EP0101334A2 - Metallenthaltender Detergens-Dispergierzusatz von hoher Alkalität für Schmieröle - Google Patents

Metallenthaltender Detergens-Dispergierzusatz von hoher Alkalität für Schmieröle Download PDF

Info

Publication number
EP0101334A2
EP0101334A2 EP83401255A EP83401255A EP0101334A2 EP 0101334 A2 EP0101334 A2 EP 0101334A2 EP 83401255 A EP83401255 A EP 83401255A EP 83401255 A EP83401255 A EP 83401255A EP 0101334 A2 EP0101334 A2 EP 0101334A2
Authority
EP
European Patent Office
Prior art keywords
glycol
new additive
additive according
molar ratio
amine
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.)
Granted
Application number
EP83401255A
Other languages
English (en)
French (fr)
Other versions
EP0101334B1 (de
EP0101334A3 (en
Inventor
Jean-Louis Le Coent
Bernard Demoures
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.)
Orogil SA
Original Assignee
Orogil SA
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 Orogil SA filed Critical Orogil SA
Priority to AT83401255T priority Critical patent/ATE30716T1/de
Publication of EP0101334A2 publication Critical patent/EP0101334A2/de
Publication of EP0101334A3 publication Critical patent/EP0101334A3/fr
Application granted granted Critical
Publication of EP0101334B1 publication Critical patent/EP0101334B1/de
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M159/00Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
    • C10M159/12Reaction products
    • C10M159/20Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products
    • C10M159/24Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products containing sulfonic radicals
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M159/00Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
    • C10M159/12Reaction products
    • C10M159/20Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products
    • C10M159/22Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products containing phenol radicals
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/023Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/028Overbased salts thereof
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/26Overbased carboxylic acid salts
    • C10M2207/262Overbased carboxylic acid salts derived from hydroxy substituted aromatic acids, e.g. salicylates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/046Overbased sulfonic acid salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/08Thiols; Sulfides; Polysulfides; Mercaptals
    • C10M2219/082Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
    • C10M2219/087Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Derivatives thereof, e.g. sulfurised phenols
    • C10M2219/089Overbased salts

