WO2018113645A1 - Composition de détergent pour le linge - Google Patents

Composition de détergent pour le linge Download PDF

Info

Publication number
WO2018113645A1
WO2018113645A1 PCT/CN2017/117074 CN2017117074W WO2018113645A1 WO 2018113645 A1 WO2018113645 A1 WO 2018113645A1 CN 2017117074 W CN2017117074 W CN 2017117074W WO 2018113645 A1 WO2018113645 A1 WO 2018113645A1
Authority
WO
WIPO (PCT)
Prior art keywords
perfume
process according
detersive surfactant
particle
detersive
Prior art date
Application number
PCT/CN2017/117074
Other languages
English (en)
Inventor
Alan Thomas Brooker
Neil Joseph Lant
Nigel Patrick Somerville Roberts
Gang SI
Phillip Jan Howard
Pu Zhao
Original Assignee
The Procter & Gamble Company
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
Priority claimed from EP17173004.7A external-priority patent/EP3339416A1/fr
Priority claimed from EP17173007.0A external-priority patent/EP3339419A1/fr
Priority claimed from EP17172999.9A external-priority patent/EP3339413A1/fr
Priority claimed from EP17173001.3A external-priority patent/EP3339407A1/fr
Priority claimed from EP17173000.5A external-priority patent/EP3339414A1/fr
Priority claimed from EP17173005.4A external-priority patent/EP3339417A1/fr
Priority claimed from EP17173006.2A external-priority patent/EP3339418A1/fr
Priority claimed from EP17173002.1A external-priority patent/EP3339415A1/fr
Application filed by The Procter & Gamble Company filed Critical The Procter & Gamble Company
Priority to EP17883274.7A priority Critical patent/EP3559194A4/fr
Publication of WO2018113645A1 publication Critical patent/WO2018113645A1/fr

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
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/10—Carbonates ; Bicarbonates
    • 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
    • C11D1/66—Non-ionic compounds
    • C11D1/83—Mixtures of non-ionic with anionic 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
    • 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
    • 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
    • C11D3/50—Perfumes
    • C11D3/502—Protected perfumes
    • C11D3/505—Protected perfumes encapsulated or adsorbed on a carrier, e.g. zeolite or clay

