EP3642319B1 - Compositions de détergents particulaires comprenant un parfum - Google Patents

Compositions de détergents particulaires comprenant un parfum Download PDF

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Publication number
EP3642319B1
EP3642319B1 EP18729125.7A EP18729125A EP3642319B1 EP 3642319 B1 EP3642319 B1 EP 3642319B1 EP 18729125 A EP18729125 A EP 18729125A EP 3642319 B1 EP3642319 B1 EP 3642319B1
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EP
European Patent Office
Prior art keywords
perfume
detergent
detergent particle
particle
coating
Prior art date
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EP18729125.7A
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German (de)
English (en)
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EP3642319A1 (fr
Inventor
Judith Maria Bonsall
Stephen Thomas Keningley
Patrick Thomas MCGUIRE
Fakhruddin Esmail Pacha
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Unilever Global IP Ltd
Unilever IP Holdings BV
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Unilever PLC
Unilever NV
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Publication of EP3642319A1 publication Critical patent/EP3642319A1/fr
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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
    • 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 detergent particles having perfume, particularly to detergent particles having a coating applied around a surfactant core.
  • Perfumes are generally incorporated into the detergent compositions either to deliver fragrance in the headspace of the package or to deliver fragrance to the clothes being washed, in order to give a fresh clean smell.
  • the free oil and perfume in particulate or powder forms are added onto the detergent powder by spraying or other means for incorporating the free oils.
  • the perfume added at this stage is held in the small pores present in the powder structure by capillary pressure.
  • Detergent composition may also be produced by an extrusion process, in such a process the perfume addition is along with the extrudable mass.
  • the perfume is added into the extrudable mass prior to the process of extrusion for multiple reasons. Addition of the perfume prior to the extrusion process makes the product sticky and forming an easily extrudable mass which is also more consumer acceptable upon extrusion.
  • the process of extrusion eliminates the small capillary channels that would normally hold the perfume in the powder detergent composition, thus prior addition of perfume into the extrudable mass ensures that perfume is better held in the extruded particle.
  • WO2005/059083 A1 discloses a granulated detergent composition having encapsulated perfume.
  • the granulated detergent product includes coated granules which has a functional core and a coating having encapsulated perfume for improving the dispersion of the dry encapsulated perfume throughout the detergent composition without the use of significant shear forces, which may result in noticeable perfume losses.
  • EP2627748 B1 (2014, Unilever ) discloses a particulate detergent composition having an extruded surfactant core having an inorganic coating.
  • the detergent composition has perfume added into the core either as a liquid or as encapsulated perfume particles.
  • the present inventors have observed perfume losses in the range of 10 to 50% by way of evaporation, when exposed to temperature conditions generally employed during extrusion. Furthermore, the exhaust air carrying such perfume impacts environment and surroundings and thereby the exhaust air requires further treatment before releasing into the environment.
  • a detergent particle having a core and a coating enveloping the core, said detergent particle having perpendicular dimensions x, y and z, wherein x is from 0.2 to 2 mm, y is from 2 to 8 mm, and z is from 2 to 8 mm and the particle comprises:
  • Disclosed detergent particle has perpendicular dimensions x, y and z, where x is from 0.2 to 2 mm, y is from 2 to 8 mm, and z is from 2 to 8 mm.
  • a detergent formulation having the detergent particle according to the present invention at least 90 to 100 % of the detergent particle in the x, y and z dimensions are within a 20 %, preferably 10%, variable from the largest to the smallest detergent particle.
  • the detergent particles are larger and less spherical than conventional detergent powders.
  • the detergent particle is curved.
  • the size is such that y and z are at least 2 mm, preferably at least 2.5 mm, still preferably at least 3mm, more preferably at least 4 mm, and x lies in the range 0.2 to 2 mm, preferably 0.5 to 2 mm, more preferably 1 to 2 mm, still preferably 0.6 to 1.6mm.
  • Preferred ranges of y lies in the range from 3 to 8 mm, more preferably from 4 to 6 mm, still preferably from 4.5 mm to 5.5 mm.
  • Preferred ranges of z lies in the range from 3 to 8 mm, more preferably from 4 to 6 mm, still preferably from 4.5 mm to 5.5 mm.
  • the detergent particle may be shaped as a disc.
  • the detergent particle are oblate spheroids.
  • the coated detergent particle does not have hole; that is to say, the detergent particle does not have a conduit passing there through that passes through the core, i.e., the coated detergent particle has a topologic genus of zero.
  • Porosity of the detergent particle of the present invention having a coating enveloping the core is in the range from 0 to 0.2 volume fraction, more preferably from 0.01 to 0.1, still preferably from 0.04 to 0.1, most preferably from 0.05 to 0.1. It is surprisingly found that the detergent particle having intra-particle porosity in the range from 0 to 0.1 volume fraction is capable of holding the perfume in the coating of the detergent particle of the present invention without altering the flow properties of the detergent particle.
  • the detergent particle of the present invention includes an extruded core and the intra particle porosity of the detergent particle having an extruded core and coated with a coating material is preferably in the range of 0 to 0.1 volume fraction.