Definitions

  • the subject of the present invention is a new high alkalinity metal detergent-dispersant additive for lubricating oils.
  • the Applicant has in fact found a detergent-dispersant additive having a TBN of at least 225, containing more than 3.8% by weight of magnesium and, generally, of the order of 2 to 3 X by weight of calcium, this which gives said additive, in addition to the detergency and dispersion characteristics, a good activity as anti-wear.
  • magnesium alkylbenzenesulfonate denotes any solution containing from 25 to 80% by weight, preferably from 30 to 70%. by weight of a magnesium alkylbenzenesulfonate in a dilution oil which may or may not be the same as that used to prepare the new additive.
  • magnesium alkylbenzenesulfonates which can be used, mention may be made of the magnesium salts of sulfonic acids obtained by sulfonation of alkylbenzenes derived from olefins or from C 15 -C 30 olefin polymers.
  • the amount of dilution oil that can be used is such that the amount of oil contained in the final product (including that from the starting magnesium alkylbenzenesulfonate) represents from 20 to 60 by weight of said product, preferably from 25 to 55% and very particularly from 30 to 45% by weight of said product.
  • sulfurized calcium alkylphenate denotes any solution containing from 25 to 70% by weight, preferably from 30 to 55% by weight of a sulfurized calcium alkylphenate in a dilution oil which may or may not be the same than that used to prepare the new additive.
  • sulfurized calcium alkylphenates which can be used, there may be mentioned: those obtained by the action of lime on a sulfurized alkylphenol preferably carrying one or more C 9 -C 30 alk y substituents, (and preferably C 9 -C 22 ), such as nonyl, decyl, dodecyl or sulfurized tetradecylphenols followed optionally by carbonation; those obtained by sulfurization with sulfur of an alkylphenol preferably having one or more C 9 -C 30 alkyl substituents (preferably C 9 -C 22 ) in the presence of lime and glycol, optionally followed by carbonation .
  • a sulfurized calcium alkylphenate characterized by a lime / alkylphenol molar ratio of between 0.2 and 2.5 and preferably between 0.4 and 2, and by a sulfur / alkylphenol molar ratio of between 1.1 and 2.2 and preferably between 1.3 and 1.8.
  • active magnesium oxide denotes magnesium oxide MgO with a specific surface greater than or equal to 80 m2 / g, for example between 100 and 170 m2 / g.
  • magnesium oxide MgO with a specific surface greater than or equal to 80 m2 / g, for example between 100 and 170 m2 / g.
  • Maglite DE with a specific surface area close to 140 m2 / g marketed by Merck
  • the "Ferumag” with a specific surface area close to 160 m2 / g and marketed by Rhône-Poulenc.
  • polyalkyleneamines such as polyethyleneamines and very particularly ethylenediamine
  • etheramines and most particularly tris (3-oxa-6-amino hexyl) amine.
  • the amine used may be present in the "milk of magnesia" at the start of the carbonation operation or during it.
  • the carbonation operation is favorably carried out at a temperature which can range from 90 to 140 ° C. and preferably from 110 to 140 ° C., in one or more stages with the introduction of "milk of magnesia” into the medium containing the alkylbenzenesulfonate of magnesium, the sulfurized calcium alkylphenate and the dilution oil in one or more stages, each stage of introduction of "milk of magnesia” being followed by a stage of carbonation. Said carbonation operation is carried out until the sediment level stabilizes; this lasts a maximum of 6 hours.
  • a variant of the process making it possible to prepare the new additive consists in preceding the carbonation operation with a step of precarbonation of the reaction medium consisting of magnesium alkylbenzene sulfonate, sulfurized calcium alkylphenate and oil dilution, in the presence of glycol and possibly sulfur.
  • the new additive which is the subject of the invention has the advantage of being perfectly compatible with viscous oils, of containing a low level of sediment and of being slightly viscous.
  • the present invention also relates to the use of the new additive to improve the detergent, dispersing and anti-wear properties of lubricating oils.
  • the amount of additive to be used depends on the future use of said oils.
  • the amount of additive to be added is generally between 1 and 3.5%; for a diesel engine oil it is generally between 1.8 and 5 X; for a marine engine oil, it can go up to 25%.
  • the lubricating oils which can thus be improved can be chosen from a wide variety of lubricating oils, such as naphthenic, paraffinic and mixed base lubricating oils, other hydrocarbon lubricants, for example lubricating oils derived from products.
  • coal, and synthetic oils for example alkylene polymers, alkylene oxide type polymers and their derivatives, including alkylene oxide polymers prepared by polymerizing alkylene oxide to presence of water or alcohols, for example ethyl alcohol, esters of dicarboxylic acids, liquid esters of phosphorus acids, alkylbenzenes and dialkylbenzenes, polyphenyls, alkylbiphenyl ethers, polymers of silicon.
  • Additional additives may also be present in said lubricating oils alongside the new additive of the invention; include, for example, anti-oxidant, anti-corrosion additives, ashless dispersant additives //
  • the reaction medium is heated for 30 minutes at 110 ° C at atmospheric pressure, then 30 minutes in vacuo so as to distill the reaction water.
  • the mixture is heated to 120 ° C. for 2 hours (1 hour 30 minutes at atmospheric pressure and 30 minutes under a vacuum of 120 10 2 Pa), then the vacuum is broken.
  • Milk of magnesia is prepared in a beaker by mixing, with stirring, active magnesium oxide, glycol and an amine.
  • This milk is divided into three relatively equal fractions.
  • the carbonation operation is continued for 2 hours.
  • the flask is gradually placed under vacuum (40 10 2 Pa) and then heated for 2 hours at 200 ° C.
  • This test is carried out by adding 10% by weight of product to be tested to a SAE 30 mineral oil, storing the solution obtained for 1 month at 20 ° C. and studying the appearance of the solution as a function of time.
  • the finished product is added to a SAE 50 oil with a paraffinic tendency so as to obtain a solution containing 125 milliliters of calcium + magnesium.
  • the solution is stored for 24 hours and then centrifuged under the following conditions:
  • Example 1 The operations described in Example 1 are repeated, carrying out the start of the carbonation step at 130 ° C. instead of 110 ° C.
  • the mixture is heated to 110 ° C. and 112 g of glycol are charged in 1 hour. 0n continues to heat up to 160 ° C.
  • the reactor is placed under vacuum.
  • the vacuum is broken, the heating is stopped and carbonated for 1 hour at a rate of 0.5 g / min.
  • a mixture of 129 g of Mg0 and 349 g of glycol is prepared in a beaker, which mixture is introduced into the reactor over 5 minutes.
  • CO 2 is introduced into the medium. Two hours later, 16.5 g of ethylenediamine are introduced, then two hours more after 85 g of water, then carbonation is continued for a further 2 hours.
  • Example 12 The operations described in Example 12 are repeated in the absence of ethylene diamine.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
  • Detergent Compositions (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
EP83401255A 1982-06-24 1983-06-17 Metallenthaltender Detergens-Dispergierzusatz von hoher Alkalität für Schmieröle Expired EP0101334B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT83401255T ATE30716T1 (de) 1982-06-24 1983-06-17 Metallenthaltender detergens-dispergierzusatz von hoher alkalitaet fuer schmieroele.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8211059A FR2529225B1 (fr) 1982-06-24 1982-06-24 Nouvel additif detergent-dispersant metallique de haute alcalinite pour huiles lubrifiantes
FR8211059 1982-06-24