Definitions

  • the present invention relates to a process for making a laundry detergent composition having a lenticular size and shape.
  • the lenticular laundry detergent compositions made by the process of the present invention exhibit good freshness performance.
  • compositions that are in the form of lenticles.
  • These solid particles are of a shape and size that exhibit difference product performance characteristics compared to the conventional particulate detergent products.
  • the cleaning and freshness performance have very different characteristics, especially in stressed laundering conditions such as cold and quick wash cycles.
  • the present invention seeks to provide a process of making a lenticular laundry detergent product, the product having a good perfume compatibility and improved freshness profie, especially in cold and quick cycles.
  • the composition of the present invention exhibits a good perfume profile.
  • the present invention provides a process for the preparation of a coated detergent particle having perpendicular dimensions x, y and z, wherein x is from 1 to 2 mm, y is from 2 to 8mm, and z is from 2 to 8 mm, wherein the process comprises the following steps:
  • step (ii) extruding the detersive mixture of step (i) to form an extruded material
  • the process comprises the following steps:
  • step (ii) extruding the detersive mixture of step (i) to form an extruded material
  • Step (i) A detersive mixture comprising from 40wt%to 90wt%detersive surfactant and from 0.5wt%to 20wt%perfume micro-particles is formed.
  • the detersive surfactant comprises from 15wt%to 85wt%anionic detersive surfactant and from 5wt%to 75wt%non-ionic detersive surfactant.
  • the anionic detersive surfactant is selected from alkyl benzene sulphonate, alkyl ether sulphate and/or alkyl sulphate.
  • the detersive mixture has a hardness of from 1MPa to 100MPa during the roller compaction step (ii) .
  • a suitable detersive mixture comprises 85wt%detersive surfactant, 3wt %perfume oil, and 12wt%of zeolite-loaded-perfume (20wt%perfume activity) .
  • a suitable detersive surfactant comprises from 80wt%to 95wt%alkyl benzene sulphonate, and from 6wt%to 10wt%alkyl ethoxylated alcohol having an average degree of ethoxylation of from 5 to 9.
  • Such a detersive surfactant can be prepared by blending the nonionic detersive surfactant into HLAS and rapidly neutralizing the mix with aqueous caustic solution followed by drying in an oven, preferably a vacuum oven until the eRH of the surfactant is less than 10%. This surfactant can then be milled in any suitable device, such as a coffee grinder or mill.
  • a suitable detersive surfactant comprises at least 51wt%alkyl benzenesulphonate.
  • a suitable detersive surfactant comprises no more than 20wt%non-ionic detersive surfactant.
  • the detersive surfactant is dried prior to step (ii) .
  • a suitable drying means include an evaporator or drier.
  • a suitable drying means include a wiped film evaporator, fluid bed drier and/or a tube drier.
  • the detersive mixture introduced into step (ii) comprises less than 1.5 wt%water.
  • the detersive mixture is cooled prior to step (ii) .
  • a suitable cooling means inclues a chill roll.
  • the detersive surfactant may be transferred to a mill and milled to particles of less than 1.5 mm, preferably less than 1 mm, before it is fed to the extrusion step (ii) .
  • a powdered flow aid with a particle diameter of from 0.1 ⁇ m to 10 ⁇ m is added to the mill in an amount of 0.5wt%to 5 wt% (wt%based on the detersive misture) , and blended into the surfactant particles during milling.
  • Step (ii) The detersive mixture of step (i) is extruded to form an extruded material.
  • the extruder has a void commensurate with the size of the particle before coating.
  • the detersive mixture is fed into a twin-screw co-rotating extruder equipped with a die-plate and cutting mechanism.
  • the extruder is typically cooled during operation.
  • a suitable extruder is an APV 24.
  • Another suitable extruder includes a roller compactor.
  • Extrusion rates of from 2 to 8 kg/hr are suitable, and a die-plate with orifices of from 3 to 7 mm can be used.
  • the die-plate can be equipped with a rotary cutter so as to give an extrudate thickness of from 1mm to 2mm.
  • the temperature of the detersive mixture does not exceed 45°C, and preferably does not exceed 40°C, during the extrusion step (ii) .
  • the extruded material produced by step (ii) is an oblate spheroid.
  • the diameter of the extruded material produced by step (ii) is greater than 4mm
  • Step (iii) The extruded material of step (ii) is coated with water-soluble inorganic salt in the form of an aqueous solution to form a wet coated extruded material comprising from 1wt%to 40wt%water soluble inorganic salt.
  • the coating material is selected from powdered inorganic material and mixtures of such material and nonionic material with a melting point in the range 40°C to 90°C.
  • Step (iv) Water is removed from the wet coated extruded material to form the coated detergent particle.
  • step (iv) is carried out in a fluidized bed and/or a drum.
  • the coated detergent particle comprises from 1wt%to 5wt%water.
  • the coated detergent particle is curved.
  • Perfume micro-particle A suitable perfume micro-particle is selected from perfume-loaded-zeolite, perfume micro-particle is a perfume-loaded silica, or a combination thereof. A preferred perfume micro-particle is perfume-loaded-zeolite.
  • perfumes into the core of coated detergent particle in the form of perfume-containing micro-particles.
  • These particles can be zeolites or silica particles or other perfume micro-particle. Adding high levels of perfume oils into the particle core can result in sticky or soft cores which will cause processing issues especially during cutting. Pre-loading the perfume oils into micro-particles can allow higher levels of perfume oils to be added without issue.
  • Perfume can be loaded into zeolite as follows. Typically wide pore zeolites such as Zeolite 13X are preferred due to their ability to load perfume oils. The zeolite is typically dried by exposure to temperatures greater than 100°C. The anhydrous zeolite is placed into a mixer such as a paddle mixer or ploughshare mixer and the perfume oil gradually poured in with continuous mixing. The absorption of the perfume is very exothermic and the perfume loaded zeolite should be cooled prior to further use.
  • a mixer such as a paddle mixer or ploughshare mixer
  • Perfume can also be loaded into silica, such as Sipernat 22 or 22S.
  • the perfume is encapsulated into starch such or plastic materials such as melamine formaldehyde.
  • zeolites, silicas and amorphous aluminosilicates are preferred.
  • Perfume levels can be between 10wt%and 40wt%depending on the substrate used.
  • the coated detergent particle typically comprises:
  • the coated detergent particle is also referred to herein as the composition.
  • the composition has a pH in the range of from 7.6 to 10.0.
  • the composition has a reserve alkalinity to pH 7.5 of greater than 3.0.
  • the composition is in the form of a coated laundry detergent particle that is curved.
  • the coating comprises the inorganic salt (b) , and wherein the core comprises the detersive surfactant (a) .
  • x 2mm
