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
  • C11D3/39—Organic or inorganic per-compounds
  • C11D3/3947—Liquid compositions
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
  • C11D17/0026—Structured liquid compositions, e.g. liquid crystalline phases or network containing non-Newtonian phase

Definitions

• the present invention relates to liquid detergent compositions which contain a peroxygen bleach compound.
• the present invention relates to an aqueous structured liquid detergent composition
• an aqueous structured liquid detergent composition comprising one or more detergent active materials and a peroxygen bleach compound, said detergent composition showing less than 25% volume increase, preferably less than 10 %, more preferred less than 5 % while stored at a temperature of between 20 and 37°C for three months after preparation.
• the detergent composition comprises less than a structure destabilizing amount, more preferably less than 10% by weight of a water miscible organic solvent.
• the present invention is concerned with structured liquid detergent compositions, such structured liquids can be "internally structured” whereby the structure is formed by primary ingredients and/or they can be structured by secondary additives such as certain cross-­linked polyacrylates or clays, which can be added as "external structurants" to compositions of the invention.
• Such structuring is very well known in the art and may be deliberately brought about to endow properties such as consumer preferred flow properties and/or turbid appearance.
• Many structured liquids are also capable of suspending particulate solids such as detergency builders and abrasive particles.
• lamellar droplets are called "spherulites".
• the presence and identity of a surfactant structuring system in a liquid may be determined by means known to those skilled in the art for example, optical techniques, various rheometrical measurements, x-ray or neutron diffraction, and sometimes, electron microscopy.
• Electrolyte may be only dissolved in the aqueous continuous phase or may also be present as suspended solid particles. Particles of solid materials which are insoluble in the aqueous phase may be suspended alternatively or in addition to any solid electrolyte particles.
• the suspended solid can comprise suspended solids which are substantially the same as the dissolved electrolyte, being an excess of same beyond the solubility limit. This solid is usually present as a detergency builder, i.e. to counteract the effects of calcium ion water hardness in the wash.
• the suspended solid usually comprises a particulate abrasive, insoluble in the system. In that case the electrolyte, present to contribute to the structuring of the active material in the dispersed phase, is generally different from the abrasive compounds. In certain cases, the abrasive can however comprise partially soluble salts which dissolve when the product is diluted.
• the structure is usually used for thickening the product to give consumer-preferred flow properties, and sometimes to suspend pigment particles.
• compositions of the first kind are described in for example our patent specification EP-A-38,101 whilst examples of those in the second category are described in our specification EP-104,452.
• Those in the third category are for example, described in US 4,244,840.
• the dispersed structuring phase in these liquids is generally believed to consist of an onion-life configuration comprising concentric bilayers of detergent active molecules, between which is trapped water (aqueous phase).
• aqueous phase trapped water
• These configurations of active material are sometimes referred to as lamellar droplets. It is believed that the close-packing of these droplets enables the solid materials to be kept in suspension.
• the lamellar droplets are themselves a sub-set of lamellar structures which are capable of being formed in detergent active/aqueous electrolyte systems.
• detergent compositions of the lamellar droplet type are preferred.
• compositions according to the present invention comprise a peroxygen bleach.
• This bleach component may be present in the system in solubilized form, but also possible is that only part of the peroxygen bleach is solubilized, the remaining part being present as solid peroxygen particles which are suspended in the system.
• peroxygen compounds examples include hydrogen peroxide, the perborates, persulfates, peroxy disulfates, perphosphates and the crystalline peroxyhydrates formed by reacting hydrogen peroxide with urea or alkali metal carbonate.
• encapsulated bleaches may be used. Preferred bleaches are only partially soluble in the system such as for example diperoxydodecandioic acid (DPDA) or other peracid crystals and perboratetetrahydrate.
• DPDA diperoxydodecandioic acid
• the bleach component is preferably added in an amount corresponding to 0.1 to 15% by weight of active oxygen, more preferred from 0.5 to 5% active oxygen, typically from 1.0 to 3.0 % active oxygen.
• the bleach ingredients may for example be added to the composition as a dry particulate material or as a predispersion of bleach particles. If perborate­tetrahydrate bleaches are used, a suitable commercial available bleach dispersion is Proxsol (ex ICI), alternatively perborate-tetrahydrate crystals may be formed in-situ for example as described in EP 294 904.
