EP0025550B1 - Verfahren zum Extrahieren von Wasser aus Schlichte-Waschflotten - Google Patents

Verfahren zum Extrahieren von Wasser aus Schlichte-Waschflotten Download PDF

Info

Publication number
EP0025550B1
EP0025550B1 EP80105228A EP80105228A EP0025550B1 EP 0025550 B1 EP0025550 B1 EP 0025550B1 EP 80105228 A EP80105228 A EP 80105228A EP 80105228 A EP80105228 A EP 80105228A EP 0025550 B1 EP0025550 B1 EP 0025550B1
Authority
EP
European Patent Office
Prior art keywords
liquor
desizing
fabric
size
wash
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
EP80105228A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0025550A1 (de
Inventor
Wilhelm Dr. Ruettiger
Franz Suetsch
Albrecht Dr. Wuerz
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.)
BASF SE
Original Assignee
BASF SE
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
Application filed by BASF SE filed Critical BASF SE
Priority to AT80105228T priority Critical patent/ATE2278T1/de
Publication of EP0025550A1 publication Critical patent/EP0025550A1/de
Application granted granted Critical
Publication of EP0025550B1 publication Critical patent/EP0025550B1/de
Expired legal-status Critical Current

Links

Images

Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
    • D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
    • D06L1/12—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using aqueous solvents
    • D06L1/14—De-sizing

