EP0054015B1 - Procédé et appareil pour la production de cellulose - Google Patents

Procédé et appareil pour la production de cellulose Download PDF

Info

Publication number
EP0054015B1
EP0054015B1 EP81890189A EP81890189A EP0054015B1 EP 0054015 B1 EP0054015 B1 EP 0054015B1 EP 81890189 A EP81890189 A EP 81890189A EP 81890189 A EP81890189 A EP 81890189A EP 0054015 B1 EP0054015 B1 EP 0054015B1
Authority
EP
European Patent Office
Prior art keywords
digestion
pressing
piston
press
steam
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP81890189A
Other languages
German (de)
English (en)
Other versions
EP0054015A1 (fr
Inventor
Augustin Dipl.-Ing. Dr. Raggam
Hermann Dipl.-Ing. Dr. Rabitsch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Simmering Graz Pauker AG
Original Assignee
Simmering Graz Pauker AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from AT0568080A external-priority patent/AT372425B/de
Priority claimed from AT456481A external-priority patent/AT375561B/de
Application filed by Simmering Graz Pauker AG filed Critical Simmering Graz Pauker AG
Publication of EP0054015A1 publication Critical patent/EP0054015A1/fr
Application granted granted Critical
Publication of EP0054015B1 publication Critical patent/EP0054015B1/fr
Expired legal-status Critical Current

Links

Images

Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/22—Other features of pulping processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B15/00—Details of, or accessories for, presses; Auxiliary measures in connection with pressing
    • B30B15/34—Heating or cooling presses or parts thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B9/00—Presses specially adapted for particular purposes
    • B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
    • B30B9/04—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using press rams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B9/00—Presses specially adapted for particular purposes
    • B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
    • B30B9/12—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C7/00—Digesters
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S162/00—Paper making and fiber liberation
    • Y10S162/02—Chip soaking

