EP2012929B1 - Flotationsreagenz für silikathaltige mineralien - Google Patents

Flotationsreagenz für silikathaltige mineralien Download PDF

Info

Publication number
EP2012929B1
EP2012929B1 EP07724263.4A EP07724263A EP2012929B1 EP 2012929 B1 EP2012929 B1 EP 2012929B1 EP 07724263 A EP07724263 A EP 07724263A EP 2012929 B1 EP2012929 B1 EP 2012929B1
Authority
EP
European Patent Office
Prior art keywords
flotation
silicate
collector
group
carbon atoms
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.)
Not-in-force
Application number
EP07724263.4A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP2012929A1 (de
Inventor
Klaus-Ulrich Pedain
Tobias Rau
Michael Patzke
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.)
Clariant Finance BVI Ltd
Original Assignee
Clariant Finance BVI Ltd
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 Clariant Finance BVI Ltd filed Critical Clariant Finance BVI Ltd
Publication of EP2012929A1 publication Critical patent/EP2012929A1/de
Application granted granted Critical
Publication of EP2012929B1 publication Critical patent/EP2012929B1/de
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/01—Organic compounds containing nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/02—Collectors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; Specified applications
    • B03D2203/02—Ores
    • B03D2203/04—Non-sulfide ores

Definitions

  • the present invention relates to the use of alkyltriarnines in the flotation of siliceous minerals and ores.
  • Calcium carbonate is purified from silicate-containing and color-providing minerals with the aid of quaternary ammonium salts based on fatty acids or fatty alkylimidazoline compounds. Since calcium carbonate is used in addition to kaolin, rutile and talc as a white pigment in paper and plastic production, the highest possible whiteness or a low concentration of coloring minerals is desired. Due to the hardness of silicate, this would also lead to increased wear on the calenders of paper machines in papermaking. Therefore, calcium carbonate is purified in addition to dry processing via the flotation process.
  • the aim is to reduce the silicate content, which in the case of calcium carbonate is often characterized as an acid-insoluble constituent, by less than 1.0% by weight due to the reverse flotation.
  • the content of silicate in the task can vary and in some cases be from 10 to 20% by weight.
  • fatty amines alkyl ether amines, alkyl ether diamines or quaternary ammonium salt compounds are used as silicate collectors. These are also known under the trade name Flotigam ®.
  • Alkyl ether amines and alkyl ether diamines are mostly used in their partially neutralized forms as partial acetates, as in U.S. 4,319,987 described. The reason for this is the better solubility of the partially neutralized amine functions.
  • U.S. 4,995,965 describes the use of methyl bis (2-hydroxypropyl) cocosammonium methyl sulfate as a flotation reagent to float silicate-containing impurities out of calcite.
  • the silicate flotation, including iron ore, with the help of Alkyloxyalkanaminen is in U.S. 5,540,337 described.
  • U.S. 5,720,873 describes the combination of quaternary ammonium salts with fattyoxyalkylene compounds for the purification of calcium carbonate. This combination achieved an improvement over the quaternary ammonium salts in separating acid-insoluble components.
  • the object of the present invention was therefore to provide an improved collector for the silicate flotation, which can be used in particular in the reverse flotation but also in the direct flotation.
  • the collectors used today for the flotation of silicate-containing minerals have relatively high specific amounts used, which can lead to environmental problems with regard to the residual content of amine in the concentrate or in the mountains. It is known that amines and amine derivatives have high aqua and environmental toxicity. Therefore, one strives to minimize their specific amounts. Furthermore, their residual concentration in the final product should be kept as low as possible.
  • alkyl dipropylene triamines leads to a marked improvement in the flotation of silicate-containing minerals compared to the known flotation reagents, it being possible to significantly reduce the specific amounts used.
  • the invention thus relates to the use of a compound of formula 1 RN- [A-NH 2 ] 2 (1) wherein R is a linear or branched alkyl group or alkenyl group having 6 to 20 carbon atoms and A is a propylene group (-C 3 H 6 -), as a collector in the silicate flotation.
  • Another object of the invention is a method for flotation of silicate mineral by bringing a compound of formula 1 with the silicate-containing mineral in contact.