  • y >2mm
  • y >3mm
  • the dimensions x, y and z can be measured using image analysis.
  • Suitable equipment for image analysis includes a Leica Binocular Microscope (Leica MZ16A) with motorised and indexed mount, using a digital camera (Leica IC30) to capture the images, the images would be processed within the LEICA Application Software (LAS) platform using the optional Montage MultiFocus and Analysis modules.
  • LAS LEICA Application Software
  • the X and y axial size can be determined by pixel count analysis of the Feret diameters with the maximum and minimum Feret Diameters representing the X and Y axial lengths.
  • the Z axial length can be determined via the use of focus stacking (i.e. z-stacked images) which is a digital image processing technique which combines multiple images taken at different known focus distances to give a resulting image with a greater depth of field (DOF) than any of the individual source images.
  • focus stacking i.e. z-stacked images
  • DOE depth of field
  • the coated laundry detergent particle may be shaped as a disc.
  • the coated laundry detergent particle does not have hole; that is to say, the coated laundry detergent particle does not have a conduit that passes through the core: i.e. the coated detergent particle has a topologic genus of zero.
  • composition may comprise from 0.05wt%to 4.0wt%soil release polymer.
  • the composition may comprise from 0.1wt%to 3.0wt%carboxymethylcellulose (CMC) .
  • composition may comprise from 0.1wt%to 5.0wt%calcite.
  • the composition may comprise from 1wt%to 10wt%carboxylate polymer.
  • the composition may comprise less than 10wt%total level of silicates and aluminosilicates.
  • composition may comprise from 0.001wt%to 0.5wt% hueing dye.
  • composition may comprise from 0.001wt%to 0.5wt%organic pigment and/or inorganic pigment.
  • composition may comprise from 0.2 wt%to 10wt%chelant, preferably phosphonate chelant.
  • composition preferably comprises from 10wt%to 40wt%sodium carbonate.
  • a suitable detersive surfactant system typically comprises at least 5%alcohol ether carboxylate as a percentage of the total detersive surfactant system.
  • a suitable detersive surfactant system typically comprises at least 5%alcohol ethoxylate having an average degree of ethoxylation in the range of from 10 to 50 as a percentage of the total detersive surfactant system.
  • the detersive surfactant comprises C 8 -C 24 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 20 to 50, and preferably the compositon comprises from 1wt%to 10wt%C 8 -C 24 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 20 to 50.
  • a suitable highly ethoxylated alcohol is AO30 from BASF and/or 2430 from Sasol.
  • Anionic detersive surfactant Suitable anionic detersive surfactants include sulphonate and sulphate detersive surfactants.
  • Suitable sulphonate detersive surfactants include methyl ester sulphonates, alpha olefin sulphonates, alkyl benzene sulphonates, especially alkyl benzene sulphonates, preferably C 10-13 alkyl benzene sulphonate.
  • Suitable alkyl benzene sulphonate (LAS) is obtainable, preferably obtained, by sulphonating commercially available linear alkyl benzene (LAB) ; suitable LAB includes low 2-phenyl LAB, other suitable LAB include high 2-phenyl LAB, such as those supplied by Sasol under the tradename
  • Suitable sulphate detersive surfactants include alkyl sulphate, preferably C 8-18 alkyl sulphate, or predominantly C 12 alkyl sulphate.
  • a preferred sulphate detersive surfactant is alkyl alkoxylated sulphate, preferably alkyl ethoxylated sulphate, preferably a C 8-18 alkyl alkoxylated sulphate, preferably a C 8-18 alkyl ethoxylated sulphate, preferably the alkyl alkoxylated sulphate has an average degree of alkoxylation of from 0.5 to 20, preferably from 0.5 to 10, preferably the alkyl alkoxylated sulphate is a C 8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 10, preferably from 0.5 to 5, more preferably from 0.5 to 3 and most preferably from 0.5 to 1.5.
  • alkyl sulphate, alkyl alkoxylated sulphate and alkyl benzene sulphonates may be linear or branched, substituted or un-substituted, and may be derived from petrochemical material or biomaterial.
  • anionic detersive surfactants include alkyl ether carboxylates.
  • Suitable anionic detersive surfactants may be in salt form, suitable counter-ions include sodium, calcium, magnesium, amino alcohols, and any combination thereof.
  • suitable counter-ions include sodium, calcium, magnesium, amino alcohols, and any combination thereof.
  • a preferred counter-ion is sodium.
  • Alkyl ether carboxylic acid A suitable alkyl ether carboxylic acid has the following structure:
  • R is selected from saturated and mono-unsaturated C 10 to C 26 linear or branched alkyl chains, preferably C 12 to C 24 linear or branched alkyl chains, most preferably a C 16 to C 20 linear alkyl chain;
  • n is selected from 5 to 20, preferably 7 to 13, more preferably 8 to 12, most preferably 9.5 to 10.5;
  • the alkyl ether carboxylic acid may be present from 0.5 to 20 wt%, preferably from 2 to 14 wt%, most preferably from 2.5 to 5 wt%. It may be present in acid or salt form, most preferably as its sodium salt.
  • Suitable materials are sold under the (Kao) and C (Huntsman) brand names.
  • Non-ionic detersive surfactant Suitable non-ionic detersive surfactants are selected from the group consisting of: C 8 -C 18 alkyl ethoxylates, such as, non-ionic surfactants from Shell; C 6 -C 12 alkyl phenol alkoxylates wherein preferably the alkoxylate units are ethyleneoxy units, propyleneoxy units or a mixture thereof; C 12 -C 18 alcohol and C 6 -C 12 alkyl phenol condensates with ethylene oxide/propylene oxide block polymers such as from BASF; alkylpolysaccharides, preferably alkylpolyglycosides; methyl ester ethoxylates; polyhydroxy fatty acid amides; ether capped poly (oxyalkylated) alcohol surfactants; and mixtures thereof.
  • C 8 -C 18 alkyl ethoxylates such as, non-ionic surfactants from Shell
  • Suitable non-ionic detersive surfactants are alkylpolyglucoside and/or an alkyl alkoxylated alcohol.
  • Suitable non-ionic detersive surfactants include alkyl alkoxylated alcohols, preferably C 8-18 alkyl alkoxylated alcohol, preferably a C 8-18 alkyl ethoxylated alcohol, preferably the alkyl alkoxylated alcohol has an average degree of alkoxylation of from 1 to 50, preferably from 1 to 30, or from 1 to 20, or from 1 to 10, preferably the alkyl alkoxylated alcohol is a C 8-18 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 1 to 10, preferably from 1 to 7, more preferably from 1 to 5 and most preferably from 3 to 7.
  • the alkyl alkoxylated alcohol can be linear or branched, and substituted or un-substituted.
  • Suitable nonionic detersive surfactants include secondary alcohol-based detersive surfactants.
  • Amino acid derivative complexing agent is selected from one or more of the following, in any stereoisomer or mixture of stereoisomer form:
  • the composition comprises from 0.1wt%to 10wt%methylglycinediacetic acid and salts thereof (MGDA)
  • amino acid derivative complexing agent it may be preferred to formulate the amino acid derivative complexing agent in acid form.
  • amino acid derivative complexing agent in salt form, especially preferred is the sodium salt form.
  • Suitable MGDA salts are produced by BASF.
