EP2592133B1 - Dégommage enzymatique - Google Patents

Dégommage enzymatique Download PDF

Info

Publication number
EP2592133B1
EP2592133B1 EP20110188382 EP11188382A EP2592133B1 EP 2592133 B1 EP2592133 B1 EP 2592133B1 EP 20110188382 EP20110188382 EP 20110188382 EP 11188382 A EP11188382 A EP 11188382A EP 2592133 B1 EP2592133 B1 EP 2592133B1
Authority
EP
European Patent Office
Prior art keywords
temperature
range
acid
aqueous mixture
vegetable oils
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.)
Active
Application number
EP20110188382
Other languages
German (de)
English (en)
Other versions
EP2592133A1 (fr
Inventor
Alexey Shevchenko
Ling Hua
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.)
Alfa Laval Corporate AB
Original Assignee
Alfa Laval Corporate AB
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 Alfa Laval Corporate AB filed Critical Alfa Laval Corporate AB
Priority to EP20110188382 priority Critical patent/EP2592133B1/fr
Priority to ES11188382.3T priority patent/ES2495991T3/es
Priority to ARP120104221 priority patent/AR088812A1/es
Publication of EP2592133A1 publication Critical patent/EP2592133A1/fr
Application granted granted Critical
Publication of EP2592133B1 publication Critical patent/EP2592133B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/003—Refining fats or fatty oils by enzymes or microorganisms, living or dead
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/04—Refining fats or fatty oils by chemical reaction with acids
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/10—Refining fats or fatty oils by adsorption

Definitions

  • the present invention relates to a method for treating vegetable oils and/or animal fats.
  • fatty oils - of vegetable or animal origin - contain impurities which must be removed before the oil is suitable for consumption. Also fatty oils for technical use often have to be purified to some extent to make them suitable for their purpose.
  • the removing of impurities could be carried out by a degumming and/or winterization process and may be combined into one process a so-called cold degumming process.
  • the traditional cold degumming process is not always successful because:
  • the present invention solves the above mentioned technical problems by the new inventive method.
  • the present invention relates to a new method for treating vegetable oils and/or animal fats to reduce the content of impurities, such as various phospholipids i.e. gums, wax and/or high melting glycerides.
  • impurities such as various phospholipids i.e. gums, wax and/or high melting glycerides.
  • One aspect of the invention to provide a method for efficiently removing both the phospholipids and the high melting glycerides by phospholipase at the same time.
  • Another aspect of the invention to provide a method for utilizing the enzyme reaction feature such as the reacted gum has lower viscosity and less emulsification strength to achieve less oil loss.
  • the main purpose of a degumming process is to remove phospholipids from the oil.
  • oil types such as sunflower seed oil, rice bran oil, corn oil, winterization process is needed to remove the high melting glycerides to avoid problems in the use of the oils at lower temperature or in later process.
  • the enzymatic degumming process has been proven effective in gum removal.
  • the phospholipids are converted to lyso-phospholipids and free fatty acids i.e. FFA.
  • the lyso-phospholipids have much less emulsion capacity and lower viscosity. So, it is expected that the separation at lower temperature in enzymatic degumming process is much better than in a conventional process.
  • lyso-phospholipids are water-soluble, it is expected that most lyso-phospholipids will stay in the water phase during wax crystallation and crystal growth, so that the inhibition due to the presence of gums is eliminated.
  • the cold enzymatic degumming process will provide the possibility of making degumming and dewaxing simultaneously, and with significant low loss of neutral oil
  • the new method for treating vegetable oils and/or animal fats according to the invention comprises the following steps:
  • step (i) the temperature of the vegetable oils and/or animal fats may be adjusted within the range from about 60 to about 90°C.
  • the vegetable oils and/or animal fats may be treated with acid from about 1 to about 60 minutes, preferably from about 5 to about 60 minutes, most preferred from about 20 to about 40 minutes.
  • the pH in step (iii) may be adjusted with lye to a pH within a range from about 4 to about 8 at a temperature preferably from about 40 to about 60°C.
  • the lye in step (iii) is selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium silicate, sodium carbonate, calcium carbonate, and a combination thereof, preferably sodium hydroxide or potassium hydroxide. According to the invention the mixing of the lye in step (iii) may be continued within the range from about 1 min to about 4 hours.
  • the temperature of the aqueous mixture in step (v) may be adjusted by a cooling rate and by a residence time to optimize crystallisation, preferably by a cooling rate within the range of from about 0.5 degrees per hour to about 5 degrees per hour, and a residence time within the range of from about 4 to 24 hours, preferably from 6 to 12 hours.
  • the temperature of the aqueous mixture in separation step (vi) may be adjusted to facilitate separation, preferably the temperature is within the range of from about 15 to about 50°C.
  • the enzyme in treatment step (iv) may be a phospholipase enzyme, preferably one or more phospholipase A enzymes, or one or more phospholipase C enzymes, or a combination thereof.
  • the acid used in step (ii) is selected from the group consisting of phosphoric acid, acetic acid, citric acid, tartaric acid, succinic acid, and a mixture thereof, preferrably phosphoric acid or citric acid.
  • the equipment used in this experiment was an oil bath, Erlenmeyer flasks 500 ml, magnetic stirrer with heating and temperature control, an Ultra Turrax, a laboratory centrifuge.
  • FFA is analyzed according to method according to American Oil Chemists' Society, AOCS, Ca 5a-40, moisture is analyzed according to method AOCS Ca 2b-38, and phosphorus is analyzed according to method DIN EN 14107.
  • the crude sunflower seed oil was heated in oven to 70°C to ensure all the wax crystals are melted and dissolved in the oil.
  • A normal enzymatic deep degumming
  • B cold enzymatic deep degumming
  • a citric acid solution i.e. 5 ml
  • a sodium hydroxide solution was prepared, i.e. 5 ml, by dissolving 0,5075g sodium hydroxide pellets in distilled water.
  • the oil bath for flask A is heated to 80°C to inactivate the enzyme; while flask B was moved together with the magnetic agitator to fridge (7 - 8°C), and the agitation was kept at ca. 40 rpm for an overnight.
  • flask B and the magnetic agitator were removed from the fridge, and the agitation was kept at room temperature (about 22°C) for ca. 15 min.
  • the oil from flask B was centrifuged for 5 min. at 2000X g and the moisture, FFA and phosphorus content in the light phase were analysed.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Fats And Perfumes (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Claims (13)