  • Another object of the invention is a composition containing 1 to 99 wt .-% of a collector for silicate flotation, which is an alkyl ether, alkyletherdiamine, alkylamine or quaternary ammonium salt, and 1 to 99 wt .-% of a compound of formula 1.
  • a collector for silicate flotation which is an alkyl ether, alkyletherdiamine, alkylamine or quaternary ammonium salt, and 1 to 99 wt .-% of a compound of formula 1.
  • the compound of formula 1 is also referred to below as a collector according to the invention.
  • the collector according to the invention can be used alone or in combination with other nitrogen-containing compounds for the flotation of silicate, in particular iron ore, phosphate or calcium carbonate.
  • Preferred nitrogen-containing compounds are alkyl ether amines, alkyl ether diamines, alkyl amines or quaternary ammonium salts.
  • the ratio of alkyletheramine, alkyletherdiamine, alkylamine or quaternary ammonium salt to compound of the formula is preferably between 95: 5 and 50:50 by weight.
  • R is a linear or branched hydrocarbon group. It is further preferred that R comprises 8 to 18 carbon atoms. Particularly preferred are 2-ethylhexyl, isononane, isodecane and Isotridekan- and dodecane radicals.
  • the silicate flotation collectors which are an alkyl ether amine, alkyl ether diamine, alkyl amine or quaternary ammonium salt, and which may be used together with a compound of formula 1, are preferably one or more of the compounds of formulas (II) to (V) ).
  • the use of the flotation reagent according to the invention can also be carried out in combination with foaming agents and pushers, as known from the prior art.
  • hydrophilic polysaccharides such as, for example, modified starch, carboxymethylcellulose or gum arabic in dosages of from 10 to 1000 g / t as a pusher.
  • the silicate flotation is preferably carried out at a pH of 7 to 12, in particular 8 to 11, which is set, for example, with sodium hydroxide.
  • the use according to the invention can be carried out both in direct and in reverse silicate flotation.
  • the use according to the invention is also suitable for liberating silicate sand from impurities by flotatively separating the silicate sand from the impurities using the compound of formula 1.
  • Table 1 presents the flotative results of the collector B according to the invention in comparison to the standard reagent A.
  • the flotation experiments were carried out on a silicate-containing calcium carbonate, the acid-insoluble constituents in the task accounting for 14.9%.
  • the reagent according to the invention in Example 6 already at a low dosage of only 121 g / t shows a much lower proportion of acid-insoluble constituents in the purified concentrate, which the standard reagent only reaches above 400 g / t.
  • the reagent according to the invention behaves analogously with regard to the degree of whiteness. This is already at the low dosage 92.0, which is achieved with the standard reagent only with three to four times the amount used.
  • Table 2 Effectiveness of a mixture of the collector B according to the invention and the standard collector A.
  • Examples 7 to 10 represent mixtures containing 10% of the collector B according to the invention and 90% of the standard collector A.
  • Examples 11 to 16 show mixtures containing about 29% of the collector B according to the invention and about 71% of the standard collector A, represents.
  • the flotation reagent according to the invention can be used in a wide pH range, for example 6 to 12, preferably 6 to 8, and is added to the aqueous slurry in a concentration of preferably between 0.001 and 1.0 kg / ton of crude mineral.

Landscapes

  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Detergent Compositions (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
EP07724263.4A 2006-04-27 2007-04-16 Flotationsreagenz für silikathaltige mineralien Not-in-force EP2012929B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006019561A DE102006019561A1 (de) 2006-04-27 2006-04-27 Flotationsreagenz für silikathaltige Mineralien
PCT/EP2007/003325 WO2007124853A1 (de) 2006-04-27 2007-04-16 Flotationsreagenz für silikathaltige mineralien

Publications (2)

Publication Number Publication Date
EP2012929A1 EP2012929A1 (de) 2009-01-14
EP2012929B1 true EP2012929B1 (de) 2013-12-25

Family

ID=38229339

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07724263.4A Not-in-force EP2012929B1 (de) 2006-04-27 2007-04-16 Flotationsreagenz für silikathaltige mineralien

Country Status (11)

Country Link
US (1) US8172089B2 (ru)
EP (1) EP2012929B1 (ru)
AU (1) AU2007245895B2 (ru)
BR (1) BRPI0710802A2 (ru)
CA (1) CA2650392C (ru)
DE (1) DE102006019561A1 (ru)
ES (1) ES2444409T3 (ru)
NO (1) NO20084515L (ru)
RU (1) RU2440854C2 (ru)
WO (1) WO2007124853A1 (ru)
ZA (1) ZA200808846B (ru)