Definitions

  • DE-B-2 543 815 like US-A-4106 900, describes a desizing process based on the countercurrent principle using as little water as possible in order to minimize the effort for concentrating the desizing liquor. Nevertheless, the concentration of the desizing fleet is still below the concentration of sizing agent required for sizing.
  • the invention was therefore based on the object of developing a more economical process for strengthening wash wash liquors, which is to be carried out, if possible, on standard textile finishing machines, that is to say without evaporation systems and without ultrafiltration systems.
  • Suitable wash liquors for the process according to the invention are all wash liquors of water-soluble sizes, insofar as they are suitable for reprocessing, ie. H. are essentially free of non-volatile foreign substances.
  • Foreign substances are primarily desizing agents (enzymes, surfactants, alkali), but also substances detached from the textile material such as fiber preparation agents, lubricants, lubricating oils (from the loom) and natural fiber contaminants such as pectins, waxes and the like. a., furthermore degradation products created during singeing, or "dirt" for short. Small amounts of such foreign substances in these wash liquors, which do not interfere with reuse, do not impair the process according to the invention.
  • Usual water-soluble sizing agents are synthetic or (mostly modified) natural high polymers, such as glue-like proteins, acrylate-based polymers, carboxymethyl cellulose, alginates, polyvinyl alcohol and water-soluble starch products. Sizes that are not or only poorly biodegradable are primarily suitable for repeated reuse, that is to say primarily acrylate-based polymers, and also carboxymethyl cellulose and polyvinyl alcohol.
  • the dry fabric must be loaded with essentially the same size as the size wash liquor from which water is to be removed. To a certain extent, it is also possible to work with mixed sizes using the process according to the invention, in particular if the mixture components are similar in terms of the properties mentioned below.
  • Sizing agents that have the lowest possible viscosity and that also have a high swelling rate and a low sorption hysteresis are particularly favorable for the process according to the invention. These demands are e.g. B. well fulfilled by acrylic-based sizing agents. They are therefore preferred.
  • Washing units from are particularly suitable for countercurrent flow with intimate contact Roller skid type, with vertical goods routing and partitioning being particularly advantageous. It is not necessary for the washing unit to be fully flooded.
  • the amount of liquor carried in the air passage after immersing the goods once is sufficient.
  • the lower rolls should be immersed at least 2/3 into the wash liquor.
  • the goods are preferably carried out in the broad state in the process according to the invention. Basically, similarly good results can also be obtained when treating the textile material in strand form, in particular if the strand is opened in between and is widely guided in order to squeeze it out.
  • the textile goods should be in contact with a fleet amount of at least 70, preferably at least 110 percent by weight, based on dry raw fabric, after wetting. There is no strict limit for the amount of liquor with which the textile material is in contact after wetting for the process according to the invention.
  • the fleet volume should be as small as possible, preferably less than 20 I / m 2 goods content.
  • the liquor loading is expediently selected in the range from 70 to 250%.
  • the upper limit is due to the fact that the goods do not drag too much fleet from sector to sector against the concentration gradient. Depending on the item, this value is in the range of 180 to 250%.
  • the contact times for water extraction depend mainly on the swelling time of the textile goods and their loading as well as on the intended water extraction performance. In general, 40 seconds of contact between the raw fabric and the liquor is sufficient for slightly swelling and solvating sizing agents such as acrylate sizing. Since the size wash liquor, particularly with a high concentration, also has a higher viscosity and adheres to the textile material, the water extraction can be increased to a certain extent with an additional air passage between the deflection rollers with shorter contact times. Even with 10 seconds of liquor contact time and approx. 50 seconds of air passage, very good water extraction values are still obtained.
  • the maximum goods running speed then results from the goods content of the treatment units and the required minimum contact time.
  • the countercurrent or feed (1 in Fig. 1) of wash wash liquor is adjusted so that 0.2 to 5, preferably 0.3 to 2.5 l of liquor flow against each kg of textile material.
  • the amount of water withdrawn from the textile and / or its loading of the liquor is expediently set at 0.1 to 2, preferably 0.3 to 1.3, of 1 water per kg of textile.
  • This deprivation of water can be determined with the known continuous high-humidity measuring devices (centimeter wave absorption) or by cutting out samples and weighing. Serve as control variables for water withdrawal.
  • B. the contact time, the temperature and the known intensifying devices of Wasqh and impregnation units (e.g. support rollers, planetary rollers, squeeze rollers, impact rollers, spray nozzles, crushing rollers, bulkheads, meandering) and in particular the weight ratio of the fleet used to the one loaded with size Raw fabric.
  • this weight ratio for the wash wash liquor feed so that the resulting quantity of strengthened liquor for reuse does not exceed a limit quantity which is of the order of 0.5 I / kg.
  • the exact value of this liquor limit is the amount of reuse liquor in per kg of raw fabric, with which there is no excess liquor when the size liquor is prepared for the warp yarns.