• the detergent active materials in general, may comprise one or more surfactants, and may be selected from anionic, cationic, nonionic, zwitterionic and amphoteric species, and (provided mutually compatible) mixtures thereof.
• surfactants may be chosen from any of the classes, sub-classes and specific materials described in "Surface Active Agents” Vol. I, by Schwartz & Perry, Interscience 1949 and “Surface Active Agents” Vol. II by Schwartz, Perry & Berch (Interscience 1958), in the current edition of "McCutcheon's Emulsifiers & Detergents” published by the McCutcheon division of Manufacturing Confectioners Company or in Tensid-Taschenburch", H. Stache, 2nd Edn., Carl Hanser Verlag, Munchen & Wien, 1981.
• Suitable nonionic surfactants 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.
• Specific nonionic detergent compounds are alkyl (C6-C18) primary or secondary linear or branched alcohols with ethylene oxide, and products made by condensation of ethylene oxide with the reaction products of propylene oxide and ethylenediamine.
• Other so-called nonionic detergent compounds include long chain tertiary amine oxides, long chain tertiary phosphine oxides and dialkyl sulphoxides.
• salting-out resistant active materials such as for example described in EP 328 177, especially the use of alkyl polyglycoside surfactants, such as for example disclosed in EP 70 074.
• the level of nonionic surfactants is more than 1 % by weight of the composition, preferably from 2.0 to 20.0 %.
• Suitable anionic surfactants 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 (C8-C18) alcohols produced for example from tallow or coconut oil, sodium and potassium alkyl (C9-C20) benzene sulphonates, particularly sodium linear secondary alkyl (C10-C15) benzene sulphonates; sodium alkyl glyceryl ether sulphates, especially those ethers of the higher alcohols derived from tallow or coconut oil and synthetic alcohols derived from petroleum; sodium coconut oil fatty monoglyceride sulphates and sulphonates; sodium and potassium salts of sulphuric acid esters of higher (C8-C18) fatty alcohol-alkylene oxide, particularly ethylene oxide, reaction products; the reaction products of fatty acids such as coconut fatty acids esterified with isethionic acid and neutralised with sodium hydroxide; sodium and potassium salts of fatty acid amides of methyl taurine; alkane monos
• the level of the above mentioned non-soap anionic surfactant meterials is from 1-40 % by weight of the composition.
• the weight ratio of synthetic anionic surfactants to nonionic surfactants is from 10 : 1 to 1 : 10.
• an alkali metal soap of a mono- or di-carboxylic acid especially a soap of an acid having from 12 to 18 carbon atoms, for example oleic acid, ricinoleic acid, and fatty acids derived from castor oil, rapeseed oil, groundnut oil, coconut oil, palmkernel oil, alk(en)yl succinates e.g. dodecyl succinates or mixtures thereof.
• the sodium or potassium soaps of these acids can be used.
• the level of soap in compositions of the invention is form 1 - 40 % by weight of the composition, more preferred from 5 - 25 %.
• the total detergent active material may be present at from 2% to 60% by weight of the total composition, for example from 5% to 40% and typically from 10% to 30% by weight.
• one preferred class of compositions comprises at least 20%, most preferably at least 25% and especially at least 30% of detergent active material based on the weight of the total composition.
• compositions according to the invention are preferably physically stable in,that they yield no more than 2% by volume phase separation when stored at 25°C for 21 days from the time of preparation. Especially preferred are compositions which do not yield any phase separation upon storage for 21 days at 25 o C.
• compositions according to the invention preferably have solid-suspending properties in that they yield less than 5% by volume of sediment after storage for 21 at 25°C, more preferably less than 2 % by volume sediment is formed, most preferably substantially no visible sediment is formed.
• compositions according to the invention comprise less than a structure destabilising amount of water miscible solvent, preferably less than 10% by weight, for example less than 7.5%, more preferred less than 5%, especially preferred less than 2.0%, typically less than 0.5% by weight of a water miscible solvent.
• water-miscible solvents examples include lower aliphatic monoalcohols, ethers of diethylene glycol and lower monoaliphatic monoalcohols, and mixtures thereof.
• Liquid detergent compositions according to the invention are volume stable in that they show less than 25% preferably less than 10%, more preferably less than 5% volume increase during storage at a temperature between 20 and 37°C for a period of three months after preparation.