Definitions

  • the invention relates to a process for the production of cellulose from cellulose-containing starting materials by digestion under elevated temperature and pressure.
  • the starting materials can be e.g. Wood, straw, grass or waste.
  • Another object of the invention is a device for performing this method, in which two pistons located opposite one another are arranged in a press jacket.
  • Impregnation of the pre-shredded raw materials e.g. Wood chips are made in a conventional way by mixing the chips with a basic or acidic digestion liquid and slowly bringing them to a temperature of 80 ° to 150 ° C in large pressure vessels. The slow heating to a residence time of 0.5 to 2 hours at this temperature and the resulting pressure of up to 10 bar are necessary to ensure sufficient penetration (impregnation) of the wood chips with digestion solution. Sulfate or sulfite compounds with a chemical concentration of approximately 5 to 10% are currently preferably used as the digestion solution.
  • the ratio of the mass of the digested liquid taken up to the mass of the dry wood chips in the cooker is referred to as hydromodule H and is about 3 to 5 in the current cooking processes.
  • the impregnation can also be carried out outside the cooker in a separate apparatus.
  • DE-B-2 448 547 relates to a process for improving the heat economy when cooking lignocellulosic material in batch cookers.
  • This process actually concerns pretreatment, i.e. impregnation of wood chips in the cooker with digestion liquid using a vapor pressure or gas pressure of 1 to 5 bar, preferably 1.5 to 8 bar for a duration of 3 to 70 min, if necessary with heating to a temperature of 50 to 165 ° C, with subsequent measurement and adjustment of the liquid level in the cooker to the minimum amount of digestion liquid required for the subsequent cooking process.
  • the heating takes place either indirectly by means of a heat exchanger outside the cooker, or directly by introducing steam into the cooker.
  • This process works in the liquid phase.
  • the pressure does not vent the pore volume, but rather compresses the air in the pores so that the impregnation is incomplete. A hydromodule of 0.5 to 2 cannot be achieved with this method.
  • US-A-32 15588 relates to a process for producing pulp from wood chips in a continuously operating cooker.
  • wood chips are introduced into the upper part of the stove via a sluice, where they are subjected to high-pressure steam digestion at a temperature of 180 to 190 ° C over a period of 5 to 25 minutes.
  • the lower part of the cooker is filled approximately to the middle with digestion liquid, which enters at a temperature of 70 to 120 ° C in the lower quarter of the cooker and is partially left out at the bottom or partly in the middle of the cooker.
  • the continuously moving wood chips dip into the digestion liquid and are cooled there, where they shrink and release the highly concentrated digestion liquid with which they have been impregnated, after which they remain for 5 to 30 minutes via a lock at the bottom of the Kochers are carried out.
  • Qualitative information is given about the type of impregnation and ventilation of the wood chips.
  • Various types of impregnation should result in an essentially uniform distribution of the digestion liquid within each chip, at temperatures of 100 to 150 ° C. Venting is preferably carried out by steam treatment before impregnation, whereupon the impregnation takes place under relatively high hydrostatic pressure without air being able to enter.
  • the wood chips are first treated with steam at atmospheric pressure, whereupon they are exposed to a steam with excess pressure and then the impregnation with digestion liquid takes place by rapidly reducing the excess pressure without air being added.
  • the unnecessary digestion liquid is drained off in order to separate the impregnated wood chips from the digestion liquid.
  • a hydromodule as low as can be achieved according to the invention by mechanical pressing can never be achieved.
  • the 2: 1 ratio of digestion liquid to wood given in Example 3 of this US patent specification (it is not stated whether mass or volume ratio is meant) after the impregnation is therefore a question.
  • the steps washing, sorting, bleaching and drying are usually connected to the steps of impregnation, pressing and digestion.
  • modern pulp plants are still characterized by high energy and water consumption.
  • the high energy consumption essentially results from the heating of large quantities of liquid, especially in the case of digestion and bleaching, the long residence times, and from the poor efficiency of the heat recovery systems.
  • the thin waste liquor caused by the given processes must be thickened to a dry matter content of 55 to 65% for the subsequent combustion, which in turn requires a considerable expenditure of energy.
  • the energy expenditure A pulp mill results approximately in equal parts from pulping, bleaching, lye evaporation and cellulose drying. After all, in the most modern factories, burning the thickened waste liquor can currently achieve amounts of energy that make a pulp mill almost self-sufficient in terms of energy.
  • the invention has for its object to provide a method which is characterized by minimal energy, water and chemical consumption.
  • the methods used can be seen as the maximum possible internal measures of a pulp mill to solve their environmental problems, in addition to the energy saving primarily of the wastewater problems. Since wastewater and pulp mills are currently the most difficult to treat, minimizing the amount of wastewater is essential.
  • the method according to the invention is intended to make it possible to reduce the volume of the apparatus, so that even smaller systems which can be adapted to the amount of wood involved can be operated in an economical manner.
  • An additional object of the invention is to increase the quality of the pulp produced.
  • this is achieved according to the invention in that, by pressing impregnated starting materials, a mass ratio of the absorbed digestion liquid to the dry starting materials is set to 0.5 to 2, and that the digestion in a press device at 160 ° to 300 ° C. a time of less than 10 minutes is carried out, the heating being carried out by the direct introduction of heat.
  • a hydraulic module of 1 can be selected.
  • the direct introduction of heat can preferably by electrical heating of the impregnated starting materials at a digestion temperature of z. B. 180 ° to 220 ° C, the digestion can take place for example in 10 to 60 s. Electrical heating is advantageously carried out by resistance heating.
  • the main advantages of the process according to the invention are: short digestion times, reduced energy consumption, reduced chemical consumption, small amounts of liquid, and, as tests have shown, improved pulp quality and increased wood utilization, which means that the otherwise usual grinding process, which requires additional energy expenditure, may be dispensed with can.
  • the improved pulp quality results primarily from the favorable location of the residual lignins and hemicelluloses, which results in a particular ability to bind and bleach.
  • the cellulose chains important for the basic strength of the fibers
  • the hemicelluloses important for the binding ability in the finished paper sheet
  • the impregnation in the same press device with impregnation liquid is advantageously carried out in chemical concentrations necessary for the digestion of preferably 5 to 50%, for example 10 to 20%, and at constant pressure or in the form of pressure surges, preferably above 1 bar, for example 10 to 50 bar and 2 to 10 pressure surges, to reduce the unwetted capillary length of the starting material, the impregnation time being kept short by the applied pressure, preferably less than 10 min, expediently less than 1 min, so that it is cold and without prior venting can be impregnated.
  • This impregnation process can also be used advantageously in the case of mixtures of dry and wet starting materials.
  • impregnation itself can optionally be carried out by conventional methods in a separate plant.
  • hydromodule H 0.5 corresponding lye concentration 61%
  • the evaporation system can be omitted or the lye can be burned directly.