  • the liquor limit is higher, the greater the weight proportion of the chain in the fabric, the higher the size liquor application to the chain, the less fresh sizing agent is required to replenish the target concentration of the liquor (to compensate for the otherwise increasing accumulation of impurities - provided that these are not separated - as well as loss of sizing agent due to incomplete washing out during desizing) and the lower the amount of condensate in the liquor can be kept when heating up with steam.
  • the amount of water in the wash wash liquor is sufficient (even with a high wash wash concentration) to extinguish and swell the fabric and the wash on it.
  • the textile material is freed as much as possible of adhesive wash liquor.
  • the known units such as squeezing mechanism (preferred), suction drum, suction slot are suitable for this.
  • the size wash liquor (3) separated in this way is fed to the countercurrent, preferably at that point (C) of the countercurrent arrangement at which the wash liquor has approximately the same concentration (measurement, for example, via refractive index, viscosity or conductivity) as the separated liquor . It is therefore expedient not to consistently adhere to the countercurrent principle, as is customary in countercurrent washing, ie.
  • the much more concentrated liquor separated from the textile material is not mixed with the fed wash wash liquor (1), but skips a part (D) of the countercurrent and is fed in according to the specified criteria.
  • the number of segments in the water extraction compartment can then be reduced to 2 to 3.
  • the regrind fleet for reuse is expediently taken from the point of the system at which the highest size concentration is established in the fleet. In the case of predominantly countercurrent operation, this is the contact area for the textile goods fleet (segment A, line 2 in Fig. 1) and the first fleet separation point for extinguishing technology with a regenerated fleet, for loads in the range of around 90 to 140%.
  • the final loading of the textile goods with sizing agent is set, which is of the same order of magnitude as the loading of the textile goods running dry in the countercurrent. Even if the loading of the emerging textile material with sizing agent should be slightly higher than that of the incoming one with this water extraction, which is equivalent to a negative washing effect, neither the water removal nor the success in terms of enrichment for reusing the sizing is questioned.
  • the method according to the invention can be carried out in a treatment station on its own, especially if space constraints dictate this. Normally, however, it will be used in conjunction with treatment processes in the textile industry, i.e. H. in the local area from pre-treatment in finishing to sizing in the weaving mill.
  • the water extraction station will expediently have its location in the pretreatment, preferably in combination with size washout systems. Using a suitable transport system (pipeline, container), the strengthened wash wash liquor is then fed from there to the sizing shop for reuse. It is advisable to couple the water extraction directly to the desizing in the continuous run ( Figure 2). If more water than physically and chemically required is used (cf. W.
  • the enrichment washout should be understood here to mean the known washout washout processes in which the washed out wash is used again. These are processes in which essentially no additives are added, with as little as possible, at least less than 5 fresh water / kg of textile material and a total washing efficiency (for definition and measurement method see textil praxis international, 1974, issue 1, pages 90 to 93) from 60 to 95 , mostly by 70 to 80%. In combination with the water extraction according to the invention, these processes give favorable results if the wash wash liquor obtained after the enrichment wash wash is below 1.6, preferably below 1.4 1 / kg of textile material to be desized.
  • the washing effect in the enrichment wash can then be increased to washing efficiencies of 70 to 90%.
  • the combination of enrichment washout and water extraction according to the invention shows optimum results if, during the enrichment washout according to the countercurrent principle, the wash liquor separated from the textile goods at the outlet of the textile goods (and - preferably at the same concentration as possible - fed into the counterflow of the last washing compartment) has a concentration of size in the range of 5 to 50 g / l. If this concentration is lower, this means washing out so thoroughly that the washing out of impurities in the textile goods can hardly be avoided. These then accumulate in the wash wash liquor and lead to faults. With a higher concentration of the sized wash wash liquor of size, too much size remains on the textile, i. H. not enough sizing agent is recovered and also the subsequent finishing stage, e.g. B.
  • the concentration range proposed here can be monitored using known methods. Refractive index or viscosity of the liquor can lead to greater effort at the lower values.
  • the conductivity method proved to be particularly simple and safe, although it only led to good results with the sizes based on ionogenic polymers.
  • the method according to the invention not only saves a considerable amount of energy, but also the purchase of an evaporation system, because the method according to the invention can in principle be carried out with treatment units which can also be used for other washing processes in the textile finishing business. Compared to the conventional concentration using ultrafiltration, the purchase and operation of complex, intrinsically external equipment is saved.
  • the size loading was determined using various methods:
  • the gravimetric method 2c did not take into account the shrinkage of the goods and losses of impurities in the fiber material.