Publications (3)

Publication Number Publication Date
EP0101334A2 true EP0101334A2 (de) 1984-02-22
EP0101334A3 EP0101334A3 (en) 1985-10-09
EP0101334B1 EP0101334B1 (de) 1987-11-11

Family

ID=9275356

Family Applications (1)

Application Number Title Priority Date Filing Date
EP83401255A Expired EP0101334B1 (de) 1982-06-24 1983-06-17 Metallenthaltender Detergens-Dispergierzusatz von hoher Alkalität für Schmieröle

Country Status (17)

Country Link
US (1) US4470916A (de)
EP (1) EP0101334B1 (de)
JP (1) JPS6025079B2 (de)
AT (1) ATE30716T1 (de)
AU (1) AU559589B2 (de)
BR (1) BR8303369A (de)
CA (1) CA1182627A (de)
DE (1) DE3374403D1 (de)
DK (1) DK289983A (de)
ES (1) ES523539A0 (de)
FR (1) FR2529225B1 (de)
GB (1) GB2123023B (de)
GR (1) GR78595B (de)
PH (1) PH19405A (de)
PT (1) PT76929B (de)
SG (1) SG54685G (de)
ZA (1) ZA834558B (de)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4614602A (en) * 1985-05-01 1986-09-30 Amoco Corporation Lubricant overbased detergent-dispersants with improved solubility
FR2588269B1 (fr) * 1985-10-03 1988-02-05 Elf France Procede de preparation d'additifs surbases tres fluides et a basicite elevee et composition contenant lesdits additifs
US4767551A (en) * 1985-12-02 1988-08-30 Amoco Corporation Metal-containing lubricant compositions
US4664822A (en) * 1985-12-02 1987-05-12 Amoco Corporation Metal-containing lubricant compositions
GB8723909D0 (en) * 1987-10-12 1987-11-18 Exxon Chemical Patents Inc Lubricant oil additive
JP3112569B2 (ja) * 1992-06-25 2000-11-27 ジヤトコ・トランステクノロジー株式会社 自動変速機の変速制御装置
US7084092B2 (en) * 2003-08-25 2006-08-01 M-I L.L.C. Shale hydration inhibition agent and method of use
CN113186015B (zh) * 2021-02-02 2024-02-06 安徽澳润新材料有限公司 一种高碱值磺酸镁清净剂及其制备方法

