WO2013064340A1 - Composition liquide de nettoyage antimicrobien de surfaces dures - Google Patents

Composition liquide de nettoyage antimicrobien de surfaces dures Download PDF

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Publication number
WO2013064340A1
WO2013064340A1 PCT/EP2012/069945 EP2012069945W WO2013064340A1 WO 2013064340 A1 WO2013064340 A1 WO 2013064340A1 EP 2012069945 W EP2012069945 W EP 2012069945W WO 2013064340 A1 WO2013064340 A1 WO 2013064340A1
Authority
WO
WIPO (PCT)
Prior art keywords
composition
weight
hard surface
antimicrobial
present
Prior art date
Application number
PCT/EP2012/069945
Other languages
English (en)
Inventor
Sameer Keshav Barne
Amit Chakrabortty
Maya Treesa Saji
Original Assignee
Unilever N.V.
Unilever Plc
Hindustan Unilever Limited
Conopco, Inc., D/B/A Unilever
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 Unilever N.V., Unilever Plc, Hindustan Unilever Limited, Conopco, Inc., D/B/A Unilever filed Critical Unilever N.V.
Priority to CN201280054005.1A priority Critical patent/CN103946356B/zh
Priority to PL12772771T priority patent/PL2780438T3/pl
Priority to EP12772771.7A priority patent/EP2780438B1/fr
Priority to EA201400534A priority patent/EA024105B1/ru
Priority to BR112014009455-1A priority patent/BR112014009455B1/pt
Priority to MX2014005412A priority patent/MX348308B/es
Publication of WO2013064340A1 publication Critical patent/WO2013064340A1/fr
Priority to ZA2014/02430A priority patent/ZA201402430B/en

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/38—Cationic compounds
    • C11D1/62—Quaternary ammonium compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2082—Polycarboxylic acids-salts thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2086—Hydroxy carboxylic acids-salts thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/36—Organic compounds containing phosphorus
    • C11D3/362—Phosphates or phosphites

