, First stage, enriched with lumen fillers Solvent of the lumen fillers and the solvent largely And with corresponding degrees of purity Can be reused.
The process according to the invention has proved particularly useful, When the individual steps are from 0.3 to 10 times, preferably 0.6 to 5 times, the volume of hollow fibers of the solvent Is used. This volume corresponds to that for Total cleaning.
The method according to the invention is described with reference to the following Figures and examples.
Show it:<dl tsize="8" compact="compact"><dt>FIG</dt><dd>The schematic representation of the inventive Process with 4 spraying stages</dd><dt>FIG</dt><dd>The cross-section through a centrifuge</dd><dt>FIG</dt><dd>3 shows the top view of the centrifuge according to FIG lidless </dd><dt>FIG</dt><dd>A container for a hollow-fiber bundle is used In the centrifuge.</dd></dl>
FIG. 1 shows schematically the sequence of the inventive method Process with 4 spraying stages. First The hollow fiber bundles are centrifuged (centrifugation Lumen filler), the major part of the lumen filler being removed becomes. At the first cleaning stage (cleaning centrifuge) Is prepared from liquor 3 solvent, which is already lumen filler Is sprayed on the end face of the hollow fiber bundles And into the fleet 4. Thereafter, solvent is used From liquor 2 for further removal of the lumen filler For spraying, and between extrusion 1 and liquor 2 In circulation.
After completion of this second step, the solvent is removed from the mixture Liquor 2 in liquor 3. In the third step (Extr. 2), solvent from liquor 1 is used, whereby between Extr. 2 and liquor 1 is circulated. After completion The third stage is the solvent from liquor 1 in Fleet 2 drained. In the fourth stage, Fleet 0, which previously from the tank bearing with pure or recovered Solvent, the final cleaning was carried out, Where in the cycle between extrusion 3 and liquor 0. To achieve the desired final cleanliness in the hollow fibers To reach, may be solvent in this stage The tank storage tank or with fresh solvents Can be re-cycled again if the Content of lumen filler in the solvent over a predetermined Value, eg 400 ppm, increases. Upon completion of the final cleaning, The fourth stage is the solvent from liquor 0 Into the liquor 1. Fleet 0 can be for the next Re-processing must be refilled. After the fourth Stage, dry gas is now applied to the bundles and Through which it passes, and here also in the circuit (Between drying cycle and centrifuge drying) Can be driven. The solvent is evaporated. The cleaned and dried bundles are then added Sorting and packaging. From the dry gas Solvent is again condensed out. The solvent from The liquor 4 is recycled, the recovered liquor being recycled Solvent again to the tank bearing extracting agent Respectively. The recovered lumen filler can Can be used again to produce new hollow fibers. The lumen filler obtained during centrifugation is likewise used (Not shown) and can then be returned to the Manufacture of hollow fibers.
FIG. 2 shows a device for carrying out the inventive method Centrifuge in the cross-section, in FIG. 3 In plan view. 1 is the centrifugal outer wall And 2 of the centrifuge covers. The centrifuge cap Can be opened or closed by the means 3 will. These means are not explained in more detail here. Centrifugal sieve basket 4 is a hollow-fiber bundle 5 radially inserted, as is particularly clear FIG. For this purpose, the centrifuge sieve basket 4 places 15 are provided, which are secured by spacers 16 are. A solvent can flow in the direction of the arrow A via the flange 6 Can be supplied to the distributor 7, spray nozzles 8 for Uniform spraying of the hollow-fiber bundles on the end face 5. Due to the centrifugal force of the high - Rotating rotating centrifuge strainer becomes the solvent Through the hollow-fiber bundles, namely between the hollow threads And forced outwardly through the lumen of the hollow fibers, Where it is collected by the wall 1 of the centrifuge And via the inclined centrifuge bottom 9 to the neck 10 And is drawn off in the direction of the arrow B. At the Of the dry stage (evaporation of the residual solvent), The drying gas is directed in the direction of the nozzle 11 Of the arrow C and via the connection piece 12 in the direction Of the arrow D again. As is common practice The centrifuge is fixed on a floor 13 which is supported on the base 13 Vibration damper 14 is supported.