• liquid detergent compositions according to the invention will be stored in closed bottles, say of 1.5 litre, which optionally may include venting means, for releasing generated oxygen.
• a solid peroxygen bleach component When a solid peroxygen bleach component is present in an aqueous system, generally part of the bleach material will be solubilized in the form of peracid and/or hydrogen peroxide in the aqueous phase.
• One of the problems often observed in such systems is the occurence of oxygen evolution, due to the decomposition of this peracid or hydrogen peroxide into acid and/or water and oxygen. The oxygen bubbles formed may either emerge from the liquid or be trapped in the liquid, thereby causing a volume increase.
• a similar oxygen evolution is observed when the bleach component such as for instance hydrogen peroxide is totally solubilized in the system.
• the present invention provides liquid detergent compositions wherein the volume increase is kept at an acceptable level of less than 25%, preferably less than 10% , more preferred less than 5 %. during storage of the composition at a temperature between 20 and 37°C for three months after preparation.
• the parameters to be varied in the composition to bring about the desired volume stability effect may for example be the pH, the physical state of the undissolved bleach particles when present, the amount of dissolved bleach, the presence of stabilising agents, the amount of dissolved bleach activators, the viscosity of the product directly after preparation, the presence of viscosity reducing polymers, the presence of gas bubbles in the composition directly after preparation and the presence of antifoam agents.
• the choice of an optimum value of these parameters is dependant on the nature and the choice of the active materials which are present in the composition.
• the half life time of the solubilized peracid or hydrogen peroxide should preferably be increased for increasing the volume stability of the composition. Not only the amount of oxygen formed per time unit is less by increasing the stability of the peracid or hydrogen peroxide, also -and this has been found more important- an increase in the life time of these compounds will allow the oxygen bubbles to be formed upon decomposition of the peracid or hydrogen peroxide to grow in size. An increase in the size of the bubbles to be formed is considered advantageous in that these larger bubbles have been found to be less prone to contribute to the volume increase of the liquid detergent composition, in other words they tend to escape from the liquid rather than being suspended into the system.
• the half-life time of the hydrogen peroxide or peracid is be more than 3 weeks preferably more than 6 weeks at 37°C at the conditions in the detergent composition, preferably more than 8 weeks especially preferred more than 10 weeks. Most preferred between 10 and 20 weeks.
• the stability of the peracid or hydrogen peroxide may be increased in several ways such as for instance a decrease in pH of the composition. It has been found that the volume stability of the liquid detergent composition increases by decreasing the pH of the composition. Therefore, for the purpose of formulation volume stable compositions it is preferred to avoid the use of excessive high pH values.
• the pH of the detergent compositions is less than 12, more preferred less than 11.5, especially preferred between between 6.5 and 11, typically from 7 to 10.
• the volume stability of the detergent compositions according to the present invention can be improved by using bleach particles which are encapsulated.
• These encapsulated bleach particles constitute part or all of the bleach present in the composition, the particles are mainly present in the composition in undissolved form.
• bleach particles in undissolved form is also preferred when the bleach particles are not encapsulated. Higher levels of undissolved bleach are preferred, because it is believed that bleach instability is mainly instability of dissolved bleach. Preferably at least 10% by weight, more preferably at least 30%, especially preferred more than 50%, most preferably more than 75 % or even more than 90 % by weight of the bleach is present in undissolved form. If perborate bleaches are used it has been found that the amount of dissolved bleach is reduced if the pH of the composition is relatively high say from 7-11, more preferably from 7.5 to 10.
• the weight average diameter of the undissolved bleach particles is from 0.5 to 100 micrometer, especially 5 to 60 micrometer.
• a method for obtaining these small particles is described in EP 294 904.
• One way of ensuring that the bleach is present in undissolved form is to increase the amount of electrolyte in the composition, therewith reducing the solubility of the bleach component in the system.
• Suitable electrolytes for this purpose are for instance the at least partially water soluble carbonate, sulphate and halogenide salts and metaborate.
• Other preferred electrolytes are salting out electrolytes.
• salting out electrolyte has the same meaning as in EP 79 646, namely those electrolytes which have a lyotropic number of less than 9.5.
• salting out electrolytes are water-­soluble builder salts, such as alkali metal ortho- and pyroposphates, the alkali metal tripolyphosphates, such as sodium tripolyposphate, the alkali metal silicates, - borates, -carbonates, -sulphates, alkali metal citrates; alkali metal salts of nitriloacetate; alkali metal salts of carboxymethoxy succinate.