Definitions

  • the invention relates to a liquid hard surface cleaning and disinfection composition.
  • the invention more particularly relates to a hard surface disinfection composition that
  • Liquid compositions for disinfecting and cleaning hard surfaces like floors, walls, windows, doors, furniture, and table tops in various indoor and outdoor locations are known. Toilets and bathrooms are other places where germs proliferate and
  • disinfection and cleaning compositions in liquid form are widely used.
  • Other types of hard surfaces that are cleaned by such compositions include utensils and other articles found in households, offices and other public places.
  • halogen and active oxygen are two most effective bleaches.
  • Bleaches are compounds that liberate oxidising agents like chlorine, bromine, fluorine, nascent oxygen or other oxidizing agents that break the cell walls of microbes like bacteria and virus thereby disinfecting the surfaces thus treated.
  • Phenolics are another class of anti ⁇ microbials often derived from essential oils extracted from natural sources which are formulated in an emulsified form and sold as floor and toilet cleaners.
  • these compounds are sometimes considered either harsh or take a long time for the antimicrobial action to take place.
  • these compositions include surfactants to both emulsify the oily components present therein or to enable cleaning via detergency action. To remove the residual surfactants the surfaces being treated or cleaned are soon thereafter rinsed or wiped to be substantially free of the disinfection/ cleaning composition. This allows very little time for the disinfection action to take place.
  • compositions comprising selected ingredients viz. select salts of dicarboxylic or tricarboxylic acids and sodium tripoly phosphate (STPP) in a benzalkonium chloride (BAC) containing composition provides for synergistic antimicrobial efficacy not provided by each one alone or by any of the binary combinations of these agents, in very short time scales of less than 15 seconds. Further, inclusion of essential oil agents like terpineol and/or thymol provides for further enhanced
  • composition comprising benzalkonium chloride and select salts of dicarboxylic or tricarboxylic acid provides for enhanced antimicrobial efficacy, which action was also not known
  • Liquid hard surface cleaning compositions having a pH of 9 to 12 comprising cationic surfactant like benzalkonium chloride (BAC) are known. It is also known to include alkaline agent like STPP in such compositions.
  • BAC benzalkonium chloride
  • WO09128012 discloses cleaner concentrates, associated cleaners, and associated methods that are capable of removing from surfaces fresh, greasy soils and polymerized soils and include one or more alkalinity sources, one or more chelants, one or more surfactants, and as a remainder, water.
  • GB1395839 Hoechst & Benckiser, 1975 discloses detergent compositions with reduced phosphate content which comprises (a) 2 to 40 parts by wt . of a blend of sodium tripolyphosphate and trisodium citrate in a ratio between 99: 1 and 54: 55 and (b) 1 part by wt . of at least one nonionic surfactant, said
  • composition in 1 percent aqueous solution having a pH of at most 10.
  • US2009176887 discloses a biocidal composition which comprises an effective amount of a biocidal agent such as a quaternary ammonium compound or a blend of quaternary ammonium compounds and an effective amount of a cellular membrane disruptor.
  • a biocidal agent such as a quaternary ammonium compound or a blend of quaternary ammonium compounds
  • a cellular membrane disruptor an effective amount of a cellular membrane disruptor.
  • the synergy index of the biocidal agent and the cellular membrane disruptor is less than 1.
  • Another object of the present invention is to provide a liquid hard surface cleaning and disinfecting composition that has relatively fast antimicrobial action.
  • composition with a pH in the range of 9 to 12 comprising
  • the first aspect of the invention provides for a liquid hard surface antimicrobial cleaning composition with a pH in the range of 9 to 12.
  • the composition comprises 0.5 to 4% by weight of benzalkonium chloride; 0.25 to 3% by weight of salt of di or tri carboxylic acid; 0.25 to 3% by weight sodium
  • tripolyphosphate tripolyphosphate ; and 87 to 97% by weight water.
  • the composition comprises 0.5 to 4%, more preferably 1 to 2%, further more preferably 1.25 to 1.75% cationic surfactant benzalkonium chloride.
  • the composition comprises 0.25 to 3%, preferably 0.5 to 2%, more preferably 0.5 to 1.5% by weight of the composition salt of di or tri carboxylic acid.
  • the salt of di or tri carboxylic acid is preferably chosen from an oxalate, fumarate, phthalate, maleate, malate, malonate or citrate.
  • tricarboxylic acid is most preferably a phthalate, malate, malonate, or citrate.
  • Alkali metal or alkaline earth metal salts are preferred, more preferably alkali metal salts of which sodium salt is most preferred. Structure of salts of some of the carboxylic acids are given below:
  • the composition comprises 0.25 to 3%, preferably 0.5 to 2%, more preferably 1.25 to 1.75% by weight of the composition sodium tripolyphosphate .
  • composition of the invention comprises water as a preferred carrier. Water is present in 87 to 97%, preferably 90 to 95% by weight of the composition.
  • the composition optionally comprises an antimicrobial active selected from an essential oil active.
  • an essential oil active selected from an essential oil active.
  • the essential oil antimicrobial active is present in 0.01 to 2% by weight of the composition.
  • Preferred essential oil actives are thymol, terpineol, eugenol or mixtures thereof. Most preferred essential oil active is a mixture of thymol and terpineol.
  • thymol and terpineol are present in 0.05 to 1%, more preferably 0.08 to 0.3% by weight of the composition.
  • Most useful antimicrobial compositions of the present invention preferably have thymol higher than 0.05 and lesser than 0.3% by weight of the composition.
  • Thymol may be added to the antimicrobial composition in purified form.