  • Suitable GLDA salts are produced by Akzo Nobel and Showa Denko.
  • Suitable ASDA salts are produced by Mitsubishi Rayon.
  • Alkoxylated polyaryl/polyalkyl phenol A suitable alkoxylated polyaryl/polyalkyl phenol has the following structure:
  • R 1 is selected from linear of branched C 3 -C 15 alkyl groups and aryl groups, X is selected from ethoxy or propoxy groups, n is from 2 to 70, T is selected from H, SO 3 - , COO - and PO 3 2-
  • the alkoxylated polyaryl or alkoxylated polyalkyl phenol is preferably selected from groups (i) to (iv) :
  • R is selected from SO 3 - , COO - and PO 3 2- , preferably selected from SO 3 - and COO - , wherein n is selected from 2 to 54.
  • n is selected from 2 to 50
  • R is selected from SO 3 - , COO - and PO 3 2- , preferably selected from SO 3 - and COO - , wherein n is selected from 6 to 50.
  • Such compounds are available from industrial suppliers, for example Solvay under the Soprophor trade name, from Clariant under the Emulsogen trade name, Aoki Oil Industrial Co. under the Blaunon trade name, from Stepan under the Makon trade name, and from TOTO Chemical Industry Co. under the Sorpol trade name.
  • suitable compounds are TS160, BV conc., T110 or T139, all from Clariant.
  • the alkoxylated polyaryl/polyalkyl phenol may be present at levels of 0.5-20wt%, preferably 1-15wt%, most preferably 3-10wt%.
  • Amylase variant comprises:
  • R118P Q; V; F; C; G; A; C; D; E; H; I; K; L; M; N; S; T; Y, particularly R118P; Q; V; F; C; G,
  • E190P R; V; F; C; G; A; C; D; Q; H; I; K; L; M; N; S; T; Y, particularly E190P,
  • V213Q P; R; F; C; G; A; C; D; E; H; I; K; L; M; N; S; T; Y, particularly V213T; A; G; S; C; L; P,
  • V214Q P; R; F; C; G; A; C; D; E; H; I; K; L; M; N; S; T; Y, particularly V214T; I,
  • T246Q P; R; F; C; G; A; C; D; E; H; I; K; L; M; N; Y; S; V, particularly T246Q; M,
  • amylase variant has at least 95%, such as at least 96%, or at least 97%, or at least 98%, or at least 99%but less than 100%sequence identity to the polypeptide having the amino acid sequence of SEQ ID NO: 1 and wherein the variant has alpha-amylase activity.
  • One preferred amylase variant comprises a sequence corresponding to SEQ ID NO: 1 with the following mutations: H183*+G184*+I405L+A421H+A422P+A428T.
  • a suitable amylase is commercially available from Novozymes under the brand name, for example as a liquid raw material as 12L.
  • a suitable lipase is a variant of SEQ ID NO: 2 comprising:
  • the positions correspond to the positions of SEQ ID NO 2 and wherein the lipase variant has at least 95%but less than 100%sequence identity to the polypeptide having the amino acid sequence of SEQ ID NO: 2 and wherein the variant has lipase activity.
  • One preferred lipase is a variant of SEQ ID NO: 2 comprising the following substitutions: T231R, N233R, D27R, G38A, D96E, D111A, G163K, D254S and P256T
  • One preferred lipase is a variant of SEQ ID NO: 2 comprising the following substitutions: T231R, N233R, N33Q, G91Q, E210Q, I255A.
  • Suitable lipases are commercially available from Novozymes, for example as Lipex Evity 100L (a liquid raw material) and Lipex Evity 105T (a granulate) . These lipases have different structures to the products Lipex 100L, Lipex 100T and Lipex Evity 100T which are outside the scope of this particular lipase definition.
  • Metalloproteases can be derived from animals, plants, bacteria or fungi. Suitable metalloprotease can be selected from the group of neutral metalloproteases and Myxobacter metalloproteases. Suitable metalloproteases can include collagenases, hemorrhagic toxins from snake venoms and thermolysin from bacteria.
  • thermolysin enzyme variants include an M4 peptidase, more preferably the thermolysin enzyme variant is a member of the PepSY ⁇ Peptidase_M4 ⁇ Peptidase_M4_C family.
  • thermolysin enzyme variant can have at least 50%identity to the thermolysin set forth in SEQ ID NO: 3.
  • the thermolysin enzyme variant is from a genus selected from the group consisting of Bacillus, Geobacillus, Alicyclobacillus, Lactobacillus, Exiguobacterium, Brevibacillus, Paenibacillus, Herpetosiphon, Oceanobacillus, Shewanella, Clostridium, Staphylococcus, Flavobacterium, Stigmatella, Myxococcus, Vibrio, Methanosarcina, Chryseobacterium, Streptomyces, Kribbella, Janibacter, Nocardioides, Xanthamonas, Micromonospora, Burkholderia, Dehalococcoides, Croceibacter, Kordia, Microscilla, Thermoactinomyces, Chloroflexus, Listeria, Plesiocystis, Hal
  • thermolysin enzyme variant is from a genus selected from the group consisting of Bacillus, Geobacillus, Alicyclobacillus, Lactobacillus, Exiguobacterium, Brevibacillus, Paenibacillus, Herpetosiphon, Oceanobacillus, Shewanella, Clostridium, Staphylococcus, Flavobacterium, Stigmatella, Myxococcus, Vibrio, Methanosarcina, Chryseobacterium, and Pseudoalteromonas.
  • thermolysin enzyme is from the genus Bacillus.
  • Preferred metalloproteases include thermolysin, matrix metalloproteinases and those metalloproteases derived from Bacillus subtilis, Bacillus thermoproteolyticus, Geobacillus stearothermophilus or Geobacillus sp., or Bacillus amyloliquefaciens, as described in US PA 2008/0293610A1.
  • a specially preferred metalloprotease belongs to the family EC3.4.24.27.
  • thermolysin variants described in WO2014/71410.
  • the metalloprotease is a variant of a parent protease, said parent protease having at least 60%, or 80%, or 85%or 90%or 95%or 96%or 97%or 98%or 99%or even 100%identity to SEQ ID NO: 3 including those with substitutions at one or more of the following sets of positions versus SEQ ID NO: 3:
  • the metalloprotease protease is a variant of a parent protease, said parent protease having at least 60%, or 80%, or 85%or 90%or 95%or 96%or 97%or 98%or 99%or even 100%identity to SEQ ID NO: 3 including those with substitutions at one or more of the following sets of positions versus SEQ ID NO: 3:
  • metalloproteases are the NprE variants described in WO2007/044993, WO2009/058661 and US 2014/0315775.
  • the protease is a variant of a parent protease, said parent protease having at least 45%, or 60%, or 80%, or 85%or 90%or 95%or 96%or 97%or 98%or 99%or even 100%identity to SEQ ID NO: 4 including those with substitutions at one or more of the following sets of positions versus SEQ ID NO: 4:
  • Another suitable metalloprotease is a variant of a parent protease, said parent protease having at least 60%, or 80%, or 85%or 90%or 95%or 96%or 97%or 98%or 99%or even 100%identity to SEQ ID NO: 4 including those with substitutions at one or more of the following sets of positions versus SEQ ID NO: 4:
  • M138L/V190I/D220P S129I/V190I, S129V/V190I, S129V/D220P, S129I/F130L/D220P,
  • T004V/S023N T059K/S66Q/S129I, T059R/S66N/S129I, S129I/F130L/M138L/V190I/D220P and T059K/S66Q/S129V.
  • Especially preferred metalloproteases for use herein belong belong to EC classes EC 3.4.22 or EC3.4.24, more preferably they belong to EC classes EC3.4.22.2, EC3.4.24.28 or EC3.4.24.27.
  • the most preferred metalloprotease for use herein belong to EC3.4.24.27.
  • Suitable commercially available metalloprotease enzymes include those sold under the trade names by Novozymes A/S (Denmark) , the range including 2TS, N, L10, LAP and 7089 from AB Enzymes, Protex 14L and Protex 15L from DuPont (Palo Alto, California) , those sold as thermolysin from Sigma and the Thermoase range (PC10F and C100) and thermolysin enzyme from Amano enzymes.