  1. Procédé de traitement d'huiles végétales et/ou de graisses animales, comprenant les étapes suivantes :
    (i) ajustement de la température des huiles végétales et/ou graisses animales dans la fourchette d'environ 20 à environ 90 °C ;
    (ii) prétraitement des huiles végétales et/ou graisses animales avec un acide pendant au moins 1 minute ;
    (iii) ajustement du pH avec de la lessive jusqu'à un pH dans une fourchette d'environ 4 à environ 8 à une température d'au moins 20 °C pour obtenir un mélange aqueux ;
    (iv) addition d'enzymes au mélange aqueux ;
    (v) réduction de la température du mélange aqueux jusqu'à la température de cristallisation des glycérides à haut point de fusion ;
    (vi) séparation du mélange aqueux en une phase aqueuse et une phase d'huiles végétales et/ou de graisses animales traitées ; et
    (vii) éventuellement, traitement de la phase d'huiles végétales et/ou de graisses animales traitées avec de l'eau chaude ou avec une adsorption sur silice.
  2. Procédé selon la revendication 1, dans lequel la température dans l'étape (i) est ajustée dans une fourchette d'environ 40 à environ 90 °C.
  3. Procédé selon la revendication 1 ou 2, dans lequel dans l'étape de prétraitement (ii), les huiles végétales et/ou graisses animales sont traitées avec un acide pendant environ 1 à environ 60 minutes, de préférence environ 5 à environ 60 minutes, mieux encore environ 20 à environ 40 minutes.
  4. Procédé selon la revendication 1, 2 ou 3, dans lequel le pH dans l'étape (iii) est ajusté avec la lessive à un pH compris dans la fourchette d'environ 4 à environ 8 à une température d'environ 40 à environ 60 °C.
  5. Procédé selon l'une quelconque des revendications 1 à 4, dans lequel la température du mélange aqueux dans l'étape (v) est ajustée par une vitesse de refroidissement et par un temps de séjour visant à optimiser la cristallisation, de préférence par une vitesse de refroidissement comprise dans la fourchette d'environ 0,5 degré par heure à environ 5 degrés par heure, et un temps de séjour compris dans la fourchette d'environ 4 à 24 heures, de préférence de 6 à 12 heures.
  6. Procédé selon l'une quelconque des revendications 1 à 5, dans lequel la température du mélange aqueux dans l'étape de séparation (vi) est ajustée pour faciliter la séparation.
  7. Procédé selon l'une quelconque des revendications 1 à 6, dans lequel la température du mélange aqueux dans l'étape de séparation (vi) est ajustée pour faciliter la séparation, de préférence la température est comprise dans la fourchette d'environ 15 à environ 50 °C.
  8. Procédé selon l'une quelconque des revendications 1 à 7, dans lequel l'enzyme dans l'étape de traitement (iv) est une enzyme phospholipase, de préférence des enzymes phospholipases A ou des enzymes phospholipases C, ou une combinaison de celles-ci.
  9. Procédé selon l'une quelconque des revendications 1 à 8, dans lequel l'acide dans l'étape (ii) est choisi dans l'ensemble consistant en acide phosphorique, acide acétique, acide citrique, acide tartrique, acide succinique et une combinaison de ceux-ci, de préférence l'acide phosphorique ou l'acide citrique.
  10. Procédé selon l'une quelconque des revendications 1 à 9, dans lequel la température dans l'étape (i) est ajustée pour être comprise dans la fourchette d'environ 60 à environ 90 °C.
  11. Procédé selon l'une quelconque des revendications 1 à 10, dans lequel le mélange de l'enzyme dans l'étape (iv) est poursuivi pendant une durée comprise dans la fourchette d'environ 1 min à environ 6 heures.
  12. Procédé selon l'une quelconque des revendications 1 à 11, dans lequel le mélange de la lessive dans l'étape (iii) est poursuivi pendant une durée comprise dans la fourchette d'environ 1 min à environ 4 heures.
  13. Procédé selon l'une quelconque des revendications 1 à 12, dans lequel la lessive dans l'étape (iii) est choisie dans l'ensemble consistant en hydroxyde de sodium, hydroxyde de potassium, silicate de sodium, carbonate de sodium, carbonate de calcium et une combinaison de ceux-ci, de préférence l'hydroxyde de sodium ou l'hydroxyde de potassium.
EP20110188382 2011-11-09 2011-11-09 Dégommage enzymatique Active EP2592133B1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP20110188382 EP2592133B1 (fr) 2011-11-09 2011-11-09 Dégommage enzymatique
ES11188382.3T ES2495991T3 (es) 2011-11-09 2011-11-09 Desengomado enzimático
ARP120104221 AR088812A1 (es) 2011-11-09 2012-11-08 Desgomado enzimatico