  • thyme oil or thyme extract comprising thymol may be added to the antimicrobial composition, while ensuring that thymol is present in the desired concentration in the composition of the present invention.
  • Thyme oil or thyme extract is obtained from the thyme plant.
  • Thyme plant refers to a plant belonging be genus Thymus and includes but is not limited to the following species: Thymus vulgaris, Thymus zygis , Thymus satureoides, Thymus mastichina , Thymus broussonetti , Thymus maroccanus , Thymus pallidus , Thymus algeriensis , Thymus serpyllum, Thymus pulegoide, and Thymus citriodorus .
  • Most of the useful fast acting antimicrobial compositions of the present invention preferably have terpineol higher than 0.05 and lesser than 1% by weight of the composition.
  • the terpineol is preferably selected from alpha-terpineol , beta- terpineol, gamma-terpineol or mixtures thereof. It is
  • terpineol is alpha-terpineol.
  • Terpineol may be added to the antimicrobial composition in purified form.
  • pine oil comprising terpineol may be added to the antimicrobial composition.
  • composition of the invention optionally comprises a
  • surfactant is a non-ionic surfactant.
  • Non-ionic surfactant is preferably present in an amount of 2 to 10% by weight of the composition.
  • Particularly preferred nonionic surfactants are fatty alcohol ethoxylates preferably C8-C22, more preferably C8-C16 fatty alcohol ethoxylates, comprising between 1 and 8 ethylene oxide groups.
  • Suitable surfactant concentrations in liquid forms of hard surface cleaning application are preferably from 1 to 5 % by weight of the composition.
  • composition of the invention has pH in the range of 9 to 12, preferably in the range of 10.5 to 11.5. This could be achieved by incorporating the essential ingredients of the invention in selected amounts, else may be attained by
  • the alkaline agent is a compound having a hydrophilic property and a hydrophilic property.
  • the alkaline agent is preferably present in 0.1 to 1% by weight of the composition.
  • composition of the invention can be achieved in the absence of conventional disinfectants like bleaches e.g. halogens, halogenated
  • bleaches compounds and active oxygen based bleaches.
  • small amount of such bleaches may be present in the composition e.g. less than 1%, preferably less than 0.5%, more preferably less than 0.1% and the efficacy of the composition is achievable even with the bleaches being absent from the composition.
  • composition may further comprise various additional ingredients known to a person skilled in the art.
  • additional ingredients known to a person skilled in the art.
  • additional ingredients include but are not limited to:
  • perfumes perfumes, pigments, preservatives, emollients, sunscreens, emulsifiers, gelling agents, or thickening agents.
  • the antimicrobial composition may be in form of a liquid but the liquid composition may be further thickened to a gel or a paste.
  • the antimicrobial composition of the present invention can be used for cleansing and care of hard surfaces such as glass, metal, plastic, wood, ceramic and the like.
  • a method of cleaning and disinfecting a hard surface comprising applying to said hard surface a composition of the invention diluted with water in a weight ratio of 1: 20 to 1: 200, preferably in a ratio of 1:40 to 1:80.
  • the method preferably comprises a step of rinsing the surface with a suitable solvent preferably water or the surface may be wiped with a suitable wipe.
  • composition of the invention provides an antimicrobial action where the contact time of the antimicrobial actives with the surface is low, i.e. of the order of less than 5 minutes, preferably less than 2 minutes, further more preferably less than a minute and in many cases less than 15 seconds.
  • compositions comprising benzalkonium chloride and a salt of di or tricarboxylic acid for providing antimicrobial benefit.
  • the antimicrobial use is preferably non-therapeutic.
  • the composition for use in antimicrobial activity preferably has benzalkionium chloride at a
  • Antibacterial Compositions for hard surface cleaning as shown in Table - 1 were prepared. The compositions were tested for antibacterial efficacy using the European Suspension Test BS EN1276 which is briefly described below: A test suspension of bacteria (1 ml) was added to a sample of the product under a certain dilution condition (8 ml) along with a specific soil (1 ml) . The mixture was maintained at 20°C for 5 minutes. After this period of contact time, an aliquot is taken and is immediately neutralized by a validated method. The number of bacteria in each sample are determined by plating in TSA agar and the reduction in viable count is calculated after incubating for 48 hours.
  • BS EN1276 European Suspension Test BS EN1276 which is briefly described below: A test suspension of bacteria (1 ml) was added to a sample of the product under a certain dilution condition (8 ml) along with a specific soil (1 ml) . The mixture was maintained at 20°C for 5 minutes. After this period of contact time
  • Table - 1 indicates that the compositions as per the invention (Examples 2 and 3) provides for vastly improved antibacterial efficacy as compared to a composition outside the invention (Example - 1) .
  • Examples 4 to 6 Examples at low contact times
  • compositions of the invention are effective even at short contact times of about 30 seconds.
  • compositions similar to Examples 1 to 3 were prepared and tested against various other types of bacteria as shown in
  • BSA Serum Albumin
  • Examples 10 to 15 are vastly superior to sampl outside the invention (Examples 7 to 9) in terms of
  • compositions of the invention additionally comprising essential oil actives Compositions as shown in Table - 4 were tested for
  • Examples 17 to 21 give vastly superior antibacterial efficacy as compared to a sample outside the invention (Example 16) .
  • Table - 5 Various compositions as shown in Table - 5 were prepared and the antimicrobial efficacy was measured using the procedure used for Example -1 (except that in the present case, the dilution used was 1:60) . The data on the log reduction of bacteria is shown in Table - 5. Table - 5
  • the invention thus provides for a composition for hard surface disinfection that interact synergistically to enable