Families Citing this family (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006010939A1 (de) * 2006-03-09 2007-09-13 Clariant International Limited Flotationsreagenz für Silikate
BRPI0705593B1 (pt) * 2007-11-22 2016-04-12 Univ Minas Gerais método de quantificação de aminas em resíduos de flotação de minério de ferro
CN101337204B (zh) * 2008-08-13 2011-03-30 中南大学 一种双季铵盐类化合物在硅酸盐矿物浮选上的应用及硅酸盐矿物浮选捕收剂
CN101869874A (zh) * 2009-04-22 2010-10-27 莱芜市金石特种合金材料有限公司 高纯铁精矿粉用浮选药剂
DE102010004893A1 (de) * 2010-01-19 2011-07-21 Clariant International Limited Flotationsreagenz für magnetit- und/oder hämatithaltige Eisenerze
US9346061B2 (en) 2011-04-13 2016-05-24 Basf Se Diamine compounds and their use for inverse froth flotation of silicate from iron ore
KR20140023974A (ko) * 2011-04-13 2014-02-27 바스프 에스이 철광석으로부터 규산염의 역 포말 부유선별을 위한 아민 및 디아민 화합물 및 이의 용도
EP2679311A1 (en) * 2012-06-30 2014-01-01 Clariant S.A., Brazil Foam prevention in the reverse flotation process for purifying calcium carbonate
CN103272699B (zh) * 2013-05-31 2015-05-27 北京矿冶研究总院 一种花岗岩型矿石的分离方法
CN103657859A (zh) * 2013-11-21 2014-03-26 成都兴能新材料有限公司 石英砂浮选除长石的方法
BR112017001835B1 (pt) * 2014-08-01 2023-02-07 Samarco Mineração S.a. Processo para concentração de um minério de ferro
US20160114337A1 (en) * 2014-10-23 2016-04-28 Georgia-Pacific Chemicals Llc Polyamidoamine cationic collectors and methods for making and using same
WO2016065185A1 (en) * 2014-10-23 2016-04-28 Georgia-Pacific Chemicals Llc Cationic collectors with mixed polyamidoamines and methods for making and using same
EP3481558B1 (en) * 2016-07-08 2020-09-16 Nouryon Chemicals International B.V. Process to treat magnetite ore and collector composition
CN107899753B (zh) * 2017-10-09 2019-12-27 中南大学 一种无氟浮选分离石英和长石的阴离子组合捕收剂及其制备方法与应用
CN110152889A (zh) * 2019-06-04 2019-08-23 瓮福（集团）有限责任公司 一种硅钙质磷矿反浮选脱硅除杂组合捕收剂及其制备方法和应用
AU2023238067A1 (en) 2022-03-25 2024-09-12 Clariant International Ltd Novel cationic collectors for improving a process for froth flotation of silicates
CN115957891A (zh) * 2022-08-30 2023-04-14 武汉工程大学 一种磷石膏浮选净化方法
CN117258995B (zh) * 2023-09-19 2024-03-22 安徽省地质实验研究所(国土资源部合肥矿产资源监督检测中心) 一种从花岗伟晶岩选矿尾矿中提取低铁高纯石英和长石的方法