  • chemical cycle closing process come in de- 'nen spent liquors having a solids content of 35% in boilers for combustion, but the use of energy is correspondingly lower.
  • the measure of lowering the hydromodule H in the same way also reduces the energy consumption when digesting and evaporating the waste liquor.
  • the process according to the invention in comparison to conventional processes, corresponding to the reduced hydromodule H, with more concentrated digestion solutions and a smaller amount per Batch worked, which means that a smaller amount of concentrated fresh or waste liquor has to be processed, so that the total number of auxiliary systems is reduced in number and extent, and the theoretical chemical consumption per kg of pulp is reduced to around half of the usual consumption due to the increased concentration can.
  • the pressure when adjusting the hydromodule H can be lower if more time is available or if the temperature of the wood chips is increased so that they become more elastic and the structural resistance decreases. Temperatures up to 130 ° C have proven to be advantageous, at which no appreciable digestion reactions take place and a hydromodule H of approx. 1 is reached in approx. 30 s with mechanical pressures around 50 bar.
  • a filling density of z. B. 160 to 220 kg / m 3 for softwood stands at a mechanical pressure of, for example, 50 bar and a temperature of 130 ° C after the adjustment of the hydromodule, an increased fill density of 800 kg / m 3 . With this measure, the volume of the pressing device can be reduced to a third to a fifth of the previous volume of the pressure vessels.
  • the hydromodule changes continuously during the process and can be determined at the end of the process as a function of the reaction parameters.
  • a further embodiment of the method according to the invention provides that, in the case of wet starting materials, the moisture (water content) is brought to a value of below 50%, for example 20 to 40%, preferably 30%, by pressing off the wet starting materials in the same pressing device becomes, whereby the majority of the capillaries of the starting material for the impregnating liquid is removable.
  • the direct introduction of heat into the impregnated starting materials can also take place, for example, by capacitive or inductive high-frequency heating or by microwave heating.
  • the digestion can also take place as a continuous process step.
  • the invention is basically suitable for all digestion processes (acidic to alkaline).
  • a pressing device according to the invention for carrying out the method is characterized in that two pistons lying opposite one another are arranged in a pressing jacket, between which the compact is located as an electrical resistance load, both the pistons relative to one another and the pressing jacket being relatively movable relative to the pistons.
  • FIG. 1 to 5 each show different exemplary embodiments of discontinuously operating pressing devices according to the invention in cross section
  • FIG. 6 shows the schematic structure of a continuously working screw press in cross section according to the invention
  • FIG. 7 shows a largely simplified vertical section through a further embodiment of the pressing device .
  • a pressing device of a basic type is shown.
  • a cylindrically shaped press jacket 1 is lined with an electrical insulation 2, which also extends over the lower edge of the press jacket 1 and thus also insulates the bottom cover 3.
  • a piston 4 is pressurized in the press jacket 1, e.g. hydraulically moved up and down and is provided with a seal 5.
  • a drain opening 6 for the waste liquor, which continues in a pipeline with a valve 7.
  • the bottom cover 3 and the piston 4 are provided with electrically conductive contacts which are connected to the poles of a power source. AC sources are preferably used.
  • the mechanical pressure of the piston is superimposed on the vapor pressure which arises during the development of heat when the current passes through the compact 8.
  • Fig. 2 shows a second embodiment, similar to that of FIG. 1, but with the piston 4a is offset, and the seal 5a is laid in the upper part of the press casing 1a.
  • a measuring opening 9 for the connection of a steam pressure meter 10 is laid in the upper third of the press casing 1a.
  • the gap formed between the piston 4a and the press jacket 1a enables the steam produced to escape upwards, as a result of which steam pressure and mechanically applied pressure can be metered separately and also measured. Power is supplied as shown in Fig. 1.
  • Fig. 3 shows a third embodiment in which the electrical insulation can be made simpler.
  • a central opening is provided in the floor cover 3a, in which an electrode 11 projects into the press jacket 1.
  • Insulation 2a insulates the bottom cover 3a from the press jacket 1 and the electrode 11.
  • a cover 12 closes the press jacket 1 at the top.
  • a linkage 13 leads via the seals 14 into the interior of the press casing and is connected to a piston ring 4b.
  • the mechanical pressure is transmitted via the linkage 13 to the piston ring 4b, and from there to the compact 8.
  • a gap is provided between the piston ring 4b and the press jacket 1, and between the electrode 11 and the piston ring 4b, so that A vapor space is created above the compact 8.
  • FIG. 4 shows a fourth exemplary embodiment in which the electrode 11a has been enlarged in diameter and at the same time functions as a piston for the mechanical pressure.
  • This version proves to be advantageous due to the omission of seals; only the insulation 2a assumes a sealing function at the same time.
  • the compact is heated under mechanical pressure by heat, preferably electrical heat, i.e. H. the electrical current is conducted through the compact.
  • the electrodes are the pistons and the press jacket and their possible combinations, the electrical insulation being attached at those points in the area of the press chamber which would otherwise bridge the current flow through the compact.
  • This measure is also used for heating by inductive or capacitive HF heating, or microwave heating, and is a problem that can be solved by a person skilled in the art when specifying this criterion.
  • FIG. 5 shows a pressing device according to the invention as an exemplary embodiment in cross section.
  • 1 b denotes a hydraulically liftable and lowerable press jacket, in which a movable, likewise hydraulically liftable and lowerable upper piston 4 and a lower piston 4 ′ rigidly connected to a base plate 3 b are arranged.
  • the cloth cake or pellet 8 is located between the two pistons 4 and 4 ', which are each equipped with seals 5 b.
  • the two pistons are electrically connected to the poles of a power source via contacts.
  • Insulation 2b is provided in the press jacket 1b in order to prevent current flow through the press jacket.
  • the press jacket 1 b is attached to the base plate 3 b by auxiliary devices, e.g.
  • Hydraulic or pneumatic cylinder 15 raised and lowered, whereby an easy discharge of the compact is accomplished or the introduction of the wood chips is made possible via a funnel 16 arranged around the upper piston 2, which is carried by a rod 17 mounted on the press jacket 1 b.
  • the auxiliary device can also be of a mechanical type, e.g. B. be a spindle drive.
  • the upper piston 4 is provided with a bore 18, which serves to supply liquid or gaseous treatment media, and ends in many small bores on the end face of the piston 4, as a result of which the liquid can be fed to the compact 8.
  • a bore 19 is provided in the lower piston 4, which is used to discharge the treatment media from the press chamber and opens into many small bores on the end face of the piston 4 '. Treatment media can also be fed in and out via bores in the press jacket 1 b (not shown).
  • the treatment media can also be distributed within the press room using sieve or perforated plates, etc. (not shown).
  • an insulation 20 is provided between each cylinder 15 and a flange 21 rigidly arranged on the press jacket 1 b, so that the entire current flow is conducted over the compact 8 and heats it directly.
  • resistance heating is used, but, as mentioned, high-frequency heating of an inductive or capacitive type and microwave heating can also be used for the press jacket 1 b and the two pistons 4 and 4 'with a suitable choice of material.