  • the extruded particle has a lower intra-particle porosity as compared to a detergent particle prepared by a high shear mixer granulator.
  • the typical values of the intra-particle porosity of a high shear mixer granulated detergent particle is in the range from 0.3 to 0.5 volume fraction.
  • a high shear mixer granulated detergent particle due to the capillary pressure resulting from the intra particle porosity is capable of effectively entrapping liquid added to the particle surface, such as perfume.
  • a detergent particle preferably having an extruded core and subsequently coated with the coating material has lower intra-particle porosity and has low liquid absorption capability via capillary absorption.
  • the porosity of the detergent particle of the present invention was measured determined using a Quantachrom Helium Pycnometer, Model Ultra pycnometer 1000.
  • the intra particle porosity E ⁇ for the detergent particle was calculated to be 0 to 0.2, more preferably 0 to 0.18, more preferably 0 to 0.1.
  • Disclosed detergent particle has a core and a coating applied to the core, which coating envelops the core.
  • the appearance of the coated particle is pleasing if the core of the detergent particle is formed by extrusion.
  • the core of the detergent particle includes the surfactant and the coating includes the coating material and the perfume.
  • the coating material forms a layer enveloping the core and the perfume forms a layer enveloping at least an outer surface of the coating material.
  • the detergent particle has a core to coating ratio of from 3:1 to 20:1, most preferably 5:1 to 15:1; the optimal ratio of core to coating ratio is 9:1.
  • the detergent particle according to the present invention has 20 wt% to 39wt% surfactant and the core of the detergent particle includes 95 parts to 100 parts of the total surfactant content.
  • the detergent particle includes 96 parts to 100 parts, still preferably 97.5 parts to 100 parts and still more preferably 98 to 100 parts of the total surfactant content.
  • nonionic and anionic surfactants of the surfactant system may be chosen from the surfactants described " Surface Active Agents” Vol. 1, by Schwartz & Perry, Interscience 1949 , Vol. 2 by Schwartz, Perry & Berch, Interscience 1958 , in the current edition of " McCutcheon's Emulsifiers and Detergents” published by Manufacturing Confectioners Company or in " Tenside-Taschenbuch", H. Stache, 2nd Edn., Carl Hauser Verlag, 1981 .
  • the surfactant used are saturated.
  • the detergent particle of the present invention includes 20 to 39wt% of a surfactant, preferably 25 to 39wt% and still preferably 30 wt% to 35wt% surfactant.
  • the surfactant is preferably selected from anionic surfactant, non-ionic surfactant or mixtures thereof.
  • Preferably 15 to 85 parts of the total surfactant content in the detergent particle is anionic surfactant and from 5 to 75 parts of the total surfactant content is non-ionic surfactant.
  • Suitable anionic detergent compounds which may be used are usually water-soluble alkali metal salts of organic sulphates and sulphonates having alkyl radicals containing from about 8 to about 22 carbon atoms, the term alkyl being used to include the alkyl portion of higher acyl radicals.
  • suitable synthetic anionic detergent compounds are sodium and potassium alkyl sulphates, especially those obtained by sulphating higher C 8 to C 18 alcohols, produced for example from tallow or coconut oil, sodium and potassium alkyl C 9 to C 20 benzene sulphonates, particularly sodium linear secondary alkyl C 10 to C 15 benzene sulphonates; and sodium alkyl glyceryl ether sulphates, especially those ethers of the higher alcohols derived from tallow or coconut oil and synthetic alcohols derived from petroleum.
  • anionic surfactants are sodium lauryl ether sulfate (SLES), particularly preferred with 1 to 3 ethoxy groups, sodium C 10 to C 15 alkyl benzene sulphonates and sodium C 12 to C 18 alkyl sulphates. Also applicable are surfactants such as those described in EP-A-328 177 (Unilever ), which show resistance to salting-out, the alkyl polyglycoside surfactants described in EP-A-070 074 , and alkyl monoglycosides. The chains of the surfactants may be branched or linear.
  • the fatty acid soap used preferably contains from about 16 to about 22 carbon atoms, preferably in a straight chain configuration.
  • the anionic contribution from soap is preferably from 0 to 30 wt % of the total anionic.
  • At least 50 wt % of the anionic surfactant is selected from: sodium C 11 to C 15 alkyl benzene sulphonates; and, sodium C 12 to C 18 alkyl sulphates. Even more preferably, the anionic surfactant is sodium C 11 to C 15 alkyl benzene sulphonates.
  • Nonionic surfactant is N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N-N-N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N-(2-aminoethyl)-2-aminoethyl-N
  • Suitable nonionic detergent compounds which may be used include, in particular, the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example, aliphatic alcohols, acids, amides or alkyl phenols with alkylene oxides, especially ethylene oxide either alone or with propylene oxide.
  • Preferred nonionic detergent compounds are C 6 to C 22 alkyl phenol-ethylene oxide condensates, generally 5 to 25 EO, i.e. 5 to 25 units of ethylene oxide per molecule, and the condensation products of aliphatic C 8 to C 18 primary or secondary linear or branched alcohols with ethylene oxide, generally 5 to 50 EO.
