EP0035679B1 - Procédé et appareillage pour l'hydrolyse continue de matières végétales cellulosiques pour l'obtention de sucres - Google Patents

Procédé et appareillage pour l'hydrolyse continue de matières végétales cellulosiques pour l'obtention de sucres Download PDF

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Publication number
EP0035679B1
EP0035679B1 EP81101260A EP81101260A EP0035679B1 EP 0035679 B1 EP0035679 B1 EP 0035679B1 EP 81101260 A EP81101260 A EP 81101260A EP 81101260 A EP81101260 A EP 81101260A EP 0035679 B1 EP0035679 B1 EP 0035679B1
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stage
screw
hydrolysate
pressure
reaction
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EP81101260A
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German (de)
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EP0035679A1 (fr
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Franz Johann Reitter
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/02—Glucose; Glucose-containing syrups obtained by saccharification of cellulosic materials

Definitions

  • the invention relates to a process for the continuous hydrolysis of pentosan-containing hemicelluloses, cellulose and corresponding compounds in vegetable biosubstance to sugar, in which the biosubstance, which has been suitably pre-comminuted, is subjected to temperature and pressure conditions in a first stage in the presence of dilute acid, in which essentially the hemicelluloses and only partially the cellulose are hydrolyzed to pentoses and partially hexoses during a first reaction time, whereupon the reaction mixture suddenly relaxes on the one hand and on the other hand the hydrolyzate is separated from the biosubstance, in at least one further stage in the presence of dilute mineral acid and under increased temperature and pressure conditions cellulose in the biosubstance is hydrolyzed to hexoses during a further reaction time, whereupon the reaction mixture suddenly relaxes again on the one hand and the hydrolyzate from the remaining bios on the other hand substance is separated, and the hydrolysis in each hydrolysis stage is carried out in a continuous horizontal tube cooker as the reaction space
  • DD-A-130 582 has already proposed the use of a tubular reactor provided with movable internals for carrying out short-term intensive hydrolysis, into which the biomass is to be fed against the internal pressure with a plug-forming, conical feed screw with acid supply.
  • the discharge device can be a screen screw press, which enables the liquid to be separated under pressure, which enables a partial dehumidification of the residue and a separate expansion of the liquid and residue.
  • the object of the present invention is to provide specific procedural and corresponding device-specific configurations of the method with which a short-term reaction is possible under improved conditions.
  • the aim is to further reduce the energy requirement compared to known working methods and to increase the yield of sugars obtained.
  • This object is achieved according to the invention for a process of the type mentioned at the outset by largely removing air and excess liquid in the filling screw in the biosubstance, carrying out the hydrolysis in the reaction chamber in the vapor phase and the hydrolyzate behind each hydrolysis stage in several separation stages from the reaction mixture is separated.
  • the word “continuously” refers primarily to the course of the process within a hydrolysis stage.
  • the at least two-stage hydrolysis process according to the invention can therefore, if necessary, also be carried out with a one-stage system by operating it intermittently as the first stage or subsequent stage. In larger systems, however, the system should also be designed in several stages, since certain circuit advantages according to the invention can only be achieved with a multi-stage system.
  • the perforated casing of the filling screw makes it possible to introduce the pre-shredded material largely free of excess liquid and, more importantly, largely free of air pockets, which have a negative effect on the chemistry of hydrolysis, into the pressurized reaction space in the digester .
  • the biosubstance comes into contact with liquid before it enters the reaction space.
  • the biosubstance is expediently pre-impregnated with the mineral acid-containing digestion liquid before entering the first hydrolyzing stage. For a perfect impregnation it is necessary to work with a certain excess of liquid, which can be reduced to the level provided for the hydrolysis again without a further process step by means of the perforated filling screw upstream of the cooker.
  • the tube cooker itself offers the possibility of carrying out the hydrolysis with the shortest reaction times and with the least possible excess of liquid in the vapor phase, with considerable immediate energy savings in the cooking and secondary energy savings resulting from the fact that the hydrolyzate is obtained in a relatively high concentration.
  • the reaction mixture can be discharged from the cooker by means of a known blow valve via a blow line into a cyclone-like blow tank.
  • the separation of the hydrolyzate from the reaction mixture is followed by the sudden expansion, namely the blowing out of the reaction mixture from the cooker.
  • the multistage removal of the hydrolyzate from the reaction mixture behind each hydrolyzation stage is expediently carried out in countercurrent to the hydrolyzate, with separation here being understood to mean practically countercurrent washing with the lowest possible hydrolyzate dilution, in which the last separation stage is generally carried out with fresh water for washing out the organic substance, and the concentrated hydrolyzate to be fed for further processing is removed from the first separation stage following the cooker alone.