  • the press jacket 1 b can, for. B. be made of high-strength ceramic insulating material.
  • a screw press 22 according to FIG. 6 is proposed, in which the impregnated wood chips are broken down optimally in a continuous form.
  • a feed screw 23 conveys the pressed material (pre-impregnated wood chips) into the cooking area, which is formed between a screw electrode 24 as the first electrode and the cooker housing 25 as the second electrode.
  • the lye escaping from the compression of the wood chips on a particular hydromodule can escape from the screw press 22 via a sieve 26 and is returned to a separate impregnation plant (not shown).
  • the feed screw 23 is connected to the screw electrode 24 via an insulating coupling 27.
  • the cooker housing 25 and the screw electrode 24 are connected to a power source via contacts. The current flows via the screw electrode 24 to the cooker housing 25 and heats the wood chip mass lying in between. If, for example, the consistency (solid concentration) of the wood chips mass can be assumed to be 50% in the inlet with a hydromodule of 1, this consistency drops to around 30% due to the increasing dissolution of the lignin against the outlet.
  • the pulp is again concentrated to about 55% in the discharge screw 28, as a result of which a large part of the primary liquor is separated off in a hot state (low viscosity) at a concentration of about 60% via a sieve 29.
  • the dwell time in the cooking area and the mechanical pressure on the wood chips can be set as desired by varying the speed between the feed and discharge screws.
  • the press jacket 1 can be raised and lowered by appropriately loading the cylinder 15 with pressure oil or the like pressure medium. In its highest position, the press jacket 1 is at a sufficient distance from the piston 4 ', so that the previously pressed material can be removed from the press jacket 1 laterally between the cylinders 15.
  • the cylinders 15 stand on a circle concentric to the press jacket 1 and have a lateral distance from one another which is greater than the inside diameter of the press jacket 1.
  • the lower piston 4 ' is attached to the foundation 3 b. It is penetrated in the axial direction by a tube 31 which is connected to a steam line 34 via a valve 32 and a valve 33. An additional valve 63 may be present.
  • the tube 31 opens at the piston head 35.
  • a filter plate or perforated plate 46 is held at a distance from the piston head 35 and has a multiplicity of small bores 47. These holes can be tapered towards the top to avoid clogging and to facilitate cleaning.
  • the sieve plate can be supported on the piston head by strips or similar stiffeners (not shown). Between the perforated plate 46 and the piston head 35, a distribution and collection space 48 is created. Between the piston 4 'and the valve 32, a branch 59 with a valve 40 is provided on the pipe 31, which leads to a liquid supply and discharge pipe 41.
  • annular seal 5b is provided, which is inserted into a circumferential groove near the piston head 35 or into the press jacket 1 near its end.
  • the upper piston 4 can be moved up and down by a hydraulic or mechanical device, not shown. It is penetrated by an axial line 43, which opens at the piston crown 44 and with its other end in a manner not shown further out of the piston and z. B. is connected via a hose 45 and a valve 42 to a liquid inlet and outlet 57.
  • the upper piston 4 like the lower one, is provided with a filter plate 46 with optionally conical bores 47, so that a distributor and collecting space 48 is also formed on the upper piston 4 between the piston crown 44 and the filter plate.
  • a circumferential groove provided in a piston crown 44 or in the press jacket 1 near its end has an annular seal 5b effecting the seal between the press jacket 1 and the upper piston 4.
  • the press jacket 1 In its upper part, the press jacket 1 is provided with a number of radial passages 52, which are closed at their inner mouth with sieve plates 38. In order to avoid damage to the ring seal 5 b by the sieve plate 38, the sieve plates are set back somewhat in relation to the inner wall of the press jacket 1.
  • a ring line 51 On the outside of the press casing 1, a ring line 51 is provided, into which all radial passages 52 open.
  • a circulation line 53 extends from the ring line 51 via a valve 62 and contains a flexible or length-variable connection (here a telescopic tube 54) and a blower 55.
  • the other end of the circulation line 53 is connected via the valve 32 to the pipe 31 leading into the lower piston 4 '.
  • the upper end face of the press casing 1 can carry a filling funnel 56 which concentrically surrounds the upper piston 4. Supports 67 serve to hold the funnel.
  • the upper piston 4 can be lifted out of the press jacket 1, so that the press jacket 1 can be filled with solid material through the annular gap between the upper piston 4 and the press jacket edge.
  • the upper piston 4 For filling the press, the upper piston 4 is moved into its highest position 'and the press belt 1 is brought by appropriately energizing the operating cylinder 15 to its lowermost position. This creates a sufficiently large space between the perforated plates 46 of the piston 4 and the upper edge of the press casing 1, through which wood chips, which could have already been introduced into the hopper 56, can fall into the interior of the press cylinder. After the desired filling quantity has been reached (if desired, with intermediate compression by the piston 4), the upper piston 4 is brought into the position shown, ie it penetrates into the press jacket 1 to such an extent that the ring seal 5 b effects the sealing of the press jacket 1, which radial passages 52 but remain free.
  • valves 32 and 33 By opening the valves 32 and 33, but with the valves 40 and 62 and possibly 63 closed, steam can be brought into the interior of the press casing 1 in order to pre-dampen the wood chips.
  • the wood chips filled in the press are very moist, they can be pressed to a desired degree of dryness. After opening the valve 40 and closing all other valves, the upper piston 4 can be lowered. Due to the resulting high pressure (e.g. 100 to 200 bar), the liquid squeezed out of them penetrates through the bore 47 in the lower perforated plate 46 and flows out via the line 41.
  • the resulting high pressure e.g. 100 to 200 bar
  • valves 32, 33 all other valves closed. This heats the impregnation liquid (also in the wood chips) above its boiling point.
  • the valves 32, 33 are closed and by opening the valve 46 (the line 57 can now lead to the outside, for example), the excess pressure is released and the impregnation liquid evaporates. This evaporation also takes place inside the wood chips, the air contained therein being displaced by steam. This procedure can be repeated several times; it is possible to completely remove the air from the wood chips, which corresponds to a «perfect impregnation».
  • the high pressure that can be achieved with the press e.g. 100 to 200 bar
  • the press can be used for the impregnation by simply pressing the upper piston 4 (all valves closed) mechanically into the pores of the wood (the wood chips) ) is pressed.
  • any hydromodule can be pressed onto any hydromodule.
  • a hydromodule of about 0.5 to 2, but preferably about 1 is pressed, i. H. the ratio between the mass of the dry wood chips and the mass of the impregnation liquid they absorb is then approximately equal to one.
  • the pressing takes place by lowering the upper piston 4, the resulting, pressed liquid, as already mentioned, being able to flow out through the valve 40 into the line 41.
  • the press jacket 1 can e.g. about half filled with already pressed wood chips, above which there is a steam-air mixture.
  • steam is again blown into the interior of the press.
  • the temperature of this steam is, for example, 10 to 50 ° above the desired final digestion temperature, which can be approximately 170 ° to 220 °.
  • the pressure of the steam preferably corresponds to the equilibrium pressure at the selected maximum digestion temperature. So it is superheated steam; when the digestion temperature is reached, the steam supply stops automatically.
  • the steam supplied condenses on the relatively cold wood chips and heats them both by the heat of condensation and by conduction.