  • a preferred metalloprotease is selected from the M4 Metalloprotease Family.
  • a suitable water-soluble builder system comprising one or more aminocarboxylates, selected from: methylglycine diacetic acid (MGDA) and/or alkali metal or ammonium salts thereof; N, N-dicarboxymethyl glutamic acid (GLDA) and/or alkali metal or ammonium salts thereof; Aspartic acid N, N-diacetic acid (ASDA) and/or alkali metal or ammonium salts thereof; Ethylene diamine-N, N'-disuccunic acid (EDDS) and/or alkali metal or ammonium salt thereof; 2-hydroxy propylene diamine-N, N'-disuccunic acid (HPDDS) , and/or alkali metal or ammonium salt thereof; ethylenediamine-N, N'-diglutaric acid (EDDG and/or alkali metal or ammonium salt thereof; ethylenediamine-N, N'-bis- (orthohydroxyphenyl) acetic acid (EDDG) and
  • a suitable phosphonate chelant is selected from: 1-hydroxyethane-1, 1-diphosphonic acid (HEDP) ; Diethylene triamine pentamethylene phosphonic acid (DTPMP, CW-Base) ; 2-phosphonobutane-1, 2, 4-tricarboxylic acid (PBTC) ; Amino trimethylene phosphonic acid (ATMP) ; Ethylenediamine tetramethylene phosphonic acid (EDTMP) ; Diethylenetriamine pentamethylene phosphonic acid (DTPMP) ; Aminotrimethylene phosphonic acid (ATMP) ; salts of the aforementioned materials; and any combination thereof.
  • HEDP 1-hydroxyethane-1, 1-diphosphonic acid
  • DTPMP Diethylene triamine pentamethylene phosphonic acid
  • CW-Base 2-phosphonobutane-1, 2, 4-tricarboxylic acid
  • PBTC 2-phosphonobutane-1, 2, 4-tricarboxylic acid
  • ATMP Amin
  • Carboxylate polymer The composition may comprise a carboxylate polymer, such as a maleate/acrylate random copolymer, maleic-olefin copolymers or polyacrylate homopolymer.
  • Suitable carboxylate polymers include: polyacrylate homopolymers having a molecular weight of from 4,000 Da to 9,000 Da; maleate/acrylate random copolymers having a molecular weight of from 50,000 Da to 100,000 Da, or from 60,000 Da to 80,000 Da.
  • the Acusol series are available from Rohm &Haas, Philadelphia, PA and the Sokolan series are available from BASF (Germany and New Jersey) .
  • Suitable carboxylate polymers can contain other monomers including modified acrylic, fumaric, maleic, itaconic, aconitic, mesaconic, citraconic and methylenemalonic acid or their salts, modified maleic anhydride, acrylamide, alkylene, vinylmethyl ether, styrene and any mixtures thereof.
  • Suitable carboxylate polymers can also containing 2-acrylamido-2-methyl-l-propanesulfonic acid, 2-methacrylamido-2-methyl-1-propanesulfonic acid, 3-methacrylamido-2-hydroxy-propanesulfonic acid, allysulfonic acid, methallysulfonic acid, 2-hydroxy-3- (2-propenyloxy) propanesulfonic acid, 2-methyl-2-propenen-l-sulfonic acid, styrenesulfonic acid, vinylsulfonic acid, 3-sulfopropyl acrylate, 3-sulfopropylmethacrylate, sulfomethylacrylamide, sulfomethylmethacrylamide and water soluble salts thereof.
  • Another suitable carboxylate polymer is a co-polymer that comprises: (i) from 50 to less than 98 wt%structural units derived from one or more monomers comprising carboxyl groups; (ii) from 1 to less than 49 wt%structural units derived from one or more monomers comprising sulfonate moieties; and (iii) from 1 to 49 wt%structural units derived from one or more types of monomers selected from ether bond-containing monomers represented by formulas (I) and (II) :
  • R 0 represents a hydrogen atom or CH 3 group
  • R represents a CH 2 group, CH 2 CH 2 group or single bond
  • X represents a number 0-5 provided X represents a number 1-5 when R is a single bond
  • R 1 is a hydrogen atom or C 1 to C 20 organic group
  • R 0 represents a hydrogen atom or CH 3 group
  • R represents a CH 2 group, CH 2 CH 2 group or single bond
  • X represents a number 0-5
  • R 1 is a hydrogen atom or C 1 to C 20 organic group.
  • the polymer has a weight average molecular weight of at least 50kDa, or even at least 70kDa.
  • Soil release polymer The composition may comprise a soil release polymer.
  • a suitable soil release polymer has a structure as defined by one of the following structures (I) , (II) or (III) :
  • a, b and c are from 1 to 200;
  • d, e and f are from 1 to 50;
  • Ar is a 1, 4-substituted phenylene
  • sAr is 1, 3-substituted phenylene substituted in position 5 with SO 3 Me;
  • Me is Li, K, Mg/2, Ca/2, Al/3, ammonium, mono-, di-, tri-, or tetraalkylammonium wherein the alkyl groups are C 1 -C 18 alkyl or C 2 -C 10 hydroxyalkyl, or mixtures thereof;
  • R 1 , R 2 , R 3 , R 4 , R 5 and R 6 are independently selected from H or C 1 -C 18 n-or iso-alkyl;
  • R 7 is a linear or branched C 1 -C 18 alkyl, or a linear or branched C 2 -C 30 alkenyl, or a cycloalkyl group with 5 to 9 carbon atoms, or a C 8 -C 30 aryl group, or a C 6 -C 30 arylalkyl group.
  • Suitable soil release polymers are sold by Clariant under the series of polymers, e.g. SRN240 and SRA300.
  • Other suitable soil release polymers are sold by Solvay under the series of polymers, e.g. SF2 and Crystal.
  • Anti-redeposition polymer Suitable anti-redeposition polymers include polyethylene glycol polymers and/or polyethyleneimine polymers.
  • Suitable polyethylene glycol polymers include random graft co-polymers comprising: (i) hydrophilic backbone comprising polyethylene glycol; and (ii) hydrophobic side chain (s) selected from the group consisting of: C 4 -C 25 alkyl group, polypropylene, polybutylene, vinyl ester of a saturated C 1 -C 6 mono-carboxylic acid, C 1 -C 6 alkyl ester of acrylic or methacrylic acid, and mixtures thereof.
  • Suitable polyethylene glycol polymers have a polyethylene glycol backbone with random grafted polyvinyl acetate side chains.
  • the average molecular weight of the polyethylene glycol backbone can be in the range of from 2,000 Da to 20,000 Da, or from 4,000 Da to 8,000 Da.
  • the molecular weight ratio of the polyethylene glycol backbone to the polyvinyl acetate side chains can be in the range of from 1: 1 to 1: 5, or from 1: 1.2 to 1: 2.
  • the average number of graft sites per ethylene oxide units can be less than 1, or less than 0.8, the average number of graft sites per ethylene oxide units can be in the range of from 0.5 to 0.9, or the average number of graft sites per ethylene oxide units can be in the range of from 0.1 to 0.5, or from 0.2 to 0.4.
  • a suitable polyethylene glycol polymer is Sokalan HP22. Suitable polyethylene glycol polymers are described in WO08/007320.
  • Cellulosic polymer Suitable cellulosic polymers are selected from alkyl cellulose, alkyl alkoxyalkyl cellulose, carboxyalkyl cellulose, alkyl carboxyalkyl cellulose, sulphoalkyl cellulose, more preferably selected from carboxymethyl cellulose, methyl cellulose, methyl hydroxyethyl cellulose, methyl carboxymethyl cellulose, and mixures thereof.
  • Suitable carboxymethyl celluloses have a degree of carboxymethyl substitution from 0.5 to 0.9 and a molecular weight from 100,000 Da to 300,000 Da.
  • Suitable carboxymethyl celluloses have a degree of substitution greater than 0.65 and a degree of blockiness greater than 0.45, e.g. as described in WO09/154933.
  • Suitable care polymers include cellulosic polymers that are cationically modified and/or hydrophobically modified. Such modified cellulosic polymers can provide anti-abrasion benefits and dye lock benefits to fabric during the laundering cycle.