  • Separating screws and / or twin-wire presses are advantageously used as separating or separating devices. In general, a three-stage hydrolyzate separation is sufficient for the process.
  • separating screws should be understood to mean screw presses which are similar in principle to the filling screws. They are provided with a perforated jacket for liquid separation, but, if they are not required to work against a container pressure, do not need to form a pressure-stopper and can also be operated with less compression if required.
  • the hydrolyzate is separated off, at least in the first separation stage, while the pressure in the reaction space is closed, the sudden expansion of the reaction mixture into the blow tank only taking place after this first separation stage.
  • the first separating device consists of a screw separator which is connected directly to the discharge end of the tube cooker and forms a unit under pressure with the cooker.
  • the screw separator is provided outside of its conical, perforated casing with a pressure-resistant housing arranged at a distance from the casing, through which only the plug tube at the end of the screw casing is passed.
  • the separated liquid collects in the pressure-resistant housing and can be drawn off via an outlet line under pressure or via a pressure relief valve.
  • the reaction mixture or the mass remaining after the first hydrolyzate separation is blown out of the plug tube of the screw separator into a blow tank via a blow line. Further separation stages for the hydrolyzate separation can then follow the blow tank.
  • it can be expedient to blow out the hydrolyzate separated in this screw separator into a separate blow tank via a blow valve. If work is to be carried out in the complete countercurrent of the hydrolyzate for the hydrolyzate separation, this must be raised to the corresponding pressure level of the boiler outlet for the first separation stage by means of a pump.
  • This embodiment of the method or the system provided for carrying out the method has the advantage that a separate blow valve for the solid substance on the stove. which u. U. has a certain susceptibility to failure, can be dispensed with.
  • the discharge end of the cooker is formed solely by the separating screw and its conical jacket.
  • the metered discharge of the reaction mixture from the cooker takes place by a corresponding rotary movement of the screw. It is not absolutely necessary to squeeze the hydrolyzate in the screw separator, since hydrolyzate separation is already caused by a pressure difference between the interior of the cooker and the shell of the screw giving housing can take place.
  • Another advantage of this procedure is that, for example, in a two-stage process, the hydrolyzate separated in the second stage can be kept under such a pressure that either the steam escaping from the hydrolyzate with a certain relaxation can be used to heat the first stage, or the hydrolyzate itself can be used as an acidic disintegrant under pressure for simultaneous heating in the first hydrolyzing stage.
  • the latter option is only available if the hydrolyzates of the individual hydrolyzation stages are not to be sent directly to further processing.
  • the hydrolyzate of the second stage which generally still contains sufficient mineral acids, directly as the digestion liquid for the first hydrolysis stage.
  • the hydrolyzate would not only be conducted in the hydrolyzate separation stages following each hydrolysis stage, but through the entire system in countercurrent, so that only the hydrolyzate of the first separation stage is fed to the first hydrolysis stage for further processing.
  • the filling screw for the boiler of the next stage is expediently used at the same time as the last separation stage for the hydrolyzate separation in the previous stage.
  • these separating screws can be designed essentially in the same way as the filling screws of the cookers. This results in considerable simplifications in terms of plant technology. Since the filling screw is used anyway to remove excess liquid from the organic substance before it enters the cooker, the filling screw can also be used at the same time to remove residues of the hydrolysate produced in the previous stage from the mass.
  • a vertical downpipe is generally arranged between the filling screw and the actual cooking tube, in the upper end of which the plug of the filling screw opens horizontally.
  • This arrangement is therefore chosen in order to arrange a closure device for the mouth, a so-called “blow back damper”, opposite the mouth of the filling screw, which can be used to prevent the stove from being blown out if the pressure stop fails due to the material plug.
  • the lowest possible liquid-to-solid ratio should be aimed for, which should be in the range of 3: 1 to 1.5: 1, but preferably in the range of 2:.
  • the use of a filling screw with a perforated screw housing has the particular advantage that, even after impregnation of the organic substance in a two-cell mixer, excess digestion liquid can be squeezed out again immediately before the mass enters the cooker, without an additional process step being necessary for this. It should again be emphasized that an essential point of the claimed process is that, using a filling screw, it is possible to remove almost 100% of the air, which is extremely damaging to the hydrolysis, from the comminuted organic substance before entering the cooker.
  • the invention also relates to a system suitable for carrying out the method.
  • the above description of the features essential to the method of the invention is extensive also applicable to the associated system.
  • the process according to the invention and associated systems are explained in more detail below with reference to the attached process diagrams.