Family Cites Families (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2494132A (en) * 1948-03-10 1950-01-10 American Cyanamid Co Beneficiation of acidic minerals
US2569417A (en) * 1948-03-10 1951-09-25 American Cyanamid Co Beneficiation of acidic minerals
DE1259264B (de) 1966-12-24 1968-01-25 Hoechst Ag Verfahren zur Flotation von Sylvin aus Kali-Rohsalzen
DD64275A5 (de) * 1967-11-09 1968-10-20 Hoechst Ag Verfahren zur flotation von sylvin aus kali-rohsalzen
FR2104657B1 (ru) * 1970-05-08 1973-12-21 Pierrefitte Auby Sa
US3834533A (en) * 1972-09-11 1974-09-10 Continental Oil Co Concentration of oxide copper ores by flotation separation
SE386083B (sv) 1975-01-15 1976-08-02 Berol Kemi Ab Forfarande for flotation av bly-, uran- och sellsynta jordartsmineral ur malmer
FR2367820A1 (fr) * 1976-10-18 1978-05-12 Ceca Sa Procede de flottation de minerais oxydes
JPS53117014A (en) * 1977-03-24 1978-10-13 Kao Corp Emulsifier for asphalt emulsions
US4227996A (en) * 1979-03-22 1980-10-14 Celanese Corporation Flotation process for improving recovery of phosphates from ores
US4198288A (en) * 1979-03-22 1980-04-15 Celanese Polymer Specialties Company Desliming of potash ores
US4319987A (en) 1980-09-09 1982-03-16 Exxon Research & Engineering Co. Branched alkyl ether amines as iron ore flotation aids
US4830739A (en) 1985-02-20 1989-05-16 Berol Kemi Ab Process and composition for the froth flotation beneficiation of iron minerals from iron ores
FR2625115B1 (fr) 1987-12-24 1990-10-19 Denain Anzin Mineraux Refract Procede d'enrichissement de l'andalousite
DE3818482A1 (de) * 1988-05-31 1989-12-07 Henkel Kgaa Tensidmischungen als sammler fuer die flotation nichtsulfidischer erze
US4995965A (en) 1988-06-13 1991-02-26 Akzo America Inc. Calcium carbonate beneficiation
DE4133063A1 (de) * 1991-10-04 1993-04-08 Henkel Kgaa Verfahren zur herstellung von eisenerzkonzentraten durch flotation
US5261539A (en) 1992-10-07 1993-11-16 American Cyanamid Company Flotation process for purifying calcite
FR2700976B1 (fr) * 1993-02-04 1995-04-21 Mircal Procédé de récupération des micas par flottation et micas ainsi obtenus.
SE501623C2 (sv) 1993-05-19 1995-04-03 Berol Nobel Ab Sätt att flotera kalciumkarbonatmalm samt ett flotationsreagens därför
US5540337A (en) 1994-04-04 1996-07-30 Baker Hughes Incorporated Alkyloxyalkaneamines useful as cationic froth flotation collectors
SE521949C2 (sv) 1997-11-27 2003-12-23 Akzo Nobel Nv Förfarande för skumflotation av silikatinnehållande järnmalm
SE514435C2 (sv) 1999-04-20 2001-02-26 Akzo Nobel Nv Kvartära ammoniumföreningar för skumflotation av silikater från järnmalm
CH703678B1 (de) * 2004-04-06 2012-03-15 Empa Testmaterialien Ag Verfahren und Einrichtung zum Testen bakterizider Wirkung von Substanzen.
DE102006010939A1 (de) 2006-03-09 2007-09-13 Clariant International Limited Flotationsreagenz für Silikate

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
V. E. LIMANOV, S. A. RAPIN AND S. B. IVANOV: "Synthesis of higher aliphatic alkylpolyamines", PHARMACEUTICAL CHEMISTRY JOURNAL, vol. 15, no. 3, March 1981 (1981-03-01), pages 213 - 214, DOI: 10.1007/BF00758467 *

Also Published As

Publication number Publication date
WO2007124853A1 (de) 2007-11-08
RU2440854C2 (ru) 2012-01-27
DE102006019561A1 (de) 2007-10-31
EP2012929A1 (de) 2009-01-14
NO20084515L (no) 2008-11-04
ES2444409T3 (es) 2014-02-24
BRPI0710802A2 (pt) 2011-08-23
US8172089B2 (en) 2012-05-08
RU2008146768A (ru) 2010-06-10
AU2007245895B2 (en) 2010-09-02
CA2650392A1 (en) 2007-11-08
US20090152174A1 (en) 2009-06-18
ZA200808846B (en) 2009-12-30
CA2650392C (en) 2014-01-07
AU2007245895A1 (en) 2007-11-08