  • the excess steam can be circulated by opening the valve 62 and starting the blower 55: sieves 38, passages 52, ring line 51, valve 62, circulation line 53, valves 63 and 32, pipe 31.
  • a swirling or intensive mixing and flow around the impregnated wood chip particles - now to be referred to as "pulping material" - is achieved.
  • This swirling of the material does not have to correspond to the ideal fluidized bed process, but only turbulent, so that the heat transfer takes place quickly and homogeneously from a static point of view. With a low filling quantity, the vortex will be strong, with a larger filling quantity it may be slight or only a certain movement.
  • the circulation of the steam or steam-air mixture is interrupted.
  • the digestion material remains at the maximum temperature for a short time - for example about 10 seconds to about six minutes.
  • the upper piston 4 is lowered, the digestion material is pressed off by exerting the highest possible pressure.
  • the original liquor that flows off flows through the correspondingly switched lines 41 and 57. The more this pressing takes place, the lower the water consumption in the subsequent washing processes.
  • the pressing takes place approximately on hydromodule 1, if possible lower than 1, based on the cellulose produced. Since approximately 50% yield is achieved, half of the wood is dissolved, half of the original impregnation liquid is pressed off and the press in this example is therefore a quarter full.
  • the shear forces applied at the digestion temperature support the rapid separation of the individual fibers.
  • the upper piston can be shown in the te position are raised.
  • Any amount of washing or bleaching liquid can now be introduced into the press jacket via the valve 42 and or the valve 40, so that, for example, liquid is above the compact digestion mass and displacement washing can be carried out.
  • the liquid is pressed through the digestion material by the action of, for example, the upper piston 4, the primary liquor being replaced by the fresh liquid.
  • the so-called dilution wash can also be carried out by z. B.
  • the piston 4 is lowered from its drawn position until it covers the sieves 38, the valve 42 is opened and air is introduced intermittently through the line 34 via the valves 32, 33, which after the penetration of the digestion mass and the liquid and thus their mixture can escape through line 57. It can then be pressed repeatedly.
  • the piston 4 In order to dispense the extruded digestion mass, the piston 4 is lowered to the digestion mass with the valve 40 and / or the valve 42 open, without exerting any particular pressure.
  • the press jacket is then brought into its uppermost position with the aid of the working cylinders and the digestion mass is discharged laterally through the space between the lower piston 4 '(its screen plate 46) and the lower edge of the press jacket 1.
  • the upper piston 4 can also be provided with an axial tube corresponding to the tube 31 in the lower piston 4 ', which, via a valve in the valve 62, merges directly into the circulation line 53.
  • the passages 52 together with sieves 38 and ring line 51 are then omitted.
  • the lower piston 4 ' can also be vertically movable, the press jacket 1 being held stationary. The operation of the press takes place as described above, i. H. the upper piston makes the working movement, the lower piston remains at rest. To discharge the digestion mass, both pistons, holding the digestion mass between them, are moved downwards until the upper piston with its perforated plate is flush with the lower edge of the press casing 1.
  • the blower 55 can be reversible in its direction of action, i.e. after switching, it is able to blow air from outside through the valve 62 and the ring line 51 through the sieves 38 or through the axial tube of the modified embodiment and thus through the bores 47 in order to clean them.
  • the inside diameter of the press casing 1 can be somewhat enlarged in the case of a continuous transition in order to allow the ring seal 5b to slide more easily over the sieve region.
  • a cyclone 39 or the like can be provided in the direction of circulation in order to remove any entrained material from the steam or steam-air mixture flowing in the circulation pipe 53.
  • a heat exchanger for reheating the circulating steam or the steam-air mixture can also be arranged in the circulation pipe 53 (not shown).
  • the device can be filled in other ways, e.g. through a corresponding tube in the upper piston or in the press jacket, for example by gravity or pneumatically, or in another way.
  • a particular advantage of the press according to the invention is that all common types of wood chips or cellulose-containing materials can be processed.
  • wood chips typical in discontinuous sulfate pulp plants, average values are around 16-18 mm in length, 10-17 mm in width and about 3 mm in thickness.
  • mean values of 38 mm in length and width and 6 mm in thickness are more common, although the distribution around these values can be very wide in both cases.
  • a homogeneous wood chip material offers advantages in terms of uniform impregnation and heating and thus a higher-quality pulp with a lower proportion of chips and undigested.
  • turbulent heating of the digestion mass with steam or a steam-air mixture it is easier to achieve through a narrow spectrum that the flow rate is not greater than the speed of the small particles and less than the loosening rate of the largest particles.
  • the shape of the bores 47 in the sieve plates 46 is arbitrary, but is generally round.
  • the hole size must meet two conditions. Firstly, optimal squeezing of liquids, secondly, optimal introduction of gases for whirling or heating must be ensured. Both are preferably carried out through the same holes, but can in principle also be separated. The gaseous heating medium could be blown in through several larger, separately closable openings.
  • the hole diameter will be in the range of 0.2 to 10 mm, preferably 0.5 to 6 mm, and in particular 1 to 3 mm. This can also be achieved through larger holes that are covered with a sieve of the appropriate hole size.
  • the hole spacing (the division) is preferably selected such that free surfaces of 1 to 90%, preferably 3 to 80%, more preferably 10 to 70% and particularly 20 to 50% are achieved with the hole sizes indicated. For example, for a 2 mm hole size (round), a pitch of 4 mm could be used, which results in a free surface of about 23%.
  • the sieve plates 46 can both be self-supporting with a thickness corresponding to the pressure occurring in the press, but they can also consist of perforated plates which rest on webs on a thicker, load-bearing plate provided with larger bores.
  • the holes which have the above-described diameter on the inside of the press of the pistons can increase in cross section in the piston towards the outside of the press in order to achieve an easier drainage of liquids and to avoid possible blockages.
  • All or some of the bores can be inclined with respect to the press axis in order to achieve additional movement and mixing of the digestion material.
  • one or more, optionally also separately switchable, openings of larger diameter than the normal bores in the end face of the pistons, possibly arranged eccentrically, may be present in order to improve the mixing when gaseous media are introduced.
  • the type of steam or steam / air mixture supply can offer possibilities for a different inflow speed for different sections of the sieve plate 46 of the lower piston.
  • the Moeller-Scherström method the Polysius or the Fuller-Peters quadrant method are known.
  • the inflow floor the sieve plate
  • the quadrants the inflow floor
  • the sieve plate is divided into four equally large circular sectors (quadrants), with one quadrant alternately being ventilated more strongly than the other. This requires four connections and a corresponding control.
  • a high throughput of a gaseous medium through parts of the piston cross section e.g. individual quadrants
  • the speeds of the gaseous medium will depend on the digestion material, its size and moisture (hydromodule), the layer thickness, the temperature and the desired speed of the temperature increase and generally range from 0.5 to 20 m / s, preferably from 1 to 15 m / s, in particular from 3 to 10 m / s. With intermittent or pulsating operation, these speeds can also be exceeded for a short time.