  • the comminuted and pre-cleaned organic substance at 1 reaches a double-shaft mixer 3 of known type in a conveyor belt 2, which is preferably provided with an automatic weighing device (not shown), in which the organic substance is pre-impregnated with acidic digestion liquid, which is supplied via a line 5 provided with an automatic control valve 4.
  • the digestion liquid is expediently metered as a function of the biological substance weighed in per unit of time over the conveyor belt. Blown steam from the process for heating the organic substance is additionally fed into the double-shaft mixer via a line 6.
  • the liquid is intensively mixed with the organic substance by the two rotating screws of the mixer, the liquid penetrating the moist raw material in order to prepare it for the rapid vapor phase digestion.
  • the impregnated organic substance falls by gravity through a chute 7 into the feed opening of the screw filler 8, which is part of the cooker.
  • the bio-substance is pressed into the conical shell surrounding the screw by the filling screw which is rotatably mounted in the screw filler, whereby a dense plug is formed which forms the pressure-side closure of the interior of the cooker.
  • the organic substance falls from the outlet opening of the screw filler 8 through a chamber designed as a chute 10, which opens into the horizontal cooker tube of the cooker 11.
  • the inside of the cooker 11 is provided with a screw conveyor (not shown in FIG. 1), the speed of which can be changed in order to be able to influence the residence time of the organic substance in the cooker.
  • the cooker 11 is also only shown with one cooker tube, but depending on the throughput and dwell time, it can also be designed as a two-tube cooker or as a cooker with several cooker tubes.
  • the cooker 11 is heated with steam via a line 12 with a plurality of cooker connections, which in the present exemplary embodiment, as will be explained further below, is obtained by relaxing the pressurized hydrolyzate of the second hydrolysis stage.
  • the reaction mixture falls into a discharge device, which in the exemplary embodiment consists of a pellet separator 13, which is similar in construction to the screw filler 8.
  • the reaction mixture is fed via a line 14 hydrolyzate from the second hydrolyzate separation stage operated in countercurrent.
  • the hydrolyzate separated by the cone jacket of the screw separator 13, which is the total hydrolyzate from the two hydrolysis stages shown in the circuit of the exemplary embodiment leaves the hydrolysis plant here and is fed to the intended further processing.
  • the narrowed mouthpiece of the screw separator 13 is connected via a blow line 15 to a cyclone-like blow tank 16, into which the blow line 15 is inserted tangentially at the upper end.
  • An emergency valve 17 is also provided in the blow line 15 immediately behind the mouthpiece of the screw separator 13.
  • the discharge amount from the cooker is determined by the speed of rotation of the screw.
  • the hydrolyzate is separated - by the pressure drop between the interior of the cooker 11 or the screw separator 13 and the exterior surrounding the cone housing. An additional pressing action by the screw can be advantageous, but is not absolutely necessary.
  • the residual substance remaining in the screw separator 13 after separation of the total hydrolyzate is blown out via the blow line 15 into the blow tank 16, in which a pressure release takes place, through which steam is released from the remaining reaction mixture.
  • the blow tank 16 is essentially closed and is kept under a slight excess pressure in order to catch the released steam and to feed it back into the process. As already mentioned, part of this blow steam is fed to the twin-shaft mixer 3 via the line 6. Remaining blowing steam arrives via a line 17 to other recycling points in the process.
  • the screw separator 19 also serves as a screw filler for the cooker of the following stage and thus represents the connection point between the first and second hydrolysis stages.
  • the liquid squeezed out in each screw separator is in each case returned to the previous hydrolyzate separation stage.
  • the liquid squeezed out in the screw separator 19 passes via a line 20 back into the blow tank 16 and thus before the screw separator 18, and the liquid separated therein via the already mentioned line 14 into the discharge end of the cooker 11 before the screw separator 13 directly connected to it Since this requires the liquid to be fed into the pressure chamber of the cooker, a pressure booster pump 21 is provided in line 14 in order to raise the washing hydrolyzate to the corresponding pressure level.
  • the biosubstance After the residual hydrolyzate of the first hydrolyzation stage has been largely removed from the remaining biosubstance in the worm separator 19 working as the third hydrolyzate separation stage, the biosubstance, after it has passed the mouthpiece of the worm filler 19 forming the worm filler for the second hydrolysis stage, is metered in via a line 22 mineral acid , preferably dilute sulfuric acid, added as a catalyst for the hydrolysis.
  • mineral acid preferably dilute sulfuric acid
  • the impregnated residual organic substance passes through a chute 22 'into the tube cooker 23 of the second hydrolysis stage, which is of the same type as the cooker 11 of the first hydrolysis stage, but its special data can and therefore cannot be adapted to the requirements of the second stage needs to exactly match the stove of the first stage.
  • the cooker 23 of the second hydrolysis stage which is generally operated under higher pressure than the first stage, is heated with fresh steam via a line 24.
  • the units following the boiler 23 of the second hydrolyzing stage essentially correspond to those of the first hydrolyzing stage.