  • the non-ionic is 10 to 50 EO, more preferably 20 to 35 EO.
  • Alkyl ethoxylates are particularly preferred.
  • surfactants are mixed together before being dried. Conventional mixing equipment may be used.
  • the surfactant core of the detergent particle may be formed by extrusion or roller compaction and subsequently coated with an inorganic salt.
  • the core of the detergent particle is an extrudate.
  • the surfactant system used is calcium tolerant and this is a preferred aspect because this reduces the need for builder.
  • Surfactant blends that do not require builders to be present for effective detergency in hard water are preferred. Such blends are called calcium tolerant surfactant blends if they pass the test set out hereinafter. However, the invention may also be of use for washing with soft water, either naturally occurring or made using a water softener. In this case, calcium tolerance is no longer important and blends other than calcium tolerant ones may be used.
  • the surfactant blend in question is prepared at a concentration of 0.7 g surfactant solids per litre of water containing sufficient calcium ions to give a French hardness of 40 (4 x 10 -3 Molar Ca 2+ ).
  • Other hardness ion free electrolytes such as sodium chloride, sodium sulphate, and sodium hydroxide are added to the solution to adjust the ionic strength to 0.05M and the pH to 10.
  • the adsorption of light of wavelength 540 nm through 4 mm of sample is measured 15 minutes after sample preparation. Ten measurements are made and an average value is calculated. Samples that give an absorption value of less than 0.08 are deemed to be calcium tolerant.
  • Suitable calcium tolerant co-surfactants include SLES 1 to 7 EO, and alkyl-ethoxylate nonionic surfactants, particularly those with melting points less than 40°C.
  • the core is primarily surfactant, it may also include detergency additives, such as shading dye, enzymes and polymers.
  • Disclosed detergent particle has a coating enveloping the core.
  • the coating includes 95 parts to 100 parts of the total coating material content and the total perfume content of the detergent particle.
  • the coating material forms a layer enveloping the core and the perfume forms a layer on a surface of the coating material layer. It is preferred that the coating material forms a layer enveloping at least a portion of the outer surface of the core, more preferably the coating material forms a layer enveloping at least 50%, more preferably at least 60%, still preferably at least 80% and further preferably completely envelops the outer surface of the coating material.
  • the coating includes 96 parts to 100 parts, more preferably 98 parts to 100 parts most preferably 99 parts to 100 parts of the total coating material content and the total perfume content of the detergent particle.
  • the coating of the detergent particle comprises less than 5wt%, even preferably less than 2.5wt%, further preferably less than 1wt%, still preferably less than 0.5wt% surfactant, more specifically a non-ionic surfactant.
  • any known coating material may be used, for instance organic coating material, including polymer, it has been found to be particularly advantageous to use an inorganic coating material deposited by crystallisation from an aqueous solution as this appears to give positive dissolution benefits and the coating gives a good colour to the detergent particle, even at lower coating levels.
  • the coating material is preferably applied to the surface of the surfactant core, by deposition from an aqueous solution of the coating material.
  • the coating material layer is applied in the form of a slurry. It is highly preferred to coat by spraying an aqueous solution of the coating material in a fluidised bed drier.
  • the bed is typically fluidized with heated air in order to dry or partially dry moisture from the spray coating as it is applied.
  • the spraying is achieved via nozzles capable of forming a fine or atomized spray of the coating mixture to achieve complete coverage of the particles.
  • the droplet size from the atomizer is less than about 100 micrometres.
  • This atomization can be achieved either through a conventional two-fluid nozzle with atomizing air, or alternatively by means of a conventional pressure nozzle.
  • the solution or slurry rheology is typically characterized by a viscosity of less than about 500 centipoise, preferably less than about 200 centipoise.
  • the nozzle location is placed at or above the fluidized height of the particles in the fluid bed. The fluidized height is typically determined by a weir or overflow gate height.
  • the coating zone of the fluid bed is then typically followed by a drying zone and a cooling zone.
  • a drying zone and a cooling zone are also possible to achieve the resultant coating on the detergent particles of the present invention.
  • An alternative embodiment uses an agitated fluid bed, which includes mechanical and/or pneumatic mixing elements in addition to the conventional bed that is fluidized air passing through holes in a distributor plate.
  • the advantage of the agitated bed is that it can be used to apply additional shear as a means to control granular shape and smoothness while performing the coating operation.
  • the coating material is an inorganic material.
  • the inorganic material is preferably an inorganic salt, more preferably a water soluble inorganic salt.
  • Inorganic salt(s) is/are preferably present as a coating on the detergent particle, the coating is present enveloping the core.
  • the inorganic salt(s) is/are preferably present at a level that reduces the stickiness of the detergent particle to a point where the particles are free flowing.
  • Disclosed detergent particle includes 10 to 40wt% of the coating material.
  • the coating material is an inorganic salt it is preferably selected from sodium carbonate and/or sodium sulphate of which preferably at least 5 parts of the total inorganic salt is sodium carbonate.
  • the inorganic salt forms a layer covering/enveloping the core and the coating is preferably applied to the surface of the surfactant core, by deposition from an aqueous solution having 25 to 30wt% of the water-soluble inorganic salt.