  • Suitable cellulosic polymers include cationically modified hydroxyethyl cellulose.
  • Suitable care polymers also include guar polymers that are cationically and/or hydrophobically modified.
  • Other suitable care polymers include dye lock polymers, for example the condensation oligomer produced by the condensation of imidazole and epichlorhydrin, preferably in ratio of 1: 4: 1.
  • a suitable commercially available dye lock polymer is FDI (Cognis) .
  • Suitable care polymers include amino-silicone, which can provide fabric feel benefits and fabric shape retention benefits.
  • the composition may comprise an alkoxylated polyalkyleneimine, wherein said alkoxylated polyalkyleneimine has a polyalkyleneimine core with one or more side chains bonded to at least one nitrogen atom in the polyalkyleneimine core, wherein said alkoxylated polyalkyleneimine has an empirical formula (I) of (PEI) a - (EO) b -R 1 , wherein a is the average number-average molecular weight (MW PEI ) of the polyalkyleneimine core of the alkoxylated polyalkyleneimine and is in the range of from 100 to 100,000 Daltons, wherein b is the average degree of ethoxylation in said one or more side chains of the alkoxylated polyalkyleneimine and is in the range of from 5 to 40, and wherein R 1 is independently selected from the group consisting of hydrogen, C 1 -C 4 alkyls, and combinations thereof.
  • the composition may comprise an alkoxylated polyalkyleneimine, wherein said alkoxylated polyalkyleneimine has a polyalkyleneimine core with one or more side chains bonded to at least one nitrogen atom in the polyalkyleneimine core, wherein the alkoxylated polyalkyleneimine has an empirical formula (II) of (PEI) o - (EO) m (PO) n -R 2 or (PEI) o - (PO) n (EO) m -R 2 , wherein o is the average number-average molecular weight (MW PEI ) of the polyalkyleneimine core of the alkoxylated polyalkyleneimine and is in the range of from 100 to 100,000 Daltons, wherein m is the average degree of ethoxylation in said one or more side chains of the alkoxylated polyalkyleneimine which ranges from 10 to 50, wherein n is the average degree of propoxylation in said one or more side chains of the
  • Suitable bleach includes sources of hydrogen peroxide, bleach activators, bleach catalysts, pre-formed peracids and any combination thereof.
  • a particularly suitable bleach includes a combination of a source of hydrogen peroxide with a bleach activator and/or a bleach catalyst.
  • Source of hydrogen peroxide include sodium perborate and/or sodium percarbonate.
  • Suitable bleach activators include tetra acetyl ethylene diamine and/or alkyl oxybenzene sulphonate.
  • Bleach catalyst The composition may comprise a bleach catalyst.
  • Suitable bleach catalysts include oxaziridinium bleach catalysts, transistion metal bleach catalysts, especially manganese and iron bleach catalysts.
  • a suitable bleach catalyst has a structure corresponding to general formula below:
  • R 13 is selected from the group consisting of 2-ethylhexyl, 2-propylheptyl, 2-butyloctyl, 2-pentylnonyl, 2-hexyldecyl, n-dodecyl, n-tetradecyl, n-hexadecyl, n-octadecyl, iso-nonyl, iso-decyl, iso-tridecyl and iso-pentadecyl.
  • Pre-formed peracid Suitable pre-form peracids include phthalimido-peroxycaproic acid. However, it is preferred that the composition is substantially free of pre-formed peracid. By: “substantially free” it is meant: “no deliberately added” .
  • Enzymes include lipases, proteases, cellulases, amylases and any combination thereof.
  • Suitable proteases include metalloproteases and/or serine proteases.
  • suitable neutral or alkaline proteases include: subtilisins (EC 3.4.21.62) ; trypsin-type or chymotrypsin-type proteases; and metalloproteases.
  • the suitable proteases include chemically or genetically modified mutants of the aforementioned suitable proteases.
  • Suitable commercially available protease enzymes include those sold under the trade names Liquanase Savinase and by Novozymes A/S (Denmark) , those sold under the tradename Preferenz series of proteases including P280, P281, P2018-C, P2081-WE, P2082-EE and P2083-A/J, Purafect Purafect and Purafect by DuPont, those sold under the tradename and by Solvay Enzymes, those available from Henkel/Kemira, namely BLAP (sequence shown in Figure 29 of US 5,352,604 with the folowing mutations S99D + S101 R + S103A + V104I + G159S, hereinafter referred to as BLAP) , BLAP R (BLAP with S3T + V4I + V199M + V205I + L217D) , BLAP X (BLAP with S3T + V4I + V205I) and BLAP F49 (BL
  • a suitable protease is described in WO11/140316 and WO11/072117.
  • Amylase Suitable amylases are derived from AA560 alpha amylase endogenous to Bacillus sp. DSM 12649, preferably having the following mutations: R118K, D183*, G184*, N195F, R320K, and/or R458K. Suitable commercially available amylases include Plus, Natalase, Ultra, SZ, (all Novozymes) and AA, Preferenz series of amylases, and Ox Am, HT Plus (all Du Pont) .
  • a suitable amylase is described in WO06/002643.
  • Suitable cellulases include those of bacterial or fungal origin. Chemically modified or protein engineered mutants are also suitable. Suitable cellulases include cellulases from the genera Bacillus, Pseudomonas, Humicola, Fusarium, Thielavia, Acremonium, e.g., the fungal cellulases produced from Humicola insolens, Myceliophthora thermophila and Fusarium oxysporum.
  • cellulases include and Premium, and (Novozymes A/S) , series of enzymes (Du Pont) , and series of enzymes (AB Enzymes) .
  • Suitable commercially available cellulases include Premium, Classic. Suitable cellulases are described in WO07/144857 and WO10/056652.
  • Suitable lipases include those of bacterial, fungal or synthetic origin, and variants thereof. Chemically modified or protein engineered mutants are also suitable. Examples of suitable lipases include lipases from Humicola (synonym Thermomyces) , e.g., from H. lanuginosa (T. lanuginosus) .
  • the lipase may be a “first cycle lipase” , e.g. such as those described in WO06/090335 and WO13/116261.
  • the lipase is a first-wash lipase, preferably a variant of the wild-type lipase from Thermomyces lanuginosus comprising T231R and/or N233R mutations.
  • Preferred lipases include those sold under the tradenames and by Novozymes, Bagsvaerd, Denmark.
  • Liprl 139 e.g. as described in WO2013/171241
  • TfuLip2 e.g. as described in WO2011/084412 and WO2013/033318.
  • Other enzymes are bleaching enzymes, such as peroxidases/oxidases, which include those of plant, bacterial or fungal origin and variants thereof.
  • bleaching enzymes such as peroxidases/oxidases, which include those of plant, bacterial or fungal origin and variants thereof.
  • Commercially available peroxidases include (Novozymes A/S) .
  • Other suitable enzymes include choline oxidases and perhydrolases such as those used in Gentle Power Bleach TM .
  • Suitable enzymes include pectate lyases sold under the tradenames (from Novozymes A/S, Bagsvaerd, Denmark) and (DuPont) and mannanases sold under the tradenames (Novozymes A/S, Bagsvaerd, Denmark) , and (Du Pont) .
  • identity refers to the relatedness between two amino acid sequences.