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Detergent Compositions (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

La présente invention porte sur une composition liquide de nettoyage et désinfection de surfaces dures qui assure un effet antimicrobien relativement rapide. La composition est une composition aqueuse ayant un pH dans la plage de 9 à 12 comprenant des quantités choisies de chlorure de benzalkonium ; un sel d'acide dicarboxylique ou tricarboxylique ; et du tripolyphosphate de sodium.
PCT/EP2012/069945 2011-11-03 2012-10-09 Composition liquide de nettoyage antimicrobien de surfaces dures WO2013064340A1 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
CN201280054005.1A CN103946356B (zh) 2011-11-03 2012-10-09 液体硬表面抗微生物清洁组合物
PL12772771T PL2780438T3 (pl) 2011-11-03 2012-10-09 Ciekłe przeciwmikrobowe kompozycje czyszczące do twardych powierzchni
EP12772771.7A EP2780438B1 (fr) 2011-11-03 2012-10-09 Composition liquide de nettoyage antimicrobien de surface dure
EA201400534A EA024105B1 (ru) 2011-11-03 2012-10-09 Жидкая противомикробная композиция для очищения твердой поверхности
BR112014009455-1A BR112014009455B1 (pt) 2011-11-03 2012-10-09 composição líquida de limpeza antimicrobiana de superfície dura e método de limpeza e desinfecção de uma superfície dura
MX2014005412A MX348308B (es) 2011-11-03 2012-10-09 Una composicion limpiadora antimicrobiana liquida de superficie dura.
ZA2014/02430A ZA201402430B (en) 2011-11-03 2014-04-02 A liquid hard surface antimicrobial cleaning composition

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
IN3093MU2011 2011-11-03
IN3093/MUM/2011 2011-11-03
EP12150935 2012-01-12
EP12150935.0 2012-01-12

Publications (1)

Publication Number Publication Date
WO2013064340A1 true WO2013064340A1 (fr) 2013-05-10

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ID=47019009

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2012/069945 WO2013064340A1 (fr) 2011-11-03 2012-10-09 Composition liquide de nettoyage antimicrobien de surfaces dures

Country Status (8)

Country Link
EP (1) EP2780438B1 (fr)
CN (1) CN103946356B (fr)
BR (1) BR112014009455B1 (fr)
EA (1) EA024105B1 (fr)
MX (1) MX348308B (fr)
PL (1) PL2780438T3 (fr)
WO (1) WO2013064340A1 (fr)
ZA (1) ZA201402430B (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102016202846A1 (de) 2016-02-24 2017-08-24 Henkel Ag & Co. Kgaa Wasch- oder Reinigungsmittel mit verbesserter antimikrobieller Wirkung
WO2017159022A1 (fr) * 2016-03-16 2017-09-21 株式会社日立ハイテクノロジーズ Système de transport d'échantillon
US10329522B2 (en) 2016-05-19 2019-06-25 Ecolab Usa Inc. Cleaning compositions for use with calcite-based stone

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AR126534A1 (es) 2021-08-04 2023-10-18 Unilever Global Ip Ltd Una composición blanqueadora estable
AR126535A1 (es) 2021-08-04 2023-10-18 Unilever Global Ip Ltd Una composición blanqueadora antimicrobiana