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP20110188382 EP2592133B1 (fr) 2011-11-09 2011-11-09 Dégommage enzymatique

Publications (2)

Publication Number Publication Date
EP2592133A1 EP2592133A1 (fr) 2013-05-15
EP2592133B1 true EP2592133B1 (fr) 2014-06-04

Family

ID=44992680

Family Applications (1)

Application Number Title Priority Date Filing Date
EP20110188382 Active EP2592133B1 (fr) 2011-11-09 2011-11-09 Dégommage enzymatique

Country Status (3)

Country Link
EP (1) EP2592133B1 (fr)
AR (1) AR088812A1 (fr)
ES (1) ES2495991T3 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9340749B1 (en) 2015-05-06 2016-05-17 Arisdyne Systems, Inc. Method for degumming triglyceride oils
WO2016178676A1 (fr) * 2015-05-06 2016-11-10 Arisdyne Systems, Inc. Procédé de dégommage d'huiles triglycéridiques

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2600003C1 (ru) * 2012-10-31 2016-10-20 Альфа Лаваль Корпорейт Аб Ферментативное обессмоливание
DE102014210662A1 (de) * 2014-06-04 2015-12-17 Gea Westfalia Separator Group Gmbh Vorrichtung und Verfahren zur Gewinnung von Glycoglycerolipiden und Glycosphingolipiden aus lipoiden Phasen
WO2018217270A1 (fr) 2017-05-24 2018-11-29 Arisdyne Systems, Inc. Systèmes de démucilagination d'huile

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB382946A (en) * 1931-07-23 1932-10-24 Leslie William Mapson Improvements in or relating to the manufacture of concentrated edible products
DE4339556C1 (de) * 1993-11-19 1995-02-02 Metallgesellschaft Ag Verfahren zum Entschleimen von Pflanzenöl mittels Enzymen
EP1876222A1 (fr) * 2006-07-06 2008-01-09 Cognis IP Management GmbH Procede de production d 'acides gras, d'esters d'acides gras et d'esters de sterol à partir de solution savonneuse
DK2118248T3 (da) * 2007-01-30 2014-11-03 Bunge Oils Inc Enzymatisk degummiering under anvendelse af en blanding af PLA- og PLC-phospholipaser
GB0904787D0 (en) * 2009-03-20 2009-05-06 Desmet Ballestra Engineering Sa Improved enzymatic oil recuperation process

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9340749B1 (en) 2015-05-06 2016-05-17 Arisdyne Systems, Inc. Method for degumming triglyceride oils
WO2016178676A1 (fr) * 2015-05-06 2016-11-10 Arisdyne Systems, Inc. Procédé de dégommage d'huiles triglycéridiques
US9556399B2 (en) 2015-05-06 2017-01-31 Arisdyne Systems, Inc. Method for degumming triglyceride oils
EP3292190A4 (fr) * 2015-05-06 2018-12-19 Arisdyne Systems Inc. Procédé de dégommage d'huiles triglycéridiques

Also Published As

Publication number Publication date
EP2592133A1 (fr) 2013-05-15
AR088812A1 (es) 2014-07-10
ES2495991T3 (es) 2014-09-18