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Paper (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Claims (8)

1. Procédé pour la production de cellulose à partir de matières de base cellulosiques par ouverture des cellules à température et sous pression augmentées, caractérisé en ce que par pressage des matières de base imprégnées, une proportion de masse entre le liquide d'attaque et les matières de base sèches de 0,5 à 2 est atteinte et en ce que l'ouverture des cellules est effectuée dans un dispositif de pressage à 160 jusque 300°C en une durée de moins de 10 min; le réchauffement se produisant par introduction directe de chaleur.
2. Procédé suivant la revendication 1, caractérisé en ce que le réchauffement direct se produit sous forme de chauffage électrique à résistance (chauffage ohmique).
3. Procédé suivant la revendication 1, caractérisé en ce que l'amenée de chaleur directe dans les matières de base imprégnées se fait par introduction de vapeur à l'intérieur du dispositif de pressage.
4. Procédé suivant l'une des revendications précédentes, caractérisé en ce que l'imprégnation s'effectue dans le même dispositif de pressage avec un liquide d'imprégnation d'une concentration chimique nécessaire à l'ouverture des cellules, sous pression constante ou sous forme d'à- coups de pression supérieurs à 1 bar pour la réduction de la longueur capillaire non mouillée de la matière de base.
5. Dispositif de pressage pour la réalisation du procédé suivant au moins l'une des revendications 1, 2 et 4, se composant d'une cage de presse (1, 1a, 1b) dans laquelle sont disposés deux pistons opposés l'un par rapport à l'autre, perméables au liquide (4, 4', 4a, 4b) caractérisé en ce que, en cas de chauffage électrique à résistance, la paroi intérieure de la cage de presse (1, 1a, 1 b) est entièrement ou partiellement recouverte d'un isolation électrique (2, 2a, 2b), des contacts étant installés pour l'alimentation de l'énergie électrique sur le piston supérieur et inférieur (4; 4'), ces contacts pouvant être reliés à une source d'électricité et qu'éventuellement l'un des pistons est stationnaire.
6. Dispositif de pressage suivant la revendication 5, caractérisé en ce que la cage de presse (1 b) peut être levée ou baissée à l'aide de dispositifs auxiliaires, préférentiellement des cylindres (15) à commande hydraulique ou pneumatique, ou par une commande par arbre, une isolation électrique étant installée entre la cage de presse (1b) et lesdits dispositifs auxiliaires.
7. Dispositif de pressage pour réaliser le procédé suivant l'une des revendications 1, 3 et 4 se composant d'une cage de presse (1, 1a; 1b) dans laquelle sont disposés deux pistons opposés l'un par rapport à l'autre, éventuellement perméables au liquide (4; 4'; 4a; 4b) caractérisé en ce que la cage de presse (1) au cas d'un chauffage direct par introduction de vapeur, comporte des passages latéraux (52) fermés par des tamis (38), une conduite de recirculation (53) comportant un ventilateur (55) étant prévue, une extrémité de ladite conduite étant raccordée au tube (31) dans l'un des pistons (4') et l'autre extrémité, soit aux passages (52), soit au tube de l'autre piston resp. extrémité, alors que préférentiellement elle est munie d'une vanne (32, 62) à chaque extrémité et en ce que, éventuellement, l'un des pistons est stationnaire.
8. Dispositif de pressage suivant les revendications 5 ou 7, caractérisé en ce que la cage de presse (1) comporte éventuellement des perforations (6) perméables aux liquides pour l'introduction et l'évacuation des fluides de traitement.
EP81890189A 1980-11-20 1981-11-16 Procédé et appareil pour la production de cellulose Expired EP0054015B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
AT5680/80 1980-11-20
AT0568080A AT372425B (de) 1980-11-20 1980-11-20 Verfahren und vorrichtung zur gewinnung von zellstoff
AT456481A AT375561B (de) 1981-10-27 1981-10-27 Filterpresse
AT4564/81 1981-10-27