  • the degree of sequence identity between two amino acid sequences is determined using the Needleman-Wunsch algorithm (Needleman and Wunsch, 1970, J. Mol. Biol. 48: 443-453) as implemented in the Needle program of the EMBOSS package (EMBOSS: The European Molecular Biology Open Software Suite, Rice et al., 2000, Trends Genet. 16: 276-277) , preferably version 3.0.0 or later.
  • the optional parameters used are gap open penalty of 10, gap extension penalty of 0.5, and the EBLOSUM62 (EMBOSS version of BLOSUM62) substitution matrix.
  • the output of Needle labeled “longest identity” (obtained using the –nobrief option) is used as the percent identity and is calculated as follows:
  • Suitable fluorescent brighteners include: di-styryl biphenyl compounds, e.g. CBS-X, di-amino stilbene di-sulfonic acid compounds, e.g. DMS pure Xtra and HRH, and Pyrazoline compounds, e.g. SN, and coumarin compounds, e.g. SWN.
  • Preferred brighteners are: sodium 2 (4-styryl-3-sulfophenyl) -2H-napthol [1, 2-d] triazole, disodium 4, 4'-bis ⁇ [ (4-anilino-6- (N methyl-N-2 hydroxyethyl) amino 1 , 3, 5-triazin-2-yl) ] amino ⁇ stilbene-2-2'disulfonate, disodium 4, 4'-bis ⁇ [ (4-anilino-6-morpholino-1, 3, 5-triazin-2-yl) ] amino ⁇ stilbene-2-2'disulfonate, and disodium 4, 4'-bis (2-sulfostyryl) biphenyl.
  • a suitable fluorescent brightener is C.I. Fluorescent Brightener 260, which may be used in its beta or alpha crystalline forms, or a mixture of these forms.
  • Hueing agent Suitable hueing agents include small molecule dyes, typically falling into the Colour Index (C.I. ) classifications of Acid, Direct, Basic, Reactive (including hydrolysed forms thereof) or Solvent or Disperse dyes, for example classified as Blue, Violet, Red, Green or Black, and provide the desired shade either alone or in combination.
  • Preferred such hueing agents include Acid Violet 50, Direct Violet 9, 66 and 99, Solvent Violet 13 and any combination thereof.
  • hueing agents are known and described in the art which may be suitable for the present invention, such as hueing agents described in WO2014/089386.
  • Suitable hueing agents include phthalocyanine and azo dye conjugates, such as described in WO2009/069077.
  • Suitable hueing agents may be alkoxylated. Such alkoxylated compounds may be produced by organic synthesis that may produce a mixture of molecules having different degrees of alkoxylation. Such mixtures may be used directly to provide the hueing agent, or may undergo a purification step to increase the proportion of the target molecule.
  • Suitable hueing agents include alkoxylated bis-azo dyes, such as described in WO2012/054835, and/or alkoxylated thiophene azo dyes, such as described in WO2008/087497 and WO2012/166768.
  • the hueing agent may be incorporated into the detergent composition as part of a reaction mixture which is the result of the organic synthesis for a dye molecule, with optional purification step (s) .
  • Such reaction mixtures generally comprise the dye molecule itself and in addition may comprise un-reacted starting materials and/or by-products of the organic synthesis route.
  • Suitable hueing agents can be incorporated into hueing dye particles, such as described in WO 2009/069077.
  • the composition at 1wt%dilution in deionized water at 20°C has a reserve alkalinity to pH 7.5 of less than 3.0gNaOH/100g, preferably less than 2.5gNaOH/100g, or even less than 2.0gNaOH/100g.
  • the term “reserve alkalinity” is a measure of the buffering capacity of the detergent composition (g/NaOH/100g detergent composition) determined by titrating a 1% (w/v) solution of detergent composition with hydrochloric acid to pH 7.5 i.e. in order to calculate Reserve Alkalinity as defined herein:
  • T titre (ml) to pH 7.5
  • Perfume microparticles are made as follows. 200g of zeolite 13X is dried at 130 °C for 2 hours in an oven. Following this, 50g of perfume oil is mixed into the dried zeolite by hand with vigorous stirring.
  • 50g of the mix above are mixed with 450g of a surfactant powder (consisting of 85%LAS, 8%nonionic (Neodol 45-7) , 4%PEG 2000 and balance other miscellaneous/water) .
  • a surfactant powder consisting of 85%LAS, 8%nonionic (Neodol 45-7) , 4%PEG 2000 and balance other miscellaneous/water
  • This powder mix is then extruded in a twin-screw extruder (MXP19) equipped with a rotary cutter and die-plate to form extrudates of dimensions 2mm by 5mm by 5mm.
  • extrudates are then coated in a fluidized bed using a 20%aqueous solution of sodium carbonate containing 0.1%of a hueing dye and 0.2%TiO2 pigment and an air inlet temperature of 65 °C to as to form coated extrudates containing 30%by weight of sodium carbonate.
  • This composition is then blended with amylase, metalloprotease and lipase so as to introduce 0.01%by wt of each active enzyme into the composition to give the final product.
  • Zeolite 4A is dried at 130 °C for 2 hours in an oven then cool down to room temperature before use.
  • Perfume loaded zeolite 4A particle is made by spray 50 g of perfume on 450 g of zeolite 4A in drum mixer, then mixed for 3min.
  • LAS, AE30 nonionic, citric acid, sodium citrate and perfume loaded zeolite 4A particle are premixed in a cement mixer.
  • the premix is feed into extrusion/cutting equipment –SUNUP granulator SET-60 (Q) with 5mm die plate, extuded and cut (1.5mm length) .
  • cylinder core particles are then placed in coating equipment –Enger multi-function fluid bed HWBF-3G. 30%carbonate solution (at 60°C temperature) is applied and coated on the cylinder core particle under fluidize air temperature (70°C temperature) .
  • Example 5 comparative example
  • LAS, AE30 nonionic, citric acid, sodium citrate are premixed in a cement mixer.
  • the premix is feed into extrusion/cutting equipment –SUNUP granulator SET-60 (Q) with 5mm die plate, extuded and cut (1.5mm length) .
  • cylinder core particles are then placed in coating equipment –Enger multi-function fluid bed HWBF-3G.
  • Perfume loaded zeolite 4A particle (example 3) and 30%carbonate solution are mixed for 10 min (at 60°C temperature) to form coating premix.
  • the coating premix (at 60°C temperature) is applied and coated on the cylinder core particle under fluidize air temperature (70°C temperature) .
  • GC-MS Gas Chromatography-Mass Spectrometry
  • Multipurpose AutoSampler MPS (GERSTEL Inc., Linthicum, Maryland, U.S.A) ; and J&W TM DB-5ms Ultra Inert (30 m length x 0.25 mm internal diameter x 0.25 ⁇ m film thickness) (J&W Scientific/Agilent Technologies Inc., Santa Clara, California, U.S.A. ) .
  • the hexane layer collected in 2mL vial is analyzed by GC/MS.
  • MSD Full Scan mode with a minimum range of 40 to 300 m/z (a wider range may be used) .
  • perfume solutions are prepared in hexane with Tetradecane (internal standard) concentration of 25 mg/L, respectively, and transferred into glass auto sampler vials for GC-MS analysis.
  • Perfume composition is identified by matching their retention times and mass spectra with those of reference standards. Total target responses of standards are devided by target responses of internal standard (Ri) to correct error among samples. External standard curve is built on Rp/Ri vs.perfume concentration. Then Rp/Ri of each samples is used to calculate perfume concentration based on the external standard curve.
  • Example 4 Sample Perfume Concentration (in coated detergent particle) Example 4 (Inventive) 0.76% ⁇ 0.06% Example 5 (Comparative) 0.06% ⁇ 0.004%