  • the fabric also shows quite often differences in the area weight (with size) in the range of ⁇ 5% (sample size approx. 2 x 2 cm).
  • the most likely value for the size loading was set at 5.0% or 50 g / kg.
  • the goods were cut into 4 strips of equal width (45 cm) and docked for the experiments without gluing the edges.
  • the described raw material was run until the specified target concentration of 70 g / l acrylate (9.5 ° Brix) was reached in the water extraction compartment.
  • the process data was recorded and some variants of the driving style were checked.
  • the size wash liquor from the enrichment washing compartments was completely fed to the water extraction compartment (with the segments A-D in Figure 1). No liquor was withdrawn from the water extraction compartment, so that neither wastewater was obtained nor the recovery liquor was withdrawn.
  • a total of 220 m of goods corresponding to 13.2 kg of textile goods were required for the start-up operation.
  • a total of 10.1 liters of pre-sharpened wash liquor was fed into 12 batches of approx. 850 ml at the enrichment rewashing compartment II. This results in an average wash water consumption of 0.76 I / kg of raw fabric.
  • the setpoint of the level controller was set so that the lower deflection rollers were just covered with washing liquor.
  • tissue sections were removed after the final squeeze in order to analyze the size remaining.
  • the tissue samples were shaken out cold in a 1:12 liquor ratio, the following values for the weight loss being obtained:
  • the size obtained in this way was used again tel quel in the laboratory single-thread size test and did not result in any deteriorated values compared to the original size.
  • the washing efficiency chosen here for demonstration purposes is particularly high compared to the prior art, because of the dirt accumulation to be expected.
  • the size concentration in the fleet was continuously monitored (samples) by means of refractive index and conductivity measurements in both the 4 countercurrent segments (A to D in Fig. 1) and in the return (3) of the crushing unit (Q).
  • refractive index about 9 ° Brix in the three front segments of the water extraction compartment (A, B, C in the picture), i.e. H. determine an acrylate concentration of almost 70 g / l.
  • FIG 1 shows schematically the water extraction compartment consisting of 4 segments A to D with subsequent crushing unit Q and the liquor streams 1 to 3.
  • the upper deflection rollers are not shown, neither are compartments I and II for the enrichment wash.
  • the time course of the concentrations of acrylate for each segment of the water extraction compartment is shown in Figure 1.
  • the zero line indicates the submitted acrylate concentration at the start of the fabric career.
  • the remaining single-digit numbers show the concentration level in hours after the respective term. Two different digits at one level mean that the same concentration was measured at both times shown.
  • the extraction compartment shown was connected to a commercially available desizing plant of basically the same construction, here consisting of compartments I and II, the first of which is similar to the water extraction compartment shown (the second will be described later).
  • the inlet (1 in Figure 1) of this system was at the end (in the direction of flow; or at the beginning in the direction of the flow of goods) of the counterflow, i.e. at the point with the highest size concentration, taken.
  • the liquor discharge (2) consisted of the enriched wash wash liquor ready for use.
  • the squeeze liquor (3) was guided by the squeeze roller (Q) by skipping the compartment (D) or the compartments with thinner liquors into the segment with the most concentration (in Figure 1, for example, segment C).
  • the size wash liquor 1 was fed into segment D in accordance with the countercurrent principle. During stationary operation, it had a concentration of 30 g / l, which was strengthened by a factor of 2-3 through the removal of water.
  • the goods had a loading of approx. 15 g / kg (sample) of acrylate with an inlet loading of 50 g / kg into the prewashing compartment (compartment I), resulting in a washing efficiency of 70%.
  • the countercurrent fleet fed in this way had an acrylate concentration of 6-9 g / 1 in stationary operation and a volume output of 1.31 / kg.
  • Cold wash liquor was generally used for the enrichment wash (approx. 18 ° C).
  • a unit was available as a post-wash compartment, which, with a minimum bath volume of approx. 50 liters and without bulkheads, offered no possibility of building up an effective concentration gradient.
  • concentration was relatively constant at 8.5 g acrylate / l (1.1 ° Brix).
  • the fresh water consumption during stationary operation was 3.5 l / h ⁇ 60 ml / min ⁇ 1 l / kg textile material (average over 2 hours and 120 m raw fabric).
  • the size loading of the leaking textile goods during stationary operation was 4-5 g / kg according to the weight loss method and 2-3 g / kg according to the conductivity method. Thus, during the 2 to 3 hours of stationary operation, the washing efficiency of the enrichment wash was already over 90%.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Glass Compositions (AREA)
  • Iron Core Of Rotating Electric Machines (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • External Artificial Organs (AREA)
  • Detergent Compositions (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Woven Fabrics (AREA)
EP80105228A 1979-09-13 1980-09-03 Verfahren zum Extrahieren von Wasser aus Schlichte-Waschflotten Expired EP0025550B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT80105228T ATE2278T1 (de) 1979-09-13 1980-09-03 Verfahren zum extrahieren von wasser aus schlichte-waschflotten.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2937002A DE2937002C2 (de) 1979-09-13 1979-09-13 Verfahren zum Entschlichten von bahnförmigem Gewebe
DE2937002 1979-09-13