• the alkali metal salts the ammonium salts can be used.
• Particularly preferred is the use of sodium tripolyphosphate and or sodium (di)silicate as the salting out electrolyte.
• the dissolved part of the electrolyte constitutes preferably more than 2 % by weight of the composition, more preferred more than 5% by weight, especially preferred between 10 and 50 % by weight.
• the compositions according to the present invention also comprise a stabilising agent for the bleach component.
• Suitable stabilisers are well-known in art and include EDTA, Magnesium silicates and phosphonates such as for instance the Dequest range ex Monsanto and Naphthol ex Merck.
• the amount of stabilising agent is from 0.05 to 5 % by weight of the composition, more preferred from 0.05 to 1% of the composition.
• compositions of the present invention may comprise one or more bleach activator agents. These materials when combined with a peroxy bleach in the wash, will activate hydrogen peroxide at a low temperature of from 15 to 55°C therewith allowing the effective use of peroxide bleaches at low washing temperatures.
• the bleach activators used in the present invention often also referred to as peroxyacid bleach precursors are conventionally organic compounds having one or more reactive acyl groups, which at relatively low temperature react with hydrogenperoxide causing the formation of organic peroxyacids, the latter providing for a more effective bleaching action at lower temperatures than hydrogen peroxide itself.
• N,N,N,N′-tetraacyl ethylene diamine normally referred to as TAED.
• Another well-known bleach activator is sodium-4-benzoyl oxybenzene sulphonate normally referred to as BOBS, as disclosed in GB 836,988.
• organic bleach activators are other n-acyl substituted amides, for example tetraacetyl methylene diamine; carboxylic acid anhydrides for example succinic, benzoic and phthalic anhydrides; carboxylic acid esters, for example sodium acetoxy benzene sulphonate; acetates such as glycerol­triacetate, glucose pentaactetate and xylose­tetraacetate and acetyl salicylic acid.
• carboxylic acid anhydrides for example succinic, benzoic and phthalic anhydrides
• carboxylic acid esters for example sodium acetoxy benzene sulphonate
• acetates such as glycerol­triacetate, glucose pentaactetate and xylose­tetraacetate and acetyl salicylic acid.
• TAED is used as the bleach activator.
• the preferred level of bleach activator in the liquid detergent is from 0.1 to 10 % by weight preferably from 0.5 to 5 % by weight of the compositions
• the bleach activator is present in the system in at least partly undissolved form.
• One way of ensuring that the activator is present in undissolved form is the use of encapsulated activator materials.
• Another method is to increase the amount of electrolyte in the composition, therewith reducing the solubility of the activator in the system.
• Suitable electrolytes for this purpose are for instance the at least partially water soluble carbonate, sulphate and halogenide salts and metaborate.
• Other preferred electrolytes are salting out electrolytes as defined hereabove.
• the dissolved part of the electrolyte constitutes preferably more than 2 % by weight of the composition, more preferred more than 5% by weight, especially preferred between 10 and 50 % by weight.
• the viscosity of the product directly after preparation it has been found that a lower value for the viscosity generally increases the volume stability of the bleach containing product. Also for lower viscosities are genrally preferred by the consumer. However, for providing solid-suspending properties, low viscosities should preferably be avoided. Therefore in selecting the most appropriate viscosity of the product, a balance should be sought between better stability and consumer-acceptance at lower viscosities and increased solid suspending properties at higher viscosities.
• the viscosity is preferably less than 2,000 mPas at 21 s ⁇ 1, more preferred less than 1,500, most preferred between 20 and 1,000, especially preferred from 30 to 500.
• the viscosity is more than 1,000 mPas at 10 ⁇ 4 s ⁇ 1, more preferred more than 10,000, especially preferred more than 100,000.
• the techniques for obtaining the initial viscosity as desired are well-known in the art, and include for example the appropriate choice of active ingredients, the adaptation of the level of dissolved electrolyte and the inclusion of viscosity modifying agents.
• a preferred way for regulating the viscosity of the product is the inclusion of polymers in the composition.