Similar Documents

Publication Publication Date Title
EP2594625B1 (fr) Procédé d'ajustement de la teneur du 3-chloro-1,2-propanediol ou d'esters de celui-ci dans des huiles et des matières grasses
US8956853B2 (en) Enzymatic degumming utilizing a mixture of PLA and PLC phospholipases
EP2592133B1 (fr) Dégommage enzymatique
EP2118248B1 (fr) Dégommage enzymatique utilisant un mélange de phospholipases pla et plc
EP2053118B1 (fr) Démucilagination d'huile sans émulsion
US7081542B2 (en) Chemical process for the production of 1,3-diglyceride oils
WO2010126136A1 (fr) Procédé d'inhibition de la production d'un composé chloropropanol et substance de formation d'un composé chloropropanol dans l'huile et graisse de glycérides
EP2471897A1 (fr) Procédés de réduction des chloropropanols et d'une de leurs substances formatives, l'ester d'acide gras de glycidol, contenus dans les huiles glycéridiques
CN108707508B (zh) 玉米油脱胶脱蜡一步法精炼工艺
WO2017008335A1 (fr) Procédé de raffinage sans savon d'huile de maïs
JPS63191899A (ja) トリグリセリド油の脱ガム化方法
US4584141A (en) Process relating to triglyceride oils
JPS5933159B2 (ja) 油の精製方法
JP5868967B2 (ja) 植物油の処理
KR890001463B1 (ko) 유(油)의 정제방법
US10329514B2 (en) Enzymatic degumming
US8460905B2 (en) Enzymatic degumming utilizing a mixture of PLA and PLC phospholipases with reduced reaction time
US8435766B2 (en) Enzymatic oil recuperation process
CN113122381A (zh) 一种提高油脂抗冷冻性能的方法
CN112063452A (zh) 一种保健稻米油及其生产方法
JP2709126B2 (ja) フライ用油脂の製造方法
CN111040873A (zh) 一种鱼油加工精制过滤工艺
CN113122379A (zh) 一种提高油脂抗冻性能的方法
CN113122384A (zh) 提升油脂抗冻性能的方法
DK2892986T3 (en) PROCEDURE FOR TREATING A VEGETABLE FAT COMPOSITION

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

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

AX Request for extension of the european patent

Extension state: BA ME

17P Request for examination filed

Effective date: 20131112

RBV Designated contracting states (corrected)

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

RIC1 Information provided on ipc code assigned before grant

Ipc: C11B 3/04 20060101ALI20131126BHEP

Ipc: C11B 3/00 20060101AFI20131126BHEP

Ipc: C11B 3/10 20060101ALI20131126BHEP

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

INTG Intention to grant announced

Effective date: 20140109

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: AT

Ref legal event code: REF

Ref document number: 671120

Country of ref document: AT

Kind code of ref document: T

Effective date: 20140615

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602011007391

Country of ref document: DE

Effective date: 20140717

REG Reference to a national code

Ref country code: RO

Ref legal event code: EPE

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2495991

Country of ref document: ES

Kind code of ref document: T3

Effective date: 20140918

REG Reference to a national code

Ref country code: NL

Ref legal event code: T3

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

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140904

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140905

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

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

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

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

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141006

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

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141004

REG Reference to a national code

Ref country code: HU

Ref legal event code: AG4A

Ref document number: E021715

Country of ref document: HU

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602011007391

Country of ref document: DE

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: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

26N No opposition filed

Effective date: 20150305

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602011007391

Country of ref document: DE

Effective date: 20150305

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

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

Ref country code: LU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141109

Ref country code: BE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

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: LI

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

Effective date: 20141130

Ref country code: CH

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

Effective date: 20141130

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 5

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

Ref country code: IE

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

Effective date: 20141109

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

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

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

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

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

Effective date: 20151109

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

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 6

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

Ref country code: GB

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

Effective date: 20151109

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 7

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

Ref country code: MK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 8

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

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20140604

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

Ref country code: AT

Payment date: 20191025

Year of fee payment: 9

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 671120

Country of ref document: AT

Kind code of ref document: T

Effective date: 20201109

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

Ref country code: AT

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

Effective date: 20201109

P01 Opt-out of the competence of the unified patent court (upc) registered

Effective date: 20230417

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

Ref country code: NL

Payment date: 20230915

Year of fee payment: 13

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

Ref country code: FR

Payment date: 20230911

Year of fee payment: 13

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

Ref country code: ES

Payment date: 20231208

Year of fee payment: 13

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

Ref country code: TR

Payment date: 20231108

Year of fee payment: 13

Ref country code: RO

Payment date: 20231005

Year of fee payment: 13

Ref country code: IT

Payment date: 20231010

Year of fee payment: 13

Ref country code: HU

Payment date: 20231009

Year of fee payment: 13

Ref country code: DE

Payment date: 20230912

Year of fee payment: 13