Similar Documents

Publication Publication Date Title
EP2012929B1 (de) Flotationsreagenz für silikathaltige mineralien
DE102008056338B4 (de) Flotationsreagenz für silikathaltige Mineralien
EP1996333B1 (de) Flotationsreagenz für silikate
DE69422618T2 (de) Verfahren und reagenz zur flotation von kalziumkarbonaterz
DE3688591T2 (de) Verfahren zur selektiven trennung von kupfer-molybdenerz.
EP1528957B1 (de) Verwendung eines sammlers für sulfidische erze und verfahren zu seiner herstellung
EP2525915B1 (de) Flotationsreagenz für magnetit- und/oder hämatithaltige eisenerze
EP0270018B1 (de) Verwendung von N-Alkyl- und N-Alkenylasparaginsäuren als Co-Sammler für die Flotation nichtsulfidischer Erze
EP0193109B1 (de) Verfahren zur Aufbereitung von Kaolinit durch Flotation
DD237482A1 (de) Verfahren fuer die flotation von erzen
EP3740319B1 (de) Esterquats zur flotation von nicht-sulfidischen mineralien und erzen und verfahren
EP2813475B1 (de) Verfahren zum entfernen von quecksilber und selen aus sulfathaltigem abwasser
DE10217693C1 (de) Verwendung von Fettaminsalzen in Kombination mit Fettsäuren als Hilfsmittel für die Flotation von Kalisalzen (Sylvinit)
AT397047B (de) Verfahren und zusammensetzung zur anreicherung von carbonatmineralien
DE1261454B (de) Aminsammler fuer die Sylvinflotation
DE555921C (de) Schaumschwimmaufbereitungsverfahren von Phosphaten und sonstigen nichtsulfidischen Mineralien
DE622872C (de) Verfahren zur Gewinnung von Mineralien aus Erzen nach dem Schwimmverfahren
DD207694A1 (de) Verfahren zur gewinnung von quecksilber aus waessrigen loesungen
DD207693A1 (de) Verfahren zur gewinnung von gold und/oder palladium aus waessrigen loesungen

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

17P Request for examination filed

Effective date: 20081127

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC MT NL PL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: AL BA HR MK RS

RIN1 Information on inventor provided before grant (corrected)

Inventor name: RAU, TOBIAS

Inventor name: PEDAIN, KLAUS-ULRICH

Inventor name: PATZKE, MICHAEL

17Q First examination report despatched

Effective date: 20090225

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: CLARIANT FINANCE (BVI) LIMITED

DAX Request for extension of the european patent (deleted)
GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

INTG Intention to grant announced

Effective date: 20130719

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): AT BE DE ES FI NL SE

RBV Designated contracting states (corrected)

Designated state(s): AT BE DE ES FI NL SE

REG Reference to a national code

Ref country code: AT

Ref legal event code: REF

Ref document number: 646288

Country of ref document: AT

Kind code of ref document: T

Effective date: 20140115

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 502007012635

Country of ref document: DE

Effective date: 20140213

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2444409

Country of ref document: ES

Kind code of ref document: T3

Effective date: 20140224

REG Reference to a national code

Ref country code: SE

Ref legal event code: TRGR

REG Reference to a national code

Ref country code: NL

Ref legal event code: T3

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

Ref country code: SE

Payment date: 20140219

Year of fee payment: 8

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

Ref country code: BE

Payment date: 20140307

Year of fee payment: 8

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

Ref country code: FI

Payment date: 20140416

Year of fee payment: 8

Ref country code: DE

Payment date: 20140227

Year of fee payment: 8

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 502007012635

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

26N No opposition filed

Effective date: 20140926

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 502007012635

Country of ref document: DE

Effective date: 20140926

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 502007012635

Country of ref document: DE

REG Reference to a national code

Ref country code: SE

Ref legal event code: EUG

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

Ref country code: DE

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

Effective date: 20151103

Ref country code: FI

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

Effective date: 20150416

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

Ref country code: SE

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

Effective date: 20150417

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

Ref country code: ES

Payment date: 20160222

Year of fee payment: 10

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

Ref country code: NL

Payment date: 20160215

Year of fee payment: 10

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

Ref country code: AT

Payment date: 20160215

Year of fee payment: 10

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

Ref country code: BE

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

Effective date: 20150430

REG Reference to a national code

Ref country code: NL

Ref legal event code: MM

Effective date: 20170501

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 646288

Country of ref document: AT

Kind code of ref document: T

Effective date: 20170416

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

Ref country code: NL

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

Effective date: 20170501

Ref country code: AT

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

Effective date: 20170416

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20180706

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

Ref country code: ES

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

Effective date: 20170417