  • the cooker 23 is connected at its discharge end to a screw separator 25 which is connected to a blow tank 28 via a blow line 27 provided with an additional blow valve 26. This is followed by two further screw separators 29 and 30.
  • the residual organic substance is added via a line 31 washing water, which is preferably heated and can be process water obtained elsewhere in the overall system.
  • the last washing hydrolyzate separated in the screw separator 30 is returned via a line 32 into the blow tank 28 and thus before the screw separator 29 forming the second hydrolyzate separation stage.
  • the liquid separated in this passes through a line 33 upstream of the screw separator 25, which is under boiler pressure, which is why a pressure booster pump 34 is also provided in this line 33.
  • the pressurized hydrolyzate of the second hydrolyzing stage which is separated off in the screw separator 25 connected to the cooker 23, is fed back via line 35 into the first hydrolyzing stage, first to an expansion vessel 36 from which the vapor released by expansion, such as already mentioned above, is introduced via line 12 as heating steam into the cooker 11 of the first stage.
  • the relaxed hydrolyzate of the second stage passes from the expansion vessel 36 via line 4 for pre-impregnation of the fresh organic substance into the twin-shaft mixer 3 of the first hydrolysis stage.
  • live steam is only used to heat the second stage cooker.
  • the first stage cooker is heated with the flash steam from the second stage hydrolyzate.
  • the hydrolyzate is passed through the entire system in counterflow and enriched. Washing water is added only before the last separation stage after the second hydrolysis stage.
  • the three-stage hydrolyzate separation behind the second cooker is operated in countercurrent, and the hydrolyzate separated in the first separation stage behind the second cooker, namely in the screw separator 25, is completely added to the biosubstance before the first hydrolyzing stage and enriched with the hydrolyzate of this stage within the first hydrolyzing stage , a countercurrent washout also taking place behind the first stage digester, so that the concentrated total hydrolyzate of both hydrolysis stages can be removed from the first hydrolyzate separation stage behind the first digester. Since the mineral acid-containing hydrolyzate of the second hydrolysis stage is used as the digestion liquid in the first hydrolysis stage, mineral acid need not be added again here. Fresh mineral acid is added alone before the boiler of the second hydrolysis stage. On the additional representation of known control and control devices Rules of the process flow were deliberately omitted in the process diagram of FIG. 1.
  • the method variant of FIG. 2 differs from the method diagram of FIG. 1 in that not a screw separator connected to the discharge end of the cooker 11 is connected to the discharge end of the cooker 11, but only a vessel 40 is provided, which is connected via the blow line 15 the blow tank 16 is connected.
  • the discharge from the cooker 11 is regulated solely by the blow valve 17.
  • a three-stage hydrolyzate separation by means of screw separators 18, 41 and 42 is provided behind the blow tank 16 in the variant of FIG. 2, none of these separation stages being under pressure.
  • a line 43 is led into the blow line 15, via which a neutralizing agent, preferably milk of lime, can be injected directly into the blow line.
  • a neutralizing agent preferably milk of lime
  • the mouth of the line 43 into the blow line 15, which consists of suitable injection devices, is preferably located close behind the blow valve in the practical embodiment, in order to achieve effective mixing between the reaction mixture and neutralizing agent, which is practically one, by the turbulence prevailing in the blow line abrupt neutralization of the reaction mixture should lead.
  • the second (not shown) hydrolyzing stage is operated in a corresponding manner, however, it is not possible to return the neutralized hydrolyzate from the second stage as a digestion liquid to the first stage, since the acid contained in it, necessary as a catalyst, passes through neutralization has been removed. Accordingly, fresh acid is already supplied to the first hydrolysis stage via a line 44 as a catalyst. It is introduced into the twin-shaft mixer 3 and into the screw filler 8.
  • the cooker 11 of the first stage is at least partially heated with live steam via a line 45.
  • the possibility of withdrawing part of the hydrolyzate from the second cooker immediately after the pressure has been closed, from a vessel corresponding to the vessel 40 behind the first cooker 11 without an actual separating device, and of recovering some of the steam by relaxing this hydrolyzate portion. which, as shown in the exemplary embodiment in FIG. 2, can be fed via a line 46 as partial heating steam to the lower stage cooker 11 of the first stage.
  • mixed organic matter consisting of one third of wood, residual and waste materials can be made from one ton of dry-made.
  • Grain straw and waste paper about 500 kg of sugar, and that can be produced as a mixture of pentoses and hexoses.
  • the amount of catalyst required is about 0.3% based on that raw material used.
  • the reaction time in the first hydrolysis stage is approximately 2 1/2 minutes at 180 ° C. and the reaction time in the second hydrolysis stage is approximately 4 1/2 minutes at approximately 235 ° C.
  • the remaining cellulignin after the second stage is about 25 to 28% of the starting substance and is sufficient to obtain the required process heat as a vapor by combustion at a pressure of about 28 to 30 bar.
  • the steam supply that is required for the cooking process in such a way that the steam entry is provided directly behind the entry point of the compressed biomass and such is directed to the plug that disintegration can take place through the steam.