  • coating can be performed using a slurry.
  • the aqueous solution preferably contains greater than 150g/L, more preferably 300 g/L of the salt.
  • An aqueous spray-on of the coating solution in a fluidized bed has been found to give good results and may also generate a slight rounding of the detergent particle during the fluidisation process. Drying and/or cooling may be needed to finish the process.
  • the coating of the detergent particle according to the present invention includes a perfume.
  • the perfume may be present either within the coating material layer, on the outer surface of the coating material layer or at least covering a portion of the outer surface of the coating layer or a combination of thereof.
  • the perfume forms a layer on a surface of the coating material layer. It is preferred that the perfume forms a layer enveloping at least a portion of an outer surface of the coating material, more preferably completely enveloping an outer surface of the coating material.
  • Perfume is preferably sprayed onto a detergent particle having a surfactant core pre-coated with a coating material layer, which coating material is preferably an inorganic salt, still preferably a water soluble inorganic salt.
  • a coating material layer which coating material is preferably an inorganic salt, still preferably a water soluble inorganic salt.
  • pre-coated refers to the detergent particle comprising the surfactant core enveloped with a coating material but prior to coating with the perfume.
  • the perfume forms a layer on an exposed outer surface of the coating material layer.
  • the perfume layer either covers a portion of the outer surface of the coating material layer, or covers the entire outer surface of the coating material layer. It is believed that presence of perfume layer on the surface of the coating material layer improves perfume delivery and maintains the encapsulated perfume intact.
  • the spray coating is in a mixer other than a fluid bed drier.
  • the perfume layer includes a free oil perfume, perfume in encapsulated form encapsulating a free oil also termed herein as encapsulated perfume or mixtures thereof.
  • the content of perfume molecules in the free oil is in the range from 90 to 100wt% by weight of the free oil composition.
  • the free oil may have small amounts of solvent in the composition, the content of such solvent preferably is in the range from 0 to 10wt% but most preferably not more than 5wt%.
  • the encapsulated perfume is in the form of an slurry suspending the encapsulated perfume droplets/particles in a polar solvent, preferably the slurry is an aqueous slurry.
  • the encapsulated perfume composition in this form comprises from 30 to 60wt% moisture and between 30 to 50wt% perfume oil.
  • the encapsulated perfume composition includes a polymeric structuring system to increase the viscosity of the aqueous phase. The inclusion of the polymeric structuring system ensures that the encapsulated perfume is uniformly dispersed in the composition and does not separate out from the mixture. Any commercially available encapsulated perfume may be used for the present invention.
  • a preferred kind of the encapsulated perfume is shear sensitive encapsulated perfume.
  • the preferred ratio in which the free oil to encapsulated perfume is present is between 5:1 to 1:5, more preferably 2:1 to 1:2 and the most optimum ratio is 1:1.
  • the perfume layer is multi-layered.
  • the multi-layered perfume includes a layer of perfume in encapsulate form and a layer of free oil.
  • the multi-layered perfume includes a layer of perfume in encapsulate form enveloping a layer of free oil.
  • the layer of perfume in the encapsulate form preferably envelops a portion of the outer surface of free oil layer, or more preferably envelops the entire outer surface of the free oil layer.
  • the free oil layer is applied first followed by the deposition of a layer of perfume in encapsulated form.
  • the layer of free oil is proximal to an outer surface of the coating material layer of the detergent particle.
  • the particles are then treated to provide a perfume layer on the coating material layer.
  • the perfume layer is preferably provided by spraying the perfume oil or the perfume in encapsulate form in a coating mixer onto the pre-coated detergent particle.
  • the coating mixer may be any of a number of mixers including low speed mixers and drum mixers.
  • the detergent particle includes perfume preferably in the range from 0.001 to 3 wt %, most preferably from 0.1 to 2 wt %.
  • perfumes are provided in the CTFA (Cosmetic, Toiletry and Fragrance Association) 1992 International Buyers Guide, published by CFTA Publications and OPD 1993 Chemicals Buyers Directory 80th Annual Edition, published by Schnell Publishing Co.
  • compositions of the present invention it is envisaged that there will be four or more, preferably five or more, more preferably six or more or even seven or more different perfume components.
  • the perfume may be in the form of a solid, liquid solution having an organic solvent, or in the form of a slurry having a polar solvent.
  • top notes are defined by Poucher (Journal of the Society of Cosmetic Chemists 6(2):80 [1955 ]).
  • Preferred top-notes are selected from citrus oils, linalool, linalyl acetate, lavender, dihydromyrcenol, rose oxide and cis-3-hexanol.
  • the detergent particle does not contain a peroxygen bleach, e.g., sodium percarbonate, sodium perborate, and peracid.
  • a peroxygen bleach e.g., sodium percarbonate, sodium perborate, and peracid.
  • the detergent particle preferably includes from 0 to 15 wt% water, more preferably 0 to 10 wt%, most preferably from 1 to 5wt % water, at 293K and 50% relative humidity. This facilitates the storage stability of the detergent particle and its mechanical properties.