• Viscosity and/or stability regulating polymers which are preferred for incorporation in compositions according to the invention include deflocculating polymers e.g those having a hydrophilic backbone and at least one hydrophobic side chain. Such polymers are described in our copending British patent applications 8813978.7 (corresponding to EP 346 995), 8924479.2, 8924478.4 and 8924477.6.
• the amount of viscosity regulating polymer, especially deflocculating polymers is from 0.1 to 5% by weight of the total composition, more preferred from 0.2 to 2%.
• gas bubbles in the detergent composition As to the presence of gas bubbles in the detergent composition according to the invention, it has been found that both the size and the level of gas bubbles are important parameters for determining the volume stability of the composition. Generally gas bubbles in the form of air or oxygen bubbles are introduced into liquid detergent compositions during processing of the composition, which usually involves a mixing stage.
• the volume fraction of gas bubbles is less than 5.0%, preferably less than 3.5%, most preferred less than 2.0%, especially less than 1 % or even less than 0,5 %.
• the average diameter of the gas bubbles is above 0.25 mm, more preferred above 0.4 mm, most preferred above 0.5 mm.
• an antifoam agent both reduces the volume fraction of gas bubbles and increases the size of the bubbles present.
• the antifoam agents are added at a level above the level commonly used for foam reduction of detergent compositions.
• the level of antifoam agent is more than 0.2% of the detergent composition, more preferred more than 0.3% of the composition, especially preferred from 0.4 to 2.0% of the composition.
• Suitable antifoam agents include silicone antifoam agents, such as dimethyl polysiloxanes and/or silica particles.
• the aqueous continuous phase contains dissolved electrolyte.
• electrolyte means any ionic water soluble material.
• the electrolytes may be used, with one or more of the electrolytes being in the dissolved aqueous phase and one or more being substantially only in the suspended solid phase.
• Two or more electrolytes may also be distributed approximately proportionally, between these two phases. In part, this may depend on processing, e.g.
• salts includes all organic and inorganic materials which may be included, other than surfactants and water, whether or not they are ionic, and this term encompasses the sub-set of the electrolytes (water soluble materials).
• compositions optionally also contain electrolyte in an amount sufficient to bring about structuring of the detergent active material.
• the compositions contain from 1% to 60%, especially from 10 to 45% of a salting-out electrolyte.
• Salting-out electrolyte has the meaning ascribed to in specification EP-A-79 646.
• some salting-in electrolyte (as defined in the latter specification) may also be included, provided it is of a kind and in an amount compatible with the other components and the composition is still in accordance with the definition of the invention claimed herein.
• Some or all of the electrolyte may have detergency builder properties.
• compositions according to the present invention include detergency builder material, some or all of which may be electrolyte.
• the builder material is any material capable of reducing the level of free calcium ions in the wash liquor and will preferably provide the composition with other beneficial properties such as the generation of an alkaline pH, the suspension of soil removed from the fabric.
• Examples of phosphorous-containing inorganic detergency builders when present, include the water-soluble salts, especially alkali metal pyrophosphates, orthophosphates, polyphosphates and phosphonates.
• Specific examples of inorganic phosphate builders include sodium and potassium tripolyphosphates, phosphates and hexametaphosphates. Phosphonate sequestrant builders may also be used. Sometimes, however, it is preferred to minimise the amount of phosphorous-containing builders.
• non-phosphorus-containing inorganic detergency builders when present, include water-­soluble alkali metal carbonates, bicarbonates, silicates and crystalline and amorphous aluminosilicates. Specific examples include sodium carbonate (with or without calcite seeds), potassium carbonate, sodium and potassium bicarbonates, silicates and zeolites.
• organic detergency builders when present, include the alkaline metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates, polyacetyl carboxylates and polyhydroxysulphonates. Specific examples include sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylenediaminetetraacetic acid, nitrilitriacetic acid, oxydisuccinic acid, melitic acid, benzene polycarboxylic acids, CMOS, tartrate mono succinate, tartrate di succinate and citric acid.
• compositions of the present invention alternatively, or in addition to the partly dissolved polymer, yet another polymer which is substantially totally soluble in the aqueous phase and has an electrolyte resistance of more than 5 grams sodium nitrilotriacetate in 100ml of a 5% by weight aqueous solution of the polymer, said second polymer also having a vapour pressure in 20% aqueous solution, equal to or less than the vapour pressure of a reference 2% by weight or greater aqueous solution of polyethylene glycol having an average molecular weight of 6000; said second polymer having a molecular weight of at least 1000.