For the insertion of the hollow-fiber bundles 5, containers 18, As shown in FIG. The container 18 consists From a U-shaped bent sheet, wherein the one side of the U is closed by a screen plate 19. Hollow filament bundles 17 are inserted into the U-shaped container 18, One end face of which lies flush against the screen plate 19. After insertion of the hollow-fiber bundles, this is arranged in the U-shaped Container by one or more rod (s) 20.
Examples:
13 000 hollow filaments with a length of 178 mm become bundles combined. The hollow fibers had a lumen (inner diameter) Of 200 μm. In 8 U-shaped containers 150 bundles of hollow filaments were inserted in each case and these 8 containers are placed in a centrifuge in such a way that all Hollow threads and thus also the hollow-fiber bundles in the centrifuge Were radially aligned. The total length of the Centrifuge was about 2800 km. At the The hollow fibers were cellulosic hollow-fiber membranes, Which contained isopropyl myristate (IPM) as lumen fillers. Isopropyl alcohol (IPA) was used as the solvent. Solvents may also be used as solvents Such as IPA / glycerin / water.
After inserting all the U-shaped containers, the centrifuge was placed Closed and the lumen filler centrifuged. After that Was still present in the hollow-fiber bundles about 1270 g IPM. Subsequently, the removal of the remaining Lumen filler by applying different step numbers The first stage being in each case arranged in the Flow and the further stages in the circuit operated Have been. The following table shows the consumption of Solvent (IPA), when the purification is performed in 1, 2, 3, 4 or 5 steps.
When pure isopropyl alcohol is used as a rinsing agent It is necessary to re-homogenize the plasticizer such as glycerin From the inside and outside. This can be done with the same Apparatus and by spraying. <tables><table><tgroup cols="8"><tbody><row><entry align="left" /><entry align="left">Residual IPM after centrifugation</entry><entry align="right">G</entry><entry align="right">1270</entry><entry align="right">1270</entry><entry align="right">1270</entry><entry align="right">1270</entry><entry align="right">1270</entry></row><row><entry align="left" /><entry align="left">Consumption IPA</entry><entry align="right">kg</entry><entry align="right">2000</entry><entry align="right">1033</entry><entry align="right">295</entry><entry align="right">177</entry><entry align="right">147</entry></row><row><entry align="left" /><entry align="left">IPM content</entry><entry align="right">ppm</entry><entry align="right">633</entry><entry align="right">1224</entry><entry align="right">4287</entry><entry align="right">7131</entry><entry align="right">8548</entry></row><row><entry align="left">step 1</entry><entry align="left">Continuous IPM content</entry><entry align="right">ppm</entry><entry align="right">10</entry><entry align="right">230</entry><entry align="right">817</entry><entry align="right">1356</entry><entry align="right">1630</entry></row><row><entry align="left">Level 2</entry><entry align="left">Circulation IPM content</entry><entry align="right">ppm</entry><entry align="right" /><entry align="right">10</entry><entry align="right">226</entry><entry align="right">741</entry><entry align="right">1136</entry></row><row><entry align="left">level 3</entry><entry align="left">Circulation IPM content</entry><entry align="right">ppm</entry><entry align="right" /><entry align="right" /><entry align="right">10</entry><entry align="right">251</entry><entry align="right">664</entry></row><row><entry align="left">Step 4</entry><entry align="left">Circulatory IMP content</entry><entry align="right">ppm</entry><entry align="right" /><entry align="right" /><entry align="right" /><entry align="right">10</entry><entry align="right">221</entry></row><row><entry align="left">Step 5</entry><entry align="left">Circulation IPM content</entry><entry align="right">ppm</entry><entry align="right" /><entry align="right" /><entry align="right" /><entry align="right" /><entry align="right">10</entry></row></tbody></tgroup></table></tables>
As is clear from the table, the Solvent consumption surprisingly with application of the According to the invention. It is Pointed out that in the described prior art (DD-A-224 343 and DD-A-219 804, respectively) the hollow filaments first Completely dipped in solvent and then the solvent Is discharged. The consumption of IPA is clear Above the 2-step process indicated in the table, If the same membrane quality is set. Takes The same amount of detergent, the remainder is present Lumen fillers in the hollow fibers significantly higher.