Landscapes

  • 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)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)

Abstract

L'invention concerne un procédé de préparation d'une particule de détergent enrobée ayant des dimensions perpendiculaires x, y et z, x étant de 1 à 2 mm, y étant de 2 à 8 mm, et z étant de 2 à 8 mm, le procédé comprenant les étapes suivantes : (i) formation d'un mélange détersif comprenant de 40 % en poids à 90 % en poids de tensioactif détersif et de 0,5 % en poids à 20 % en poids de microparticules de parfum ; (ii) extrusion du mélange détersif de l'étape (i) pour former un matériau extrudé ; (iii) revêtement du matériau extrudé avec un sel inorganique hydrosoluble sous la forme d'une solution aqueuse pour former un matériau extrudé enrobé par voie humide comprenant de 1 % en poids à 40 % en poids de sel inorganique hydrosoluble ; et (iv) élimination de l'eau du matériau extrudé enrobé par voie humide pour former la particule de détergent enrobée.
PCT/CN2017/117074 2016-12-22 2017-12-19 Composition de détergent pour le linge WO2018113645A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP17883274.7A EP3559194A4 (fr) 2016-12-22 2017-12-19 Composition de détergent pour le linge

Applications Claiming Priority (34)

Application Number Priority Date Filing Date Title
EP16206480 2016-12-22
EP16206461 2016-12-22
EP16206480.2 2016-12-22
EP16206477.8 2016-12-22
EP16206487 2016-12-22
EP16206498.4 2016-12-22
EP16206490 2016-12-22
EP16206487.7 2016-12-22
EP16206503 2016-12-22
EP16206477 2016-12-22
EP16206451 2016-12-22
EP16206451.3 2016-12-22
EP16206503.1 2016-12-22
EP16206461.2 2016-12-22
EP16206498 2016-12-22
EP16206490.1 2016-12-22
EP17173004.7A EP3339416A1 (fr) 2016-12-22 2017-05-26 Composition de détergent pour lessive
EP17173002.1 2017-05-26
EP17173001.3 2017-05-26
EP17173007.0A EP3339419A1 (fr) 2016-12-22 2017-05-26 Composition de détergent pour lessive
EP17172999.9A EP3339413A1 (fr) 2016-12-22 2017-05-26 Composition de détergent pour lessive
EP17173004.7 2017-05-26
EP17173103.7 2017-05-26
EP17173001.3A EP3339407A1 (fr) 2016-12-22 2017-05-26 Composition de détergent pour lessive
EP17173000.5A EP3339414A1 (fr) 2016-12-22 2017-05-26 Composition de détergent pour lessive
EP17172999.9 2017-05-26
EP17173006.2 2017-05-26
EP17173000.5 2017-05-26
EP17173007.0 2017-05-26
EP17173103 2017-05-26
EP17173005.4 2017-05-26
EP17173005.4A EP3339417A1 (fr) 2016-12-22 2017-05-26 Composition de détergent pour lessive
EP17173006.2A EP3339418A1 (fr) 2016-12-22 2017-05-26 Composition de détergent pour lessive
EP17173002.1A EP3339415A1 (fr) 2016-12-22 2017-05-26 Composition de détergent pour lessive

Publications (1)

Publication Number Publication Date
WO2018113645A1 true WO2018113645A1 (fr) 2018-06-28

Family

ID=62624453

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2017/117074 WO2018113645A1 (fr) 2016-12-22 2017-12-19 Composition de détergent pour le linge

Country Status (2)

Country Link
EP (1) EP3559194A4 (fr)
WO (1) WO2018113645A1 (fr)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2441825A1 (fr) * 2010-10-14 2012-04-18 Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House Procédé pour la préparation de particules de détergent pour le lavage du linge
WO2012048948A1 (fr) * 2010-10-14 2012-04-19 Unilever Plc Particules de détergent à lessive
WO2012048910A1 (fr) * 2010-10-14 2012-04-19 Unilever Plc Composition de détergent particulaire conditionnée
WO2012048947A1 (fr) * 2010-10-14 2012-04-19 Unilever Plc Particules de détergent à lessive
EP2639291A1 (fr) * 2012-03-13 2013-09-18 Unilever PLC Composition de détergent particulaire conditionnée
WO2013139702A1 (fr) * 2012-03-21 2013-09-26 Unilever Plc Particules de détergent à lessive
WO2013149753A1 (fr) * 2012-04-03 2013-10-10 Unilever Plc Particules de détergent à lessive
WO2013149752A1 (fr) * 2012-04-03 2013-10-10 Unilever Plc Particules de détergent à lessive
WO2013149754A1 (fr) * 2012-04-03 2013-10-10 Unilever Plc Particules de détergent à lessive

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2441825A1 (fr) * 2010-10-14 2012-04-18 Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House Procédé pour la préparation de particules de détergent pour le lavage du linge
WO2012048948A1 (fr) * 2010-10-14 2012-04-19 Unilever Plc Particules de détergent à lessive
WO2012048910A1 (fr) * 2010-10-14 2012-04-19 Unilever Plc Composition de détergent particulaire conditionnée
WO2012048947A1 (fr) * 2010-10-14 2012-04-19 Unilever Plc Particules de détergent à lessive
EP2639291A1 (fr) * 2012-03-13 2013-09-18 Unilever PLC Composition de détergent particulaire conditionnée
WO2013139702A1 (fr) * 2012-03-21 2013-09-26 Unilever Plc Particules de détergent à lessive
WO2013149753A1 (fr) * 2012-04-03 2013-10-10 Unilever Plc Particules de détergent à lessive
WO2013149752A1 (fr) * 2012-04-03 2013-10-10 Unilever Plc Particules de détergent à lessive
WO2013149754A1 (fr) * 2012-04-03 2013-10-10 Unilever Plc Particules de détergent à lessive

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP3559194A4 *

Also Published As

Publication number Publication date
EP3559194A4 (fr) 2020-05-20
EP3559194A1 (fr) 2019-10-30

Similar Documents

Publication Publication Date Title
EP2451921B1 (fr) Composition solide de détergent pour le traitement des tissus légèrement alcaline, comprenant de l'acide phtalimido peroxy caproïque
EP3301152B1 (fr) Particule de base de détergent sechée par atomisation, fournissant un bas ph dans le linge
EP2377914B1 (fr) Composition de détergent solide à faible teneur en adjuvants pour le traitement des tissus comprenant de la perhydrolase
EP3301168B1 (fr) Composition de détergent pour lessive
US20180094228A1 (en) Laundry detergent composition
WO2018067484A1 (fr) Composition de détergent à lessive
WO2019191174A1 (fr) Composition de détergent pour lessive
EP3301145A1 (fr) Composition de détergent pour lessive à bas ph
EP3339414A1 (fr) Composition de détergent pour lessive
EP3559189A1 (fr) Composition de détergent pour le linge
WO2018113646A1 (fr) Composition de détergent pour le linge
EP3339422B1 (fr) Composition de détergent pour lessive
EP3559194A1 (fr) Composition de détergent pour le linge
EP3339420A1 (fr) Composition de détergent pour lessive
WO2019191172A1 (fr) Procédé de préparation d'une particule détergente à pulvérisation sèche pour le linge
EP3339417A1 (fr) Composition de détergent pour lessive
EP3339419A1 (fr) Composition de détergent pour lessive
EP3301150A1 (fr) Composition de détergent pour lessive à bas ph
EP3339407A1 (fr) Composition de détergent pour lessive
EP3339418A1 (fr) Composition de détergent pour lessive
EP3339416A1 (fr) Composition de détergent pour lessive
EP3339415A1 (fr) Composition de détergent pour lessive
EP3339413A1 (fr) Composition de détergent pour lessive
EP3559188A1 (fr) Composition de détergent pour le linge
WO2011109292A1 (fr) Composition de détergent pour lessive solide comprenant un azurant optique sous forme particulaire micronisée

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17883274

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

ENP Entry into the national phase

Ref document number: 2017883274

Country of ref document: EP

Effective date: 20190722