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1395839A (en) 1972-06-22 1975-05-29 Hoechst Ag Basic formulation for detergents and cleansing agents
WO1998024314A1 (fr) * 1996-12-06 1998-06-11 Reckitt & Colman Inc. Composition aqueuse de nettoyage et de desinfection
US6066674A (en) * 1993-08-19 2000-05-23 Kao Corporation Germicidal-disinfectant detergent composition
US6277805B1 (en) * 1993-11-22 2001-08-21 The Procter & Gamble Co. Alkaline liquid hard-surface cleaning composition containing a quaternary ammonium disinfectant and selected dicarboxylate sequestrants
US6624126B1 (en) * 1999-11-04 2003-09-23 Kao Corporation Personal cleansing composition comprising a glyceryl ether
US20050119153A1 (en) * 2001-12-20 2005-06-02 Burt Diane J. Water soluble container containing dry actives
US20050256021A1 (en) * 2002-08-22 2005-11-17 Reckitt Benckiser Inc. Multi-phase liquid hard surface cleaning and/or disinfecting compositions
US20090176887A1 (en) 2006-08-04 2009-07-09 Victor Vlasaty Biocidal Compositions and Methods
WO2009128012A2 (fr) 2008-04-18 2009-10-22 Ecolab Inc. Concentrés de nettoyant, nettoyants associés et procédés associés

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9704989D0 (en) * 1997-03-11 1997-04-30 Unilever Plc Improvements relating to hard-surface cleaning compositions

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1395839A (en) 1972-06-22 1975-05-29 Hoechst Ag Basic formulation for detergents and cleansing agents
US6066674A (en) * 1993-08-19 2000-05-23 Kao Corporation Germicidal-disinfectant detergent composition
US6277805B1 (en) * 1993-11-22 2001-08-21 The Procter & Gamble Co. Alkaline liquid hard-surface cleaning composition containing a quaternary ammonium disinfectant and selected dicarboxylate sequestrants
WO1998024314A1 (fr) * 1996-12-06 1998-06-11 Reckitt & Colman Inc. Composition aqueuse de nettoyage et de desinfection
US6624126B1 (en) * 1999-11-04 2003-09-23 Kao Corporation Personal cleansing composition comprising a glyceryl ether
US20050119153A1 (en) * 2001-12-20 2005-06-02 Burt Diane J. Water soluble container containing dry actives
US20050256021A1 (en) * 2002-08-22 2005-11-17 Reckitt Benckiser Inc. Multi-phase liquid hard surface cleaning and/or disinfecting compositions
US20090176887A1 (en) 2006-08-04 2009-07-09 Victor Vlasaty Biocidal Compositions and Methods
WO2009128012A2 (fr) 2008-04-18 2009-10-22 Ecolab Inc. Concentrés de nettoyant, nettoyants associés et procédés associés

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102016202846A1 (de) 2016-02-24 2017-08-24 Henkel Ag & Co. Kgaa Wasch- oder Reinigungsmittel mit verbesserter antimikrobieller Wirkung
WO2017144420A1 (fr) 2016-02-24 2017-08-31 Henkel Ag & Co. Kgaa Produit détergent ou de nettoyage à action antimicrobienne améliorée
US10487291B2 (en) 2016-02-24 2019-11-26 Henkel Ag & Co. Kgaa Detergent or cleaning agent having GLDA-enhanced antimicrobial effect
WO2017159022A1 (fr) * 2016-03-16 2017-09-21 株式会社日立ハイテクノロジーズ Système de transport d'échantillon
US10329522B2 (en) 2016-05-19 2019-06-25 Ecolab Usa Inc. Cleaning compositions for use with calcite-based stone

Also Published As

Publication number Publication date
MX348308B (es) 2017-06-06
BR112014009455B1 (pt) 2021-01-12
BR112014009455A2 (pt) 2017-04-18
EP2780438A1 (fr) 2014-09-24
EA201400534A1 (ru) 2014-09-30
MX2014005412A (es) 2014-07-11
CN103946356B (zh) 2017-02-15
PL2780438T3 (pl) 2016-06-30
EP2780438B1 (fr) 2015-12-30
EA024105B1 (ru) 2016-08-31
ZA201402430B (en) 2016-01-27
CN103946356A (zh) 2014-07-23

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