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Claims (13)

1. Procédé pour hydrolyse continue de hémicelluloses contenant de pentosane, de cellulose et de compositions correspondantes en biosubstance végétal aux sucres dans lequel la biosubstance broyée préalablement dans une manière convenable dans une stage première en l'absence de l'acide dilué est soumise aux conditions de température et de pression, dans lesquelles essentiellement les hémicelluloses et, seulement en partie, la cellulose sont hydrolysées aux pentoses et, en partie, aux hexoses pendant un temps réactionnel, après quoi le mélange réactionnel d'une part, est subitement détendu, et d'autre part, l'hydrolysate est séparée de la biosubstance, au moins dans une autre stage en l'absence de l'acide minéral dilué et sous des conditions plus dures de température et de pression, de la cellulose dans la biosubstance est hydrolysée aux hexoses pendant un autre temps réactionnel, après quoi, encore, le mélange réactionnel d'une part, est submitement détendu, et d'autre part. l'hydrolysate est séparée de la biosubstance reste, l'hydrolyse dans chaque stage hydrolysante étant réalisée dans une bouilloire tubulaire horizontal (11. 23) continue formant l'espace réactionnel, et l'introduction de la biosubstance dans la bouilloire tubulaire horizontal (11. 23) étant effectuée par l'intermédiaire d'une vis à remplir (8. 19) formant un arrêt de pression, caractérisé en ce que de l'air contenu dans la biosubstance et du liquide en excès dans la vis à remplir soient largement enlevés, que la hydrolyse soit réalisée dans l'espace réactionnel en phase vapeur et que l'hydrolysate après chaque stage hydrolysante soit séparée dans plusieurs stages séparantes (par exemple 13, 18, 19) du mélange réactionnel.
2. Procédé suivant la revendication 1, caractérisé en ce que la biosubstance pour l'introduction dans l'espace de réaction soit condensée aux taux des volumes d'au moins 1 à 4 et comprimée à une densité d'au moins 350 kg/cm3.
3. Procédé suivant les revendications 1 ou 2, caractérisé en ce que la biosubstance introduite et pressée dans l'espace de réaction soit désintégrée par l'intermédiaire de la vapeur.
4. Procédé suivant l'une des revendications 1 à 3. caractérisé en ce que le liquide de dissolution acidifère et aqueux soit injecté directement à l'espace de réaction sous pression.
5. Procédé suivant l'une des revendications 1 à 4, caractérisé en ce que le mélange réactionnel avant ou pendant la détente subite en sortant de l'espace de réaction soit neutralisé préférablement par du lait de chaux.
6. Procédé suivant l'une des revendications 1 à 5, caractérisé en ce qu'une séparation première de l'hydrolysate du mélange réactionnel soit effectuée avant la détente subite sous arrêt sous pression de l'espace de réaction, et que l'hydrolysate séparément du reste de mélange réactionnel soit subitement détendu.