The invention also relates to a device For carrying out a method for removing a lumen filler And / or other soluble residues from hollow fiber bundles By means of centrifugation and rinsing with a Solvents or cleaning agents, such as those described in more detail Is explained with reference to FIGS. 1, 2, 3 and 4. In addition to the usual resources, Discharge of lumen fillers, rinsing agents and for operation Of the centrifuge with a centrifuge sieve basket 4 Places 15 for the radial insertion of hollow-fiber bundles, spacers 16, a distributor 7 with spray nozzles 8 to the Face spraying of the hollow fiber bundles.
3 sheets
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Every citation, both ways
| Document | Relation | Office |
|---|---|---|
| DD219804A | Cites | German Democratic Republic (until 1990) |
| DD224343A | Cites | German Democratic Republic (until 1990) |
| DE1948190A | Cites | Germany |
| DE3934406A | Cites | Germany |
| EP0018236A | Cites | European Patent Office (EPO) |
| EP0616838A | Cites | European Patent Office (EPO) |
| EP0630655A | Cites | European Patent Office (EPO) |
8 members in 6 offices
Priority claims9
| Document | Office | Kind | Date |
|---|---|---|---|
| 4423167 | Germany | A | |
| 4423167 | Germany | A | |
| 4423167 | Germany | – | |
| 9502118 | European Patent Office (EPO) | W | |
| 9502118 | European Patent Office (EPO) | W | |
| 4423167 | – | – | – |
| DE19944423167 | – | – | – |
| EP9502118 | – | – | – |
| WO1995EP02118 | – | – | – |
Members8
| Document | Office | Kind | |
|---|---|---|---|
| DE4423167A1 | Germany | A1 | |
| WO9601144A1 | World Intellectual Property Organization (WIPO) | A1 | |
| EP0716625A1 | European Patent Office (EPO) | A1 | |
| JPH09503035A | Japan | A | |
| US5779815A | United States of America | A | |
| EP0716625B1This record | European Patent Office (EPO) | B1 | |
| DE59504413D1 | Germany | D1 | |
| ES2125623T3 | Spain | T3 |
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| (expected) grantORIGINAL CODE: 0009210GRAA | GRAA | EP | |
| Despatch of communication of intention to grant a patentORIGINAL CODE: EPIDOS IGRAGRAH | GRAH | EP | |
| Despatch of communication of intention to grantORIGINAL CODE: EPIDOS AGRAGRAG | GRAG | EP | |
| Despatch of communication of intention to grant a patentORIGINAL CODE: EPIDOS IGRAGRAH | GRAH | EP | |
| Despatch of communication of intention to grantORIGINAL CODE: EPIDOS AGRAGRAG | GRAG | EP | |
| First examination report despatched17Q | 17Q | EP | |
| Request for examination filed17P | 17P | EP | |
| Designated contracting statesAK | AK | EP | |
| Public reference made under article 153(3) epc to a published international application that has entered the european phaseORIGINAL CODE: 0009012PUAI | PUAI | EP |
Numbers
- Publication
- 0716625
- Publication, DOCDB
- 0716625
- Publication, EPODOC
- EP0716625
- Application
- 95921825
- Application, DOCDB
- 95921825
- Application, EPODOC
- EP19950921825
Titles3
- German
- VERFAHREN ZUR ENTFERNUNG VON LUMENFÜLLERN UND ANDEREN LÖSLICHEN RÜCKSTÄNDEN AUS HOHLFÄDEN
- English
- METHOD OF REMOVING FILLING FLUID AND OTHER SOLUBLE RESIDUES FROM THE BORE CAVITY OF HOLLOW FIBRES
- French
- PROCEDE PERMETTANT D'EXTRAIRE DES CHARGES D'UN CANAL MEDULLAIRE ET D'AUTRES RESIDUS SOLUBLES DE FILAMENTS CREUX
Classification
- CPC, 5
- D01F1/08
- B01D65/02
- B01D2321/02
- B01D2321/16
- D01D5/24
- IPC, 8
- D06L1 22
- B01D11 02
- B01D63 02
- B01D65 02
- B01D69 08
- D01D5 24
- D01F1 08
- D06B5 26
Designated states7
- Contracting states, 7
- Germany
- Spain
- France
- Ireland
- Italy
- Netherlands (Kingdom of the)
- Sweden