  • the detergent particle according to the present invention may include further ingredients as described below which may be present in the coating or the core of the particle or in both the core as well as the coating.
  • the detergent particle preferably comprises a fluorescent agent (optical brightener).
  • fluorescent agents are well known and many such fluorescent agents are available commercially. Usually, these fluorescent agents are supplied and used in the form of their alkali metal salts, for example, the sodium salts.
  • the total amount of the fluorescent agent or agents used in the composition is generally from 0.005 to 2 wt %, more preferably 0.01 to 0.1 wt %. Suitable fluorescer for use in the invention are described in chapter 7 of Industrial Dyes edited by K.Hunger 2003 Wiley-VCH ISBN 3-527-30426-6 .
  • Preferred fluorescers are selected from the classes distyrylbiphenyls, triazinylaminostilbenes, bis(1,2,3-triazol-2-yl)stilbenes, bis(benzo[b]furan-2-yl)biphenyls, 1,3-diphenyl-2-pyrazolines and courmarins.
  • the fluorescer is preferably sulfonated.
  • Preferred classes of fluorescer are: Di-styryl biphenyl compounds, e.g. Tinopal (Trade Mark) CBS-X, Di-amine stilbene di-sulphonic acid compounds, e.g. Tinopal DMS pure Xtra and Blankophor (Trade Mark) HRH, and Pyrazoline compounds, e.g. Blankophor SN.
  • Di-styryl biphenyl compounds e.g. Tinopal (Trade Mark) CBS-X
  • Di-amine stilbene di-sulphonic acid compounds e.g. Tinopal DMS pure Xtra and Blankophor (Trade Mark) HRH
  • Pyrazoline compounds e.g. Blankophor SN.
  • Preferred fluorescers 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.
  • Tinopal® DMS is the disodium salt of disodium 4,4'-bis ⁇ [(4-anilino-6-morpholino-1,3,5-triazin-2-yl)]amino ⁇ stilbene-2-2' disulfonate.
  • Tinopal® CBS is the disodium salt of disodium 4,4'-bis(2-sulfostyryl)biphenyl.
  • the detergent particle may preferably include one or more polymers.
  • polymers include carboxymethylcellulose, poly (ethylene glycol), poly(vinyl alcohol), polyethylene imines, ethoxylated polyethylene imines, water soluble polyester polymers polycarboxylates such as polyacrylates, maleic/acrylic acid copolymers and lauryl methacrylate/acrylic acid copolymers.
  • the detergent particle includes one or more enzymes.
  • the level of each enzyme is from 0.0001 wt% to 0.5 wt% protein on product.
  • Especially contemplated enzymes include proteases, alpha-amylases, cellulases, lipases, peroxidases/oxidases, pectate lyases, laccases and mannanases, or mixtures thereof.
  • Suitable lipases include those of bacterial or fungal origin. Chemically modified or protein engineered mutants are included. Examples of useful lipases include lipases from Humicola (synonym Thermomyces), e.g. from H. lanuginosa ( T. lanuginosus ) as described in EP 258 068 and EP 305 216 or from H. insolens as described in WO 96/13580 , a Pseudomonas lipase, e.g. from P. alcaligenes or P. pseudoalcaligenes ( EP 218 272 ), P. cepacia ( EP 331 376 ), P. stutzeri ( GB 1,372,034 ), P.
  • lipase variants such as those described in WO 92/05249 , WO 94/01541 , EP 407 225 , EP 260 105 , WO 95/35381 , WO 96/00292 , WO 95/30744 , WO 94/25578 , WO 95/14783 , WO 95/22615 , WO 97/04079 and WO 97/07202 , WO 00/60063 , WO 09/107091 and WO09/111258 .
  • LipolaseTM and Lipolase UltraTM LipexTM (Novozymes A/S) and LipocleanTM.
  • the method of the invention may be carried out in the presence of phospholipase classified as EC 3.1.1.4 and/or EC 3.1.1.32.
  • phospholipase is an enzyme which has activity towards phospholipids.
  • Phospholipids such as lecithin or phosphatidylcholine, consist of glycerol esterified with two fatty acids in an outer (sn-1) and the middle (sn-2) positions and esterified with phosphoric acid in the third position; the phosphoric acid, in turn, may be esterified to an amino-alcohol.
  • Phospholipases are enzymes which participate in the hydrolysis of phospholipids.
  • phospholipases A 1 and A 2 which hydrolyze one fatty acyl group (in the sn-1 and sn-2 position, respectively) to form lysophospholipid
  • lysophospholipase or phospholipase B
  • Phospholipase C and phospholipase D release diacyl glycerol or phosphatidic acid respectively.
  • proteases include those of animal, vegetable or microbial origin. Microbial origin is preferred. Chemically modified or protein engineered mutants are included.
  • the protease may be a serine protease or a metallo protease, preferably an alkaline microbial protease or a trypsin-like protease.