Family Cites Families (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1605316A (en) * 1925-05-19 1926-11-02 Guiberson Corp Pump-rod guide
US3282835A (en) * 1963-02-12 1966-11-01 Lubrizol Corp Carbonated bright stock sulfonates and lubricants containing them
GB1144084A (en) * 1966-08-24 1969-03-05 Orobis Ltd Improvements in or relating to lubricant additives
US3464970A (en) * 1967-03-13 1969-09-02 Maruzen Oil Co Ltd Process for preparing over-based sulfurized calcium phenates
GB1280749A (en) * 1970-06-18 1972-07-05 Maruzen Oil Company Ltd Process for preparation of over-based sulphurized phenates
GB1399092A (en) * 1971-05-27 1975-06-25 Cooper & Co Ltd Edwin Lubricant additives
US3936480A (en) * 1971-07-08 1976-02-03 Rhone-Progil Additives for improving the dispersing properties of lubricating oil
BE786032A (fr) * 1971-07-08 1973-01-08 Rhone Progil Nouveaux additifs pour huiles lubrifiantes
GB1470338A (en) * 1974-05-17 1977-04-14 Exxon Research Engineering Co Lubricating oil compositions
GB1469289A (en) * 1974-07-05 1977-04-06 Exxon Research Engineering Co Detergent additives
FR2300793A1 (fr) * 1975-02-17 1976-09-10 Orogil Nouvelles compositions lubrifiantes
US4016093A (en) * 1976-03-19 1977-04-05 Mobil Oil Corporation Metal alkylphenate sulfides of reduced corrosiveness and method of preparing same
FR2416942A1 (fr) * 1978-02-08 1979-09-07 Orogil Procede de preparation de detergents-dispersants de haute alcalinite pour huiles lubrifiantes
US4222882A (en) * 1978-02-08 1980-09-16 Rhone-Poulenc Industries Polymers bearing groups derived from N-substituted lactams and their use as lubricating oil additives
US4229308A (en) * 1978-02-08 1980-10-21 Rhone-Poulenc Industries Polymer lubricating oil additives bearing nitrogen groups and their use as additives for lubricating oils
FR2429831A2 (fr) * 1978-06-26 1980-01-25 Orogil Nouveau procede de preparation de detergents-dispersants de haute alcalinite pour huiles lubrifiantes
FR2429832A1 (fr) * 1978-06-26 1980-01-25 Orogil Procede perfectionne de preparation d'additifs detergents-dispersants, metalliques de haute alcalinite notamment pour huiles lubrifiantes
FR2429833A1 (fr) * 1978-06-26 1980-01-25 Orogil Procede de preparation de detergents-dispersants metalliques suralcalinises pour huiles lubrifiantes
FR2450868A1 (fr) * 1979-03-09 1980-10-03 Orogil Procede de preparation d'alkylphenates de magnesium et application des produits obtenus comme additifs detergents-dispersants pour huiles lubrifiantes

Also Published As

Publication number Publication date
GB2123023A (en) 1984-01-25
BR8303369A (pt) 1984-02-07
DK289983D0 (da) 1983-06-23
AU559589B2 (en) 1987-03-12
PH19405A (en) 1986-04-10
PT76929A (fr) 1983-07-01
EP0101334B1 (de) 1987-11-11
GB2123023B (en) 1985-06-05
SG54685G (en) 1986-05-02
US4470916A (en) 1984-09-11
DK289983A (da) 1983-12-25
PT76929B (fr) 1986-01-27
JPS6025079B2 (ja) 1985-06-15
ATE30716T1 (de) 1987-11-15
FR2529225B1 (fr) 1986-04-25
AU1612483A (en) 1984-01-05
CA1182627A (fr) 1985-02-19
EP0101334A3 (en) 1985-10-09
ES8403963A1 (es) 1984-04-01
JPS5947299A (ja) 1984-03-16
GR78595B (de) 1984-09-27
GB8317024D0 (en) 1983-07-27
ES523539A0 (es) 1984-04-01
DE3374403D1 (en) 1987-12-17
ZA834558B (en) 1984-03-28
FR2529225A1 (fr) 1983-12-30