7. Appareil pour réaliser le procédé suivant l'une des revendications 1 à 6, ayant une bouilloire tubulaire horizontal actionnée continuement et pourvue à l'intérieur avec des organes de transport, bouilloire qui est solidaire au côté d'entrée à une vis à remplir ayant une vis conique pour introduire la biosubstance dans la chambre de réaction de la bouilloire, le côté de verse de laquelle étant pourvu d'un mécanisme de verse formant l'arrêt sous pression de la chambre de réaction au côté de sorti et étant solidaire par l'intermédiaire d'un tuyau à air, à un réservoir à air sous forme de cyclone, caractérisé en ce que la vis conique de la vis à remplir (8, 19) soit entourée par une enveloppe conique perforée.
8. Appareil suivant la revendication 7, caractérisé en ce que le tuyau-bouchon (115) pourvu à la fin de l'envelope conique de la vis à remplir (8.19) bouche directement dans le tube de la bouilloire.
9. Appareil suivant les revendications 7 ou 8. caractérisé en ce que les taux de la longueur au diamètre du tuyau-bouchon (115) soient au moins 2:1.
10. Appareil suivant la revendication 8 ou 9, caractérisé en ce que l'axe horizontal de la vis à remplir (8) soit à angles droits à l'axe de la bouilloire (11) et que le tuyau-bouchon (115) bouche à peu près tangentiellement au domaine supérieur du tube de la bouilloire (11).
11. Appareil suivant l'une des revendications 7 à 10, caractérisé en ce que le mécanisme de verse de la bouilloire (11) soit un séparateur à vis (13, 25) étant sous arrêt sous pression et servant d'un moyen premier à séparer l'hydrolysate, l'enveloppe conique perforée (66) duquel est entournée par un boîtier (71) étanche.
12. Appareil suivant la revendication 11, caractérisé en ce que le séparateur à vis (13, 15) essentiellement est de la même construction que la vis à remplir (8, 19).
13. Appareil suivant les revendications 11 ou 12, caractérisé en ce que dans un ensemble hydrolysant en plusieurs étapes la vis à remplir d'une stage suivante en même temps soit construite comme séparateur hydrolysant dernier de la stage préalable.
EP81101260A 1980-02-23 1981-02-21 Procédé et appareillage pour l'hydrolyse continue de matières végétales cellulosiques pour l'obtention de sucres Expired EP0035679B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81101260T ATE8275T1 (de) 1980-02-23 1981-02-21 Verfahren und anlage zur kontinuierlichen hydrolyse von cellulosehaltiger, pflanzlicher biosubstanz zur gewinnung von zuckern.

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Application Number Priority Date Filing Date Title
DE3006887 1980-02-23
DE3006887 1980-02-23

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EP0035679A1 EP0035679A1 (fr) 1981-09-16
EP0035679B1 true EP0035679B1 (fr) 1984-07-04

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US (1) US4427453A (fr)
EP (1) EP0035679B1 (fr)
JP (1) JPS57500091A (fr)
AT (1) ATE8275T1 (fr)
BR (1) BR8107083A (fr)
DE (1) DE3164501D1 (fr)
ES (1) ES499625A0 (fr)
FI (1) FI810523L (fr)
NZ (1) NZ196322A (fr)
WO (1) WO1981002428A1 (fr)

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NZ196322A (en) 1983-12-16
ES8201627A1 (es) 1981-12-16
BR8107083A (pt) 1982-01-05
ATE8275T1 (de) 1984-07-15
DE3164501D1 (en) 1984-08-09
WO1981002428A1 (fr) 1981-09-03
US4427453A (en) 1984-01-24
JPS57500091A (fr) 1982-01-21
EP0035679A1 (fr) 1981-09-16
FI810523L (fi) 1981-08-24
ES499625A0 (es) 1981-12-16

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