• Use of such polymers is generally described in our EP 301,883.
• the level of non-soap builder material is from 5-50 % by weight of the composition, more preferred from 5 to 35 %.
• compositions of the present invention contain low levels or are substantially free from hydrotropes.
• hydrotrope any water soluble agent which tends to enhance the solubility of surfactants in aqueous solution.
• lather boosters such as alkanolamides, particularly the monoethanolamides derived from palm kernel fatty acids and coconut fatty acids, fabric softeners such as clays, amines and amine oxides, lather depressants, inorganic salts such as sodium sulphate, and, usually present in very minor amounts, fluorescent agents, perfumes, enzymes such as proteases, amylases and lipases (including Lipolase (Trade Mark) ex Novo), germicides and colourants.
• lather boosters such as alkanolamides, particularly the monoethanolamides derived from palm kernel fatty acids and coconut fatty acids
• fabric softeners such as clays, amines and amine oxides
• lather depressants inorganic salts such as sodium sulphate
• fluorescent agents perfumes
• enzymes such as proteases, amylases and lipases (including Lipolase (Trade Mark) ex Novo), germicides and colourants.
• compositions of the invention may be prepared by any conventional method for the preparation of liquid detergent compositions.
• a preferred method involves the dispersing of the electrolyte (non-builder) -if any- together with the minor ingredients except for the temperature sensitive ingredients -if any- in water of elevated temperature, followed by the addition of the builder material -if any-, the detergent active materials (optionally as a pre-mix) under stirring and thereafter cooling the mixture and adding any temperature sensitive minor ingredients such as enzymes or perfumes and the bleach.
• the deflocculating polymer -­if any- may for example be added after the elctrolyte ingredient or as the final ingredient.
• perborate monohydrate When perborate monohydrate is used as the bleaching agent, it may be preferred to cool the final product to a temperature just above the freezing point, in order to accelerate the recrystallisation of the perborate in tetrahydrate form.
• liquid detergent compositions of the invention will generally be diluted with wash water to form a wash liquor, which may be used for detergency purposes, for example for the washing process in a washing machine.
• concentration of liquid detergent composition in the wash liquor is preferably from 0.1 to 10 % by weight, more preferred from 0.1 to 3 %.
• a basic liquid detergent composition of the following composition was prepared by addition under stirring of the components in the order listed. Na-Dobs was formed in-situ by combining NaOH and Dobs-acid. Some of the processing water was left behind because the hydrogen peroxide solution used was 27 weight % active. TABLE 1 % by weight Water balance Na-Dobs 13.8 Synperonic 7 4.0 Dequest 2060 0.1 X-Naphtol 0.2 STP thermphos NW 8.6 H2O2 (100%) 5.0 pH1) 7.9-8.1 1) pH adjusted with NaOH if necessary. TABLE 2a Raw material specification Component Supplier Dobs-acid (98%), Marlon AS-3 Hüls Synperonic 7 I.C.I. Dequest 2060 Monsanto X-Naphtol, (p.a.) Merck STP, thermphos NW Hoechst H2O2, 27% Brocacef
• the basic detergent composition according to example 1 was prepared in several versions of different viscosity direct after preparation.
• Composition A has a ratio Na-Dobs to Synperonic of 0.74:0.26 and a viscosity of 170 mPas at 21 s ⁇ 1
• composition B had a ratio Na-Dobs to Synperonic of 0.75:0.25 and a viscosity of 390 mPas
• composition C had a ratio Na-Dobs to Synperonic of 0.78:0.22 and a viscosity of 1000 mPas.
• the compositions were stored at 37°C.
• Composition A showed in the first two days of storage a slight volume increase of about 2% by volume, after 2 two days the volume in decreased to a volume which was about 1% less than the volume of the composition directly after preparation.
• Composition B showed a sharp volume increase of about 50% by volume in the first three days of storage, followed by a reduction of the volume until at the 5th day the composition had approximately its original volume.
• Composition C showed during the first 7 days a sharp volume increase of more than 125% by volume (overfoam), a reduction of volume to the original volume of the composition was observed after 15 days.
• This example illustrates that by lowering the viscosity of the composition, the volume stability of detergent compositions containing solubilized hydrogen peroxide can be increased.
• Example 1 was prepared by the method as indicated in example 1, with some small modifications.