  • Preferred commercially available protease enzymes include AlcalaseTM, SavinaseTM, PrimaseTM, DuralaseTM, DyrazymTM, EsperaseTM, EverlaseTM, PolarzymeTM, and KannaseTM, (Novozymes A/S), MaxataseTM, MaxacalTM, MaxapemTM, ProperaseTM, PurafectTM, Purafect OxPTM, FN2TM, and FN3TM (Genencor International Inc.).
  • the method of the invention may be carried out in the presence of cutinase. classified in EC 3.1.1.74.
  • the cutinase used according to the invention may be of any origin.
  • Preferably cutinases are of microbial origin, in particular of bacterial, of fungal or of yeast origin.
  • Suitable amylases include those of bacterial or fungal origin. Chemically modified or protein engineered mutants are included. Amylases include, for example, alpha-amylases obtained from Bacillus, e.g. a special strain of B . licheniformis, described in more detail in GB 1,296,839 , or the Bacillus sp. strains disclosed in WO 95/026397 or WO 00/060060 .
  • amylases are DuramylTM, TermamylTM, Termamyl UltraTM, NatalaseTM, StainzymeTM, FungamylTM and BANTM (Novozymes A/S), RapidaseTM and PurastarTM (from Genencor International Inc.).
  • Suitable cellulases include those of bacterial or fungal origin. Chemically modified or protein engineered mutants are included. Suitable cellulases include cellulases from the genera Bacillus, Pseudomonas, Humicola, Fusarium, Thielavia, Acremonium, e.g. the fungal cellulases produced from Humicola insolens, Thielavia terrestris, Myceliophthora thermophila, and Fusarium oxysporum disclosed in US 4,435,307 , US 5,648,263 , US 5,691,178 , US 5,776,757 , WO 89/09259 , WO 96/029397 , and WO 98/012307 .
  • cellulases include CelluzymeTM, CarezymeTM, EndolaseTM, RenozymeTM (Novozymes A/S), ClazinaseTM and Puradax HATM (Genencor International Inc.), and KAC-500(B)TM (Kao Corporation).
  • Suitable peroxidases/oxidases include those of plant, bacterial or fungal origin. Chemically modified or protein engineered mutants are included. Examples of useful peroxidases include peroxidases from Coprinus, e.g. from C. cinereus, and variants thereof as those described in WO 93/24618 , WO 95/10602 , and WO 98/15257 . Commercially available peroxidases include GuardzymeTM and NovozymTM 51004 (Novozymes A/S).
  • Any enzyme present in the detergent particle may be stabilized using conventional stabilizing agents, e.g., a polyol such as propylene glycol or glycerol, a sugar or sugar alcohol, lactic acid, boric acid, or a boric acid derivative, e.g., an aromatic borate ester, or a phenyl boronic acid derivative such as 4-formylphenyl boronic acid, and the composition may be formulated as described in e.g. WO 92/19709 and WO 92/19708 .
  • a polyol such as propylene glycol or glycerol
  • a sugar or sugar alcohol lactic acid, boric acid, or a boric acid derivative, e.g., an aromatic borate ester, or a phenyl boronic acid derivative such as 4-formylphenyl boronic acid
  • alkyl groups are sufficiently long to form branched or cyclic chains, the alkyl groups encompass branched, cyclic and linear alkyl chains.
  • the alkyl groups are preferably linear or branched, most preferably linear.
  • Sequesterants may be present in the coated detergent particles.
  • a process for preparing the detergent particle according to the first aspect preferably including the steps of:
  • the coating material is an inorganic salt more preferably selected from sodium carbonate and/or sodium sulphate.
  • the perfume layer is preferably applied by spraying the perfume oil or the perfume in encapsulate form in a coating mixer onto the pre-coated detergent particle.
  • the coating mixer may be any of a number of mixers including low speed mixers and drum mixers.
  • the extruder provides further opportunities to blend in ingredients other than surfactants, or even to add further surfactants.
  • all of the anionic surfactant, or other surfactant supplied in admixture with water; i.e. as paste or as solution, is added into the drier to ensure that the water content can then be reduced and the material fed to and through the extruder is sufficiently dry.
  • Additional materials that can be blended into the extruder are thus mainly those that are used at very low levels in a detergent composition: such as fluorescer, shading dye, enzymes, perfume, silicone antifoams, polymeric additives and preservatives.
  • Solid additives are generally preferred. Solid particulate structuring (liquid absorbing) materials or builders, such as zeolite, carbonate, silicate are preferably not added to the blend being extruded. These materials are not needed due to the self-structuring properties of the very dry LAS-based feed material. If any is used the total amount should be less than 5 wt%, preferably less than 4 wt%, most preferably less than 3 wt%.
  • the inorganic particulate material is added for a different purpose, for instance as a flow aid to improve the feed of particles to the extruder.
  • the output from the extruder is shaped by the die plate used.
  • the extruded material has a tendency to swell up in the centre relative to the periphery.
  • the next step involves coating the extruded core by applying 5 to 40 wt% of a coating material to form a coating material layer and preferably drying it. Coating allows the particles to be coloured easily. Coating makes the particles more suitable for use in detergent compositions that may be exposed to high humidity for long periods.
  • the extruded particles can be considered as oblate spheroids with a major radius "a" and minor radius "b".