Publications (2)

Publication Number Publication Date
EP0025550A1 EP0025550A1 (de) 1981-03-25
EP0025550B1 true EP0025550B1 (de) 1983-01-19

Family

ID=6080760

Family Applications (1)

Application Number Title Priority Date Filing Date
EP80105228A Expired EP0025550B1 (de) 1979-09-13 1980-09-03 Verfahren zum Extrahieren von Wasser aus Schlichte-Waschflotten

Country Status (10)

Country Link
US (1) US4333190A (enrdf_load_stackoverflow)
EP (1) EP0025550B1 (enrdf_load_stackoverflow)
JP (1) JPS56107060A (enrdf_load_stackoverflow)
AT (1) ATE2278T1 (enrdf_load_stackoverflow)
AU (1) AU531928B2 (enrdf_load_stackoverflow)
CA (1) CA1150912A (enrdf_load_stackoverflow)
DE (2) DE2937002C2 (enrdf_load_stackoverflow)
ES (1) ES8105805A1 (enrdf_load_stackoverflow)
FI (1) FI78511C (enrdf_load_stackoverflow)
PT (1) PT71797B (enrdf_load_stackoverflow)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4303920C2 (de) * 1993-02-10 1998-04-30 Hoechst Ag Verfahren zum Entschlichten von mit wasserlöslicher Schlichte beladenem Textilgut
US6036864A (en) * 1996-12-31 2000-03-14 Demyanovich; Robert J. Process for reducing water consumption during wet processing of textiles
RU2135662C1 (ru) * 1997-04-21 1999-08-27 АООТ "Зиновьевская мануфактура" Способ обработки ткани и устройство для его осуществления
US5980582A (en) * 1997-11-14 1999-11-09 Kleinewefers Textilmaschinen Gmbh Method and apparatus for continuously treating a web of fabric
GB0116122D0 (en) * 2001-07-02 2001-08-22 Milner Alan J Production of solutions of biosolid useful for agricultural recycling from textile efflucent
US9359721B2 (en) * 2013-03-13 2016-06-07 WestPoint Home LLC Soft feel printed fabric and method of producing same
CN119287606B (zh) * 2024-11-19 2025-07-29 浙江威尔实业有限公司 一种高效水循环的织物退浆设备

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2543815C3 (de) * 1975-10-01 1980-08-21 Basf Ag, 6700 Ludwigshafen Verfahren zum Entschlichten von Geweben
US4106900A (en) * 1977-01-18 1978-08-15 Auburn University Research Foundation Process for recycling textile warp yarn size
DE2808920A1 (de) * 1978-03-02 1979-09-13 Hoechst Ag Verfahren und vorrichtung zur extraktion von wasserloeslichen schlichtemitteln aus geschlichteten geweben

Also Published As

Publication number Publication date
AU531928B2 (en) 1983-09-08
ATE2278T1 (de) 1983-02-15
US4333190A (en) 1982-06-08
FI78511B (fi) 1989-04-28
DE3061687D1 (en) 1983-02-24
EP0025550A1 (de) 1981-03-25
AU6236080A (en) 1981-03-19
PT71797A (de) 1980-10-01
DE2937002C2 (de) 1982-04-01
FI78511C (fi) 1989-08-10
JPS633994B2 (enrdf_load_stackoverflow) 1988-01-27
ES495021A0 (es) 1981-06-16
ES8105805A1 (es) 1981-06-16
JPS56107060A (en) 1981-08-25
PT71797B (de) 1981-08-04
CA1150912A (en) 1983-08-02
DE2937002A1 (de) 1981-04-02
FI802864A7 (fi) 1981-03-14

