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
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
• • 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
  • C11D3/507—Compounds releasing perfumes by thermal or chemical activation

Definitions

• the present invention relates to a process for producing particles of amine reaction product.
• perfumed products are well-known in the art. However, consumer acceptance of such perfumed products like laundry and cleaning products is determined not only by the performance achieved with these products but also by the aesthetics associated therewith. The perfume components are therefore an important aspect of the successful formulation of such commercial products.
• perfume additives make such compositions more aesthetically pleasing to the consumer, and in some cases the perfume imparts a pleasant fragrance to fabrics treated therewith.
• the amount of perfume carried-over from an aqueous laundry bath onto fabrics is often marginal and does not last long on the fabric.
• fragrance materials are often very costly and their inefficient use in laundry and cleaning compositions and ineffective delivery to fabrics results in a very high cost to both consumers and laundry and cleaning manufacturers. Industry, therefore, continues to seek with urgency for more efficient and effective fragrance delivery in laundry and cleaning products, especially for improvement in the provision of long-lasting fragrance to the fabrics.
• the mixing of the amine reaction product with a carrier having specific melting point to form a particle fulfills such a need.
• the obtained particle is thereafter treated to form a coated particle.
• both viscous and non-viscous amine reaction product when processed by the present invention exhibit better deposition and long lasting release than amine reaction product which have not been processed according to this process.
• the mixing with such carrier acts as a shell around the amine reaction product, thus protecting it from the aggressive wash liquor as well as enhancing its fabric deposition properties.
• viscous it is meant a product which has a viscosity higher than 1000 cps.
• the viscosity is measured on a rheometer, TA Instrument CSL 2 100 at a temperature of 25C with a gap setting of 500 microns.
• the carrier for use herein has a melting point, measured at atmospheric pressure, of less than 30°C.
• the present invention is a process for making particles of amine reaction product of a compound containing a primary and/or secondary amine functional group and an active ketone or aldehyde containing component, and which comprises the steps of:
• the processed amine reaction product is further processed to form a coated particle.
• the processed amine reaction product or coated particle is incorporated in a finished composition.
• the amine reaction product for use herein is a product of reaction between a compound containing a primary and/or secondary amine functional group and an active ketone or aldehyde containing component, so called hereinafter "amine reaction product".
• primary and/or secondary amine it is meant a component which carries at least one primary and/or secondary amine and/or amide function.
• the primary and/or secondary amine compound is also characterized by an Odour Intensity Index of less than that of a 1% solution of methyl anthranilate in dipropylene glycol.
• Odour Intensity Index it meant that the pure chemicals were diluted at 1% in Dipropylene Glycol, odor-free solvent used in perfumery. This percentage is more representative of usage levels.
• Smelling strips, or so called “blotters” were dipped and presented to the expert panellist for evaluation. Expert panellists are assessors trained for at least six months in odor grading and whose gradings are checked for accuracy and reproducibility versus a reference on an on-going basis. For each amine compound, the panellist was presented two blotters: one reference (Me Anthranilate, unknown from the panellist) and the sample. The panellist was asked to rank both smelling strips on the 0-5 odor intensity scale, 0 being no odor detected, 5 being very strong odor present.
• a general structure for the primary amine compound of the invention is as follows: B-(NH2) n ; wherein B is a carrier material, and n is an index of value of at least 1.
• Compounds containing a secondary amine group have a structure similar to the above excepted that the compound comprises one or more -NH- groups instead of -NH2. Further, the compound structure may also have one or more of both -NH2 and -NH- groups.
• Preferred B carriers are inorganic or organic carriers.
• inorganic carrier carrier which are non-or substantially non carbon based backbones.
• Preferred primary and/or secondary amines, among the inorganic carriers are those selected from mono or polymers or organic-organosilicon copolymers of amino derivatised organo silane, siloxane, silazane, alumane, aluminum siloxane, or aluminum silicate compounds.
• Typical examples of such carriers are: organosiloxanes with at least one primary amine moiety like the diaminoalkylsiloxane [H2NCH2(CH3) 2Si]O, or the organoaminosilane (C6H5) 3SiNH2 described in: Chemistry and Technology of Silicone, W. Noll, Academic Press Inc. 1998, London, pp 209, 106).
• Preferred primary and/or secondary amines are those selected from aminoaryl derivatives, polyamines, amino acids and derivatives thereof, substituted amines and amides, glucamines, dendrimers, polyvinylamines and derivatives thereof, and/or copolymer thereof, alkylene polyamine, polyaminoacid and copolymer thereof, cross-linked polyaminoacids, amino substituted polyvinylalcohol, polyoxyethylene bis amine or bis aminoalkyl, aminoalkyl piperazine and derivatives thereof, bis (amino alkyl) alkyl diamine linear or branched, and mixtures thereof.