Publications (2)

Publication Number Publication Date
EP0054015A1 EP0054015A1 (fr) 1982-06-16
EP0054015B1 true EP0054015B1 (fr) 1985-01-16

Family

ID=25601301

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81890189A Expired EP0054015B1 (fr) 1980-11-20 1981-11-16 Procédé et appareil pour la production de cellulose

Country Status (7)

Country Link
US (2) US4451331A (fr)
EP (1) EP0054015B1 (fr)
BR (1) BR8107534A (fr)
CA (1) CA1180927A (fr)
DE (1) DE3168397D1 (fr)
FI (1) FI69490C (fr)
NO (1) NO156950C (fr)

Families Citing this family (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0097188A1 (fr) * 1981-12-10 1984-01-04 Battelle Memorial Institute Procede de delignification du bois et autres produits lignocellulosiques
FI67891C (fi) * 1983-02-17 1985-06-10 Larox Ag Foerfarande foer behandling av den fraon en cellulosas kokningsprocess erhaollna cellulosan
WO1984003527A1 (fr) * 1983-03-02 1984-09-13 Nivelleau Bruniere Patrick M F Procede de traitement de matieres ligno-cellulosique pour l'obtention de cellulose.
AT391104B (de) * 1985-04-01 1990-08-27 Sgp Va Energie Umwelt Dichtsystem fuer ein hochdruckgefaess
AT385061B (de) * 1985-11-29 1988-02-10 Neusiedler Ag Verfahren zur gewinnung von zellstoff aus pflanzenfasermaterial
AT384954B (de) * 1986-09-11 1988-02-10 Simmering Graz Pauker Ag Hochdruckgefaess mit stampfeinrichtung
US4826566A (en) * 1988-01-11 1989-05-02 Le Tourneau College Rapid disolution of lignin and other non-carbohydrates from ligno-cellulosic materials impregnated with a reaction product of triethyleneglycol and an organic acid
US5238538A (en) * 1991-11-25 1993-08-24 Georgia Tech Research Corporation Method for deinking recycled fiber by applying direct current electric field
CA2082557C (fr) * 1992-02-24 1997-03-11 Charles W. Hankins Procede de desintegration integre de dechets de papier produisant des fibres de papier de categorie hygienique
EP0629717B1 (fr) * 1993-06-09 1998-01-28 ALD Vacuum Technologies GmbH Appareil et procédé pour le nettoyage, en particulier le dégraissage, d'objets conducteurs électriques
DE4319166C2 (de) * 1993-06-09 2002-02-14 Ald Vacuum Techn Ag Verfahren und Vorrichtung zur Reinigung, insbesondere Entfettung und Kompaktierung von elektrisch leitfähigem Gut
SE502440C2 (sv) * 1994-02-04 1995-10-16 Kvaerner Pulping Tech Apparat för behandling av massa av cellulosahaltigt fibermaterial med en behandlingsvätska
GB9726218D0 (en) * 1997-12-12 1998-02-11 British American Tobacco Co Separation and determination of cellulosic components fron plant material
EP1056902A4 (fr) * 1998-02-19 2001-05-30 Int Paper Co Procede de production de pate chimique a partir de plantes herbacees
US20040104003A1 (en) * 2000-11-28 2004-06-03 Biopulping International, Inc. Eucalyptus biokraft pulping process
US7008505B2 (en) * 2001-06-01 2006-03-07 Biopulping International, Inc. Eucalyptus biomechanical pulping process
CA2466505A1 (fr) * 2001-11-09 2003-05-15 Biopulping International, Inc. Pre-traitement aux micro-ondes de rondins utilises dans la fabrication du papier et d'autres produits en bois
US20040040677A1 (en) * 2002-09-04 2004-03-04 Kojess Deveolpment Ltd. Organic biomass paper pulping
ITRM20020504A1 (it) * 2002-10-04 2004-04-05 Gioia Antonio La Compattatore essiccatore a gabbia a doppio flusso e
DE202007007038U1 (de) * 2007-05-14 2007-10-25 Pallmann Maschinenfabrik Gmbh & Co Kg Vorrichtung zum Entwässern von schütt- oder fließfähigem Aufgabegut durch Verdichtung
US20090019771A1 (en) * 2007-07-21 2009-01-22 Pearson Larry E Apparatus to convey material to a pressurized vessel and method for the same
FR2925533B1 (fr) * 2007-12-20 2010-01-08 Inst Francais Du Petrole Procede de conversion de solutions lignocellulosiques a haute teneur en matiere seche
DE102013114386A1 (de) * 2013-12-18 2015-06-18 Uwe D'Agnone Verfahren zur Aufbereitung von Gras für die Herstellung von Papier, Pappen und Karton
CN109196164B (zh) * 2016-05-27 2022-02-15 菲布拉技术私人有限公司 用于生产高分子量木质素的方法和系统
CN114622433B (zh) * 2022-03-09 2022-09-30 江西华昊新能源有限公司 一种锂离子电池电极材料纸浆设备及其工艺

Family Cites Families (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE415061C (de) * 1922-05-11 1925-06-19 Koholyt Akt Ges Verfahren zur Kochung von Holz zur Darstellung von Zellstoff unter Verwendung der ueblichen Kochlaugen
US1905731A (en) * 1929-05-04 1933-04-25 Ralph H Mckee Process of digesting pulp and apparatus therefor
US1991245A (en) * 1931-12-17 1935-02-12 Roza Corp De Process for producing cellulose
US1991243A (en) * 1931-12-17 1935-02-12 Roza Corp De Apparatus for producing cellulose
US1991248A (en) * 1934-03-15 1935-02-12 Goneral Electric Company Furnace control apparatus
US2159258A (en) * 1934-05-28 1939-05-23 Joaquin Julio De La Roza Sr Method and apparatus for digesting fibrous or cellular material
US2072086A (en) * 1934-12-03 1937-03-02 Roza Corp De Digesting method and apparatus
US2067480A (en) * 1935-07-18 1937-01-12 Roza Corp De Process of manufacture of pulp
US2221806A (en) * 1938-01-20 1940-11-19 Evarts G Loomis Dehydrating press and method of dehydrating
DE739004C (de) * 1938-06-29 1943-09-08 Karl Miedler Dipl Ing Verfahren zur Vorbehandlung von chemisch abzubauendem Holz durch Pressung
FR989191A (fr) * 1944-09-07 1951-09-05 Traitement Chimique Des Vegeta Procédé de traitement des matières fibreuses, plus particulièrement des végétaux en vue de l'obtention de la cellulose
FR997965A (fr) * 1945-09-15 1952-01-14 Du Pin Cellulose Procédé et dispositif pour le défibrage des matières cellulosiques ou analogues
US2771361A (en) * 1951-12-07 1956-11-20 Process Evaluation Devel Defibration processes
DE1047000B (de) * 1953-09-30 1958-12-18 Aschaffenburger Zellstoffwerke Verfahren zur Herstellung von Halbzellstoff
US2874044A (en) * 1955-12-23 1959-02-17 Wenzl Hermann Franz Joseph Multistage process relating to the alkaline digestion of raw cellulosic materials for the production of pulp with a high content of alpha cellulose
DE1072078B (de) * 1956-01-26 1959-12-24 Improved Machinery Inc., Nashua, N. H. (V. St. A.) Kontinuierlich arbeitender stehender Zellstoffkocher
DE1132423B (de) * 1957-03-07 1962-06-28 Bauer Bros Co Verfahren zur Herstellung eines holzschliffartigen Holzfaserstoffes
US3066359A (en) * 1957-11-05 1962-12-04 Chicopee Mfg Corp Methods and apparatus for producing fibrous webs
DE1288900B (de) * 1960-05-09 1969-02-06 Improved Machinery Inc Behaelter zum Behandeln zerkleinerter cellulosehaltiger Feststoffe
US3215588A (en) * 1963-08-15 1965-11-02 Lummus Co Continuous impregnation, cooking, and washing of fibrous material
US3911807A (en) * 1973-12-10 1975-10-14 Bruce H Birnbaum Refuse compactor and method
JPS5815235B2 (ja) * 1974-06-13 1983-03-24 フコクコウギヨウ カブシキガイシヤ レンゾクアツサクキ
AT336992B (de) * 1975-02-18 1977-06-10 Visch Khim T I Nis Verfahren und vorrichtung zum herstellen von fasermaterial aus pflanzenrohstoffen
US4346653A (en) * 1980-02-22 1982-08-31 General Defense Corporation Method and apparatus for refuse disposal