  • a detergent formulation including 50 to 100wt% detergent particle according to the present invention.
  • the detergent formulation is preferably present in a package.
  • the package for commercial sale includes 0.01 kg to 5 kg, preferably 0.02 kg to 2 kg and most preferably 0.5 kg to 2 kg of the detergent formulation.
  • the detergent particle of the present invention includes all the ingredients required in a fully formulated detergent formulation in which case the detergent formulation includes 100wt% of the detergent particle.
  • the detergent particle of the present invention may be admixed with additional ingredients, such as bleaching agents, enzymes, perfumes, non-coated detergent particles, and various other ingredients to produce a fully formulated detergent composition.
  • additional ingredients such as bleaching agents, enzymes, perfumes, non-coated detergent particles, and various other ingredients to produce a fully formulated detergent composition.
  • at least 50wt% the detergent particle more preferably at least 60wt%, still preferably at least 70wt% and further preferably at least 80wt% of the detergent particle is present the detergent formulation.
  • Example 1 Comparative detergent particle having perfume incorporated in the core
  • Core manufacture Surfactant raw materials were dried in a spray-drier to produce a spray-dried powder having anionic surfactant and non-ionic surfactant.
  • the spray-dried powder was fed to a twin-screw co-rotating extruder fitted with a shaped orifice plate and cutter blade to extrude the core particle.
  • perfume at a level of 0.527% was added to achieve a final perfume level of 0.4 % by weight in the full formulation, including coating and additional materials.
  • the perfume included a mixture of free oil and perfume in encapsulated form.
  • the core particle obtained in the previous step was then coated with the coating material by spray deposition.
  • Sodium carbonate was used as the coating material.
  • the core particle was charged to the fluidizing chamber of a Strea 1 laboratory fluid bed drier (Aeromatic-Fielder AG) and spray coated with a solution of sodium carbonate using a top-spray configuration to form a coating material layer enveloping the surfactant core.
  • the sodium carbonate solution was fed to the spray nozzle of the Strea 1 via a peristaltic pump (Watson-marlow model 101U/R).
  • the composition of the coating material is given below.
  • the detergent particle obtained by the above process involved the following composition:
  • the perfume concentration in the prepared detergent particle (comparative example 1) was measured immediately after coating using the Gas Chromatography method, the measurement were repeated for 5 different detergent particles prepared in the same batch and the results are tabulated in Table 1.
  • the error in the perfume oil measurement was ⁇ 0.03%.
  • the total loss during the preparation of the detergent particle were calculated by determining the actual theoretical level of perfume in the coated particle given the coating level achieved and then calculating the percentage remaining by dividing the measured value by the theoretical value and the loss is then calculated. The data obtained are provided in Table 1.
  • Table 1 Samples Measured total perfume wt% present in detergent particle according to Example 1 Total perfume (wt%) added in each detergent particle according to Example 1 Measured coating level for sample Total perfume Losses (wt%) 1 0.33 0.527 11.55 41.25 2 0.33 0.527 14.69 39.08 3 0.35 0.527 13.32 36.41 4 0.32 0.527 15.53 40.34 5 0.33 0.527 14.09 39.51 Average loss 39.32
  • table 1 shows that when the perfume is incorporated into the core (as in comparative example 1) which involves the process of extrusion and fluid bed coating post perfume addition, there is an average perfume loss of 39% in the detergent particle, further it was observed that the perfume added in the encapsulated form were ruptured in the detergent particle.
  • Example 2 Detergent particle prepared according to the present invention having a coating with perfume.
  • a core particle was prepared using a process similar to that disclosed in Example 1. The only difference in the process was that in the detergent particle prepared in Example 2 no perfume was added to the extruder during the extrusion process. Therefore there was no perfume in the core of Example 2.
  • the core particle obtained in the previous step was then coated with sodium carbonate solution by spray deposition similar to as explained in Example 1.
  • the intra particle porosity of the detergent particle after the application of the coating was determined using a Quantachrom Helium Pycnometer, Model Ultrapycnometer 1000 and was found to be 0.06 volume fraction.
  • the detergent particle pre-coated with the sodium carbonate layer was then transferred to a drum mixer.
  • a drum mixer To a batch of 300 kg detergent particle in the drum mixer, 2.73 Kg of free oil was sprayed on the detergent particle through a single phase Nozzle 4012 (from Spray systems) at a maximum pressure of 0.5 bar for a period of around 90 seconds and thereafter 1.06 Kg of perfume in encapsulated form was sprayed through an internal atomised twin phase nozzle, SU43 (from spray systems) at an atomizing pressure of 0.8 bar for a period of around 70 seconds. Thereafter mixing was continued for a further 90 seconds before discharging the detergent particle having a coating including sodium carbonate layer and a perfume layer.
  • the perfume content of the detergent particle produced by Example 2 was measured analytically using Gas Chromatography. The perfume content and loss percentage were determined for a sample of 5 different detergent particle prepared in the same batch and the results are provided in Table 2.