Similar Documents

Publication Publication Date Title
DE4004111C2 (de) Verfahren zur Vorbehandlung von textilen Flächengebilden oder Garnen
DE3152654C2 (de) Verfahren zum Waschen von Textilgegenst{nden und Vorrichtung zur Durchf}hrung des Verfahrens
DE2713800A1 (de) Verfahren zur kontinuierlichen behandlung von kettgarnen
EP0025550B1 (de) Verfahren zum Extrahieren von Wasser aus Schlichte-Waschflotten
DE3539391A1 (de) Schlichtmaschine und verfahren zum betrieb einer schlichtmaschine
DE2853242A1 (de) Vorrichtung zur nassbehandlung von fasermaterial
DD155439A5 (de) Verfahren und vorrichtung zum kontinuierlichen faerben von kettgarnen
EP0361098A1 (de) Verfahren zum Continuefärben von Baumwollware und Färbeanlage zum Durchführen des Verfahrens
DE2543815C3 (de) Verfahren zum Entschlichten von Geweben
DE2903134B2 (de) Verfahren zum Waschen von gefärbtem oder bedrucktem Textilgut
EP1498534A2 (de) Verfahren und Vorrichtung zum Färben von Textilien
DE3311707A1 (de) Einrichtung und verfahren zur chemischen behandlung eines tuches
DE4237962C2 (de) Verfahren und Vorrichtung zum Schlichten von Kettfäden
EP0545202B1 (de) Flüssigkeitsabstreifer für fotografisches Material
EP0683829B1 (de) Verfahren zum entschlichten von mit schlichte beladenem textilgut
EP0038008A1 (de) Verfahren zum Reinigen von Schlichteregeneratflotten
EP0144818B1 (de) Verfahren und Anlage zum Abkochen von textilen Warenbahnen oder dergl.
DE69007267T2 (de) Bleichen von Textilien mit Sauerstoff und Wasserstoffperoxid.
EP0711859B1 (de) Maschine zum Vorbehandeln, Färben und/oder Nachbehandeln
DE2757988A1 (de) Verfahren zum kontinuierlichen waschen von bedruckten textilen flaechengebilden
DE2951695C2 (enrdf_load_stackoverflow)
DE2518939A1 (de) Verfahren zum schrumpfen und waschen von textilen flaechengebilden
DE2812666A1 (de) Verfahren und vorrichtung zum trockenreinigen
EP1371771A1 (de) Verfahren zum Entschlichten von Geweben
DE2364742A1 (de) Verfahren zum vorbehandeln von textilerzeugnissen vor dem faerben

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): AT BE CH DE FR GB IT NL SE

17P Request for examination filed

Effective date: 19810328

RBV Designated contracting states (corrected)

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

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

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

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

REF Corresponds to:

Ref document number: 2278

Country of ref document: AT

Date of ref document: 19830215

Kind code of ref document: T

REF Corresponds to:

Ref document number: 3061687

Country of ref document: DE

Date of ref document: 19830224

EN Fr: translation not filed
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 19910805

Year of fee payment: 12

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

Ref country code: FR

Payment date: 19910807

Year of fee payment: 12

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

Ref country code: SE

Payment date: 19910808

Year of fee payment: 12

Ref country code: CH

Payment date: 19910808

Year of fee payment: 12

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

Ref country code: AT

Payment date: 19910812

Year of fee payment: 12

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

Ref country code: BE

Payment date: 19910830

Year of fee payment: 12

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

Ref country code: DE

Payment date: 19910921

Year of fee payment: 12

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: 19910930

Year of fee payment: 12

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

Ref country code: GB

Effective date: 19920903

Ref country code: AT

Effective date: 19920903

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

Ref country code: SE

Effective date: 19920904

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

Ref country code: LI

Effective date: 19920930

Ref country code: CH

Effective date: 19920930

Ref country code: BE

Effective date: 19920930

BERE Be: lapsed

Owner name: BASF A.G.

Effective date: 19920930

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

Ref country code: NL

Effective date: 19930401

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 19920903

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: 19930528

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: 19930602

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

EUG Se: european patent has lapsed

Ref document number: 80105228.3

Effective date: 19930406

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