Also Published As

Publication number Publication date
FI813684L (fi) 1982-05-21
NO813923L (no) 1982-05-21
BR8107534A (pt) 1982-08-17
DE3168397D1 (en) 1985-02-28
EP0054015A1 (fr) 1982-06-16
US4451331A (en) 1984-05-29
US4556452A (en) 1985-12-03
FI69490C (fi) 1986-02-10
NO156950C (no) 1987-12-23
FI69490B (fi) 1985-10-31
NO156950B (no) 1987-09-14
CA1180927A (fr) 1985-01-15

Similar Documents

Publication Publication Date Title
EP0054015B1 (fr) Procédé et appareil pour la production de cellulose
DE2458929C3 (de) Verfahren zum Herstellen von Faserplatten
DE3938504C2 (de) Verfahren zum kontinuierlichen Aufschließen von Zellulosefasermaterial
DE2112633B2 (de) Verfahren zum aufschliessen von zellulose und vorrichtung zur durchfuehrung des verfahrens
DE2053419A1 (de) Verfahren und Vorrichtung zum Mahlen von Papierstoff
DE2641143A1 (de) Verfahren und vorrichtung zum gewinnen von oelen aus oelhaltigen rohstoffen
DE1926516A1 (de) Verfahren und Vorrichtung zum Waschen von Cellulose
DE68905524T2 (de) Erhoehung der qualitaet bei kontinuierlichem zellstoffkochen.
DE1079442B (de) Verfahren und Vorrichtung zur kontinuierlichen Gewinnung von Halbzellstoff aus lignocellulose-haltigen Rohstoffen
DE69210692T2 (de) Diskontinuierliches Verfahren zur Herstellung von Kraft-Zellstoffen
DE102004010196A1 (de) Verfahren und Vorrichtung zum Austragen von lignozellulosem Rohmaterial aus einem Kocher und zur Förderung des Rohmaterials zu einem Refiner
DE69816478T2 (de) Verfahren zur herstellung von zellstoff
AT504589B1 (de) Verfahren und vorrichtung zur entfernung von gas aus holzschnitzeln
DE69010128T2 (de) Verfahren und Vorrichtung zum Leeren vom Zellstoffkocher.
AT375561B (de) Filterpresse
DE2528393C3 (de) Verfahren zur Behandlung von ZeIlstoffaserbrei und Vorrichtung zur Durchführung des Verfahrens
DE1267076B (de) Verfahren zum kontinuierlichen Kochen von Zellulosematerial
DE1517163A1 (de) Verfahren zum Aufschliessen von Zellulose
DE653505C (de) Verfahren und Vorrichtung zum Aufloesen von Altpapier und Papierausschuss
DE1461013A1 (de) Verfahren zum Kuehlen von Faserstoffaufschwemmungen beim Mahlen und Feinstmahlen
AT339131B (de) Verfahren und vorrichtung zum aufschliessen von fasern und/oder faserbundeln
DE69128267T2 (de) Modifizierter und kontinuierlicher Sulfitaufschluss
AT136385B (de) Verfahren und Anlage zur Gewinnung von Zellstoff.
DE10119182A1 (de) Vorrichtung und Verfahren zum kontinuierlichen Kochen von zellulosehaltigem Rohmaterial
DE1767885C3 (de) Verfahren und Vorrichtung zur Behandlung von faserigem Cellulosestoff oder cellulosehaltigem Stoff

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Designated state(s): BE CH DE FR GB IT LU NL SE

17P Request for examination filed

Effective date: 19821209

ITF It: translation for a ep patent filed
GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Designated state(s): BE CH DE FR GB IT LI LU NL SE

REF Corresponds to:

Ref document number: 3168397

Country of ref document: DE

Date of ref document: 19850228

ET Fr: translation filed
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19851130

26N No opposition filed
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 19891016

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 19891018

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: LU

Payment date: 19891019

Year of fee payment: 9

Ref country code: CH

Payment date: 19891019

Year of fee payment: 9

Ref country code: BE

Payment date: 19891019

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 19891023

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 19891031

Year of fee payment: 9

ITTA It: last paid annual fee
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 19891130

Year of fee payment: 9

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Effective date: 19901116

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Effective date: 19901117

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Effective date: 19901130

Ref country code: CH

Effective date: 19901130

Ref country code: BE

Effective date: 19901130

BERE Be: lapsed

Owner name: SIMMERING-GRAZ-PAUKER A.G.

Effective date: 19901130

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Effective date: 19910601

GBPC Gb: european patent ceased through non-payment of renewal fee
NLV4 Nl: lapsed or anulled due to non-payment of the annual fee
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Effective date: 19910731

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Effective date: 19910801

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

EUG Se: european patent has lapsed

Ref document number: 81890189.4

Effective date: 19910705