Similar Documents

Publication Publication Date Title
EP0133088B1 (de) Verfahren zur Herstellung von auf Calcium basierten Detergenz-Dispergierzusätzen mit sehr hoher Alkalität und die erhaltenen Produkte
EP0007257B1 (de) Verfahren zur Herstellung von Reinigungsmittellösungen hoher Alkalität für Schmieröle und daraus hergestelltes Produkt
EP0164286B1 (de) Verfahren zur Herstellung von auf nichtschäumenden Erdalkalimetallalkylarylsulfonaten basierenden Zusatzstoffen für Schmieröle mit detergens- und dispersierender Wirkung
FR2605329A1 (fr) Procede de preparation de derives de metal du groupe 2 d'alkylphenols sulfures rendus surbasiques.
FR2917421A1 (fr) Additifs et formulations de lubrifiants pour ameliorer les proprietes antiusure.
EP0102255B1 (de) Verfahren zur Herstellung von sulfurierten Erdalkalimetallalkylphenaten verwendbar als Schmierölzusatz
EP0102254B1 (de) Überalkalisierter Detergens-Dispergierzusatz für Schmieröle
FR2909387A1 (fr) Compositions d'huiles lubrifiantes ayant des proprietes ameliorees de protection contre la corrosion et de protection des joints d'etancheite
FR2910022A1 (fr) Composition d'huile lubrifiante contenant du titane.
FR2909683A1 (fr) Composition d'huile lubrifiante contenant du titane
EP0003694B1 (de) Verfahren zur Bereitung von hochbasischen Mitteln mit detergierender, dispergierender Wirkung für Schmieröle, und so erhaltenes Produkt
JPH0284493A (ja) 過塩基金属スルホン酸塩組成物
EP0007260B1 (de) Verfahren zur Herstellung von Metall enthaltenden reinigenden dispergierenden Zusatzstoffen hoher Alkalität, besonders für Schmieröl, und daraus hergestelltes Produkt
EP0101334B1 (de) Metallenthaltender Detergens-Dispergierzusatz von hoher Alkalität für Schmieröle
FR2915998A1 (fr) Composition d'huile lubrifiante destinee a ameliorer la limitation d'oxydation, d'augmentation de viscosite, de consommation d'huile et de depots sur les pistons.
FR2762848A1 (fr) Utilisation de composes borates pour ameliorer la compatibilite d'huiles lubrifiantes avec des elastomeres fluorocarbones
EP0308445B1 (de) Verfahren zur herstellung eines ein anorganisches borderivat enthaltenden überbasischen additivs, danach erhaltene additive und diese enthaltende schmiermittel
EP0006796B1 (de) Verfahren zur Herstellung von Metall enthaltenden überalkalisierten Reinigungsmittellösungen für Schmieröl und daraus hergestelltes Produkt
EP0211722B1 (de) Sulfonierte und sulfurisierte Detergens Dispergierzusätze für Schmieröle
FR2909684A1 (fr) Additifs et formulations de lubrifiants utilises pour obtenir des proprietes antiusure ameliorees
JP2598489B2 (ja) 過塩基マグネシウムスルホン酸塩組成物
EP4413103A1 (de) Spiroverbindung als reinigungsadditiv in schmiermitteln für schiffsmotoren
EP0957153A1 (de) Schwefelarme, Erdalkali Alkyl Salicylat enthaltende Tenside und ihre Verwendung in Schmierzusammensetzungsformulierungen für Zweitaktmotoren
JPH01308820A (ja) 過塩基化スルホン酸マグネシウムの製造方法
EP0438942A1 (de) Überbasische Detergensmittel für Schmieröle, die ein organisches Derivat von Phosphor enthalten und diese enthaltende Schmierölzusammensetzungen

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 IT LI NL SE

17P Request for examination filed

Effective date: 19840305

PUAL Search report despatched

Free format text: ORIGINAL CODE: 0009013

AK Designated contracting states

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

17Q First examination report despatched

Effective date: 19860821

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

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

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

REF Corresponds to:

Ref document number: 30716

Country of ref document: AT

Date of ref document: 19871115

Kind code of ref document: T

REF Corresponds to:

Ref document number: 3374403

Country of ref document: DE

Date of ref document: 19871217

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

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

Ref country code: AT

Payment date: 19910610

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: 19910614

Year of fee payment: 9

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

Ref country code: CH

Payment date: 19910619

Year of fee payment: 9

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

Ref country code: BE

Payment date: 19910624

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: 19910628

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: 19910630

Year of fee payment: 9

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

Ref country code: AT

Effective date: 19920617

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

Ref country code: SE

Effective date: 19920618

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

Ref country code: LI

Effective date: 19920630

Ref country code: CH

Effective date: 19920630

Ref country code: BE

Effective date: 19920630

BERE Be: lapsed

Owner name: OROGIL

Effective date: 19920630

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

Ref country code: NL

Effective date: 19930101

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee
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: 19930302

EUG Se: european patent has lapsed

Ref document number: 83401255.1

Effective date: 19930109

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

Ref country code: FR

Payment date: 20020605

Year of fee payment: 20