  • Table 2 Samples Measured total perfume (wt%) present in detergent particle according to Example 2 Total perfume (wt%) added in each detergent particle according to Example 2 Total perfume Losses (%) 1 1.1 ⁇ 4% 1.04 0 2 1.0 ⁇ 4% 1.04 4% 3 1.1 ⁇ 4% 1.04 0 4 1.1 ⁇ 4% 1.04 0
  • detergent particle having a composition according to the present invention (Example 2) having a coating with free oil and perfume in encapsulated form did not shown significant perfume loss and SEM analysis showed that the perfume in encapsulated form was predominantly intact.
  • Example 3 Determining the flow rate of the inventive detergent particle:
  • the flow rate (or CDFR) of the detergent particle of Example 2 was determined by the following method. A sample of the detergent particle was placed in a glass tube having a diameter of 59.5 millimetre and the time taken for a fixed volume (718.78 ml) to flow out of an orifice having a diameter of 40 millimeters was measured and the flow rate was then calculated in mL/s and provided in Table 3. Table 3 Week 12 CDFR (ml/s) at Trial No Day 0 CDFR (ml/s) 20°C 37°C 45°C 1 465 480 498 477 2 470 497 488 477 3 493 475 505 486 4 476 499 505 486

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

Claims (15)

  1. Particule de détergent présentant un noyau et un revêtement enveloppant le noyau, ladite particule de détergent présentant des dimensions perpendiculaires x, y et z, dans laquelle x est de 0,2 à 2 mm, y est de 2 à 8 mm, et z est de 2 à 8 mm et la particule comprend :
    i. de 20 à 39 % en masse de tensioactif ;
    ii. de 5 à 40 % en masse de matériau de revêtement ; et,
    iii. du parfum ;
    dans laquelle le noyau comprend de 95 parties à 100 parties de la teneur totale en tensioactif et le revêtement comprend de 95 parties à 100 parties du matériau de revêtement et du parfum et dans laquelle la particule de détergent présente une porosité intra-particule dans l'intervalle de 0 à 0,2 de fraction de volume.
  2. Particule de détergent selon la revendication 1, dans laquelle le matériau de revêtement est un matériau inorganique, de préférence un sel inorganique choisi parmi le carbonate de sodium, sulfate de sodium ou des mélanges de ceux-ci.
  3. Particule de détergent selon la revendication 1 ou 2, dans laquelle le matériau de revêtement forme une couche recouvrant le noyau et le parfum forme une couche recouvrant au moins une portion d'une surface externe de la couche de matériau de revêtement.
  4. Particule de détergent selon l'une quelconque des revendications précédentes, dans laquelle la couche de parfum comprend de l'huile libre, du parfum dans une forme encapsulée ou des mélanges de ceux-ci.
  5. Particule de détergent selon la revendication 4, dans laquelle la couche de parfum est multicouche comprenant une couche de parfum dans une forme encapsulée recouvrant une couche d'huile libre.
  6. Particule de détergent selon la revendication 5, dans laquelle la couche d'huile libre de la couche de parfum multicouche est proximale et recouvre une surface externe de ladite couche de matériau de revêtement.
  7. Particule de détergent selon l'une quelconque des revendications précédentes, dans laquelle le tensioactif est choisi parmi un tensioactif anionique, tensioactif non-ionique ou des mélanges de ceux-ci.
  8. Particule de détergent selon la revendication 7, dans laquelle la teneur totale en tensioactif de la particule de détergent comprend de 15 à 85 parties de tensioactif anionique et de 5 à 75 parties de tensioactif non-ionique.
  9. Particule de détergent selon l'une quelconque des revendications précédentes, dans laquelle la particule comprend de 0,001 % en masse à 3 % en masse de parfum.
  10. Particule de détergent selon l'une quelconque des revendications précédentes, dans laquelle les particules de détergent sont des sphéroïdes aplatis.
  11. Particule de détergent selon l'une quelconque des revendications précédentes, dans laquelle la quantité de revêtement sur chaque particule est de 5 % en masse à 45 % en masse, de préférence de 5 % en masse à 15 % en masse de la particule.
  12. Particule de détergent selon l'une quelconque des revendications précédentes, dans laquelle la particule comprend de 0 à 15 % en masse d'eau, de préférence de 1 à 5 % en masse d'eau.
  13. Particule de détergent selon l'une quelconque des revendications précédentes, dans laquelle le noyau de la particule de détergent est un extrudé.
  14. Formulation de détergent comprenant la particule de détergent selon l'une quelconque des revendications 1 à 12 précédentes, dans laquelle la particule de détergent comprend de 50 à 100 % en masse de la formulation de détergent dans un emballage.
  15. Formulation de détergent selon la revendication 14, dans laquelle d'au moins 90 à 100 % des particules de détergent dans les dimensions x, y et z se trouvent dans une variable de 20 % de la particule de détergent revêtue la plus large à la plus petite.
EP18729125.7A 2017-06-20 2018-06-07 Compositions de détergents particulaires comprenant un parfum Active EP3642319B1 (fr)

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PCT/EP2018/065056 WO2018234056A1 (fr) 2017-06-20 2018-06-07 Composition détergente particulaire comprenant un parfum

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CN110785481A (zh) 2020-02-11

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