• Composition D was prepared according to example 1, the ratio Na-Dobs to Synperonic was 0.77:0.23.
• Composition E was prepared as composition D, but 0.1% of silicone antifoam was added (corresponding to 0.33 % DB31 ex Dow Corning) before mixing the ingredients.
• Composition F was prepared as composition D, but the composition was deaerated by centrifuging for 5 min at 4000 G.
• Composition G was prepared as composition D, but 0.33% of DB31 was added and the composition was de-aerated by centrifuging for 5 min at 4000 G.
• the viscosity of compositions D-G was 860 mPas after preparation. The compositions were stored at room temperature and the volume increase and the bubble size were monitored.
• Composition D showed a linear increase in volume up to a maximum of about 75% volume increase after 30 days of storage.
• the diameter of the gas bubbles present during this period showed a similar increase from very small (about o.1 mm) to about 1.5 mm after 30 days.
• the volume of the compositions decreased gradually until the composition was back at its original volume after 60 days.
• the bubble diameter stayed constant at a value of 1.5 mm during this period.
• Composition E showed a linear increase in volume up to a maximum value of about 55% volume increase after 30 days of storage.
• the diameter of the gas bubbles present during this period showed a similar increase from very small (around 0.25 mm) to about 1.8 mm after 30 days.
• the volume of the composition decreased gradually until the composition was back at its original volume after about 60 days.
• Composition F showed an increase in volume during the first 7 days to a maximum value of about 10% by volume. After 7 days the volume increase decreased to a value of about 0% and remained constant during 60 days of storage. The diameter of the gas bubbles present during this period remained substantially constant at about 1.5 mm.
• Composition G did not show a substantial increase in volume during storage for 60 days.
• the diameter of the gas bubbles present during this period showed an increase from 1 mm to 1.8 mm in the first 10 days of storage, and then remained constant during the remaining of the period.
• This example illustrates that both the presence of an antifoam agent and/or the de-aeration of the composition contribute positively to the stability of the liquid detergent composition.
• compositions were prepared according to example 1, with some small modifications.
• Composition H was of the composition of example 1, and had a viscosity of between 400 and 600 mPas, Composition I contained in addition to the components of composition H 0.5% by weight of silicone, corresponding to 1.5 %by weight of DB 31 which was added at the beginning of the mixing process.
• DB 31 %by weight
• Composition H contained 5.2% by volume of gas bubbles, the size of the bubbles was between 0.1 and 0.2 mm.
• Composition I contained 1.9% by volume of gas bubbles, the size of the bubbles was between 0.25 and 0.5 mm.
• compositions were prepared by adding the electrolyte together with the minor ingredients except for the perfume and the enzymes to water of elevated temperature, followed by the addition of the detergent active material as a premix under stirring and thereafter cooling the mixture and adding the enzymes, perfumes and the bleach.
• the obtained products had the following characteristics: 5 6 7 8 Volume stability (% volume increase, 3 months 25 o C) 4 3 0 n.m 6 clear layer separation (3 weeks 37 o ) no no no no no solid sedimentation (3 weeks 37 o C) no no no no no no no no no no no Viscosity 21 s ⁇ 1 1,350 710 800 n.m Viscosity 10 ⁇ 4 s ⁇ 1 ⁇ 200,000 n.m n.m n.m dissolved perborates 5) 3 1.5 8 n.m bleach activity % (2 months ambient T) 99 99 96 n.m enzyme activity % (2 months ambient T)2) 65 62 76 n.m

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• 1990
  • 1990-02-08 DE DE1990633783 patent/DE69033783T2/de not_active Expired - Fee Related
  • 1990-02-08 EP EP90200290A patent/EP0385522B1/de not_active Expired - Lifetime
  • 1990-02-08 ES ES90200290T patent/ES2162785T3/es not_active Expired - Lifetime
  • 1990-02-20 CA CA 2010442 patent/CA2010442C/en not_active Expired - Fee Related
  • 1990-02-22 BR BR9000882A patent/BR9000882A/pt not_active IP Right Cessation
  • 1990-02-23 AU AU50104/90A patent/AU629910B2/en not_active Ceased
  • 1990-02-27 TR TR21290A patent/TR24976A/xx unknown
  • 1990-02-27 JP JP2047106A patent/JPH089719B2/ja not_active Expired - Fee Related

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