• Preferred aminoaryl derivatives are the amino-benzene derivatives including the alkyl esters of 4-amino benzoate compounds, and more preferably selected from ethyl-4-amino benzoate, phenylethyl-4-aminobenzoate, phenyl-4-aminobenzoate, 4-amino-N'-(3-aminopropyl)-benzamide, and mixtures thereof.
• Preferred polyamines are polyethyleneimines commercially available under the tradename Lupasol like Lupasol FG (MW 800), G20wfv (MW 1300), PR8515 (MW 2000), WF (MW 25000), FC (MW 800), G20 (MW 1300), G35 (MW 1200), G100 (MW 2000), HF (MW 25000), P (MW 750000), PS (MW 750000), SK (MW 2000000), SNA (MW 1000000).
• Preferred amino acids for use herein are selected tyrosine, tryptophane, lysine, glutamic acid, glutamine, aspartic acid, arginine, asparagine, phenylalanine, proline, glycine, serine, histidine, threonine, methionine, and mixture thereof, most preferably selected from tyrosine, tryptophane, and mixture thereof.
• Preferred amino acid derivatives selected from tyrosine ethylate, glycine methylate, tryptophane ethylate, and mixture thereof.
• Preferred substituted amines and amides for use herein are selected from nipecotamide, N-coco-1,3-propenediamine; N-oleyl-1,3-propenediamine; N-(tallow alkyl)-1,3-propenediamine; 1,4-diamino cyclohexane; 1,2-diamino-cyclohexane; 1,12-diaminododecane, and mixtures thereof.
• glucamines preferably selected from 2,3,4,5,6-pentamethoxy-glucamine; 6-acetylglucamine, glucamine, and mixture thereof.
• PAMAM Starburst® polyamidoamines
• amino-functional polymers are selected from the polyvinylamines, derivatives thereof, copolymer thereof, alkylene polyamine, polyaminoacids and copolymer thereof, cross-linked polyaminoacids, amino substituted polyvinylalcohol, polyoxyethylene bis amine or bis aminoalkyl, aminoalkyl piperazine and derivatives, N,N'-bis-(3-aminopropyl)-1,3-propanediamine linear or branched (TPTA), and mixtures thereof.
• Preferred amino-functional polymers for use in the present invention are selected from the polyvinylamines, derivatives thereof, copolymer thereof, alkylene polyamine, polyaminoacids and copolymer thereof, cross-linked polyaminoacids, amino substituted polyvinylalcohol, polyoxyethylene bis amine or bis aminoalkyl, aminoalkyl piperazine and derivatives, N,N'-bis-(3-aminopropyl)-1,3-
• Polyamino acid is one suitable and preferred class of amino-functional polymer.
• Polyaminoacids are compounds which are made up of amino acids or chemically modified amino acids. They can contain alanine, serine, aspartic acid, arginine, valine, threonine, glutamic acid, leucine, cysteine, histidine, lysine, isoleucine, tyrosine, asparagine, methionine, proline, tryptophan, phenylalanine, glutamine, glycine or mixtures thereof.
• chemically modified amino acids the amine or acidic function of the amino acid has reacted with a chemical reagent.
• Preferred polyamino acids are polylysines, polyarginine, polyglutamine, polyasparagine, polyhistidine, polytryptophane or mixtures thereof. Most preferred are polylysines or polyamino acids where more than 50% of the amino acids are lysine, since the primary amine function in the side chain of the lysine is the most reactive amine of all amino acids.
• the preferred polyamino acid has a molecular weight of 500 to 10.000.000, more preferably between 5.000 and 750.000.
• the polyamino acid can be cross linked.
• the cross linking can be obtained for example by condensation of the amine group in the side chain of the amino acid like lysine with the carboxyl function on the amino acid or with protein cross linkers like PEG derivatives.
• the cross linked polyamino acids still need to have free primary and/or secondary amino groups left for reaction with the active ingredient.
• the preferred cross linked polyamino acid has a molecular weight of 20.000 to 10.000.000, more preferably between 200.000 and 2.000.000.
• the polyamino acid or the amino acid can be co-polymerized with other reagents like for instance with acids, amides, acyl chlorides. More specifically with aminocaproic acid, adipic acid, ethylhexanoic acid, caprolactam or mixture thereof.
• the molar ratio used in these copolymers ranges from 1:1 (reagent/ amino acid (lysine)) to 1:20, more preferably from 1:1 to 1:10.
• the polyamino acid like polylysine can be partially ethoxylated.
• polyaminoacids containing lysine, arginine, glutamime, asparagine are given in the Bachem 1996, Peptides and Biochemicals catalog.
• polyaminoacid can be obtained before reaction with the active ingredient, under a salt form.
• polylysine can be supplied as polylysine hydrobromide.
• Polylysine hydrobromide is commercially available from Sigma, Applichem, Bachem and Fluka.
• Suitable amino functional polymers containing at least one primary and/or secondary amine group for the purpose of the present invention are :
• the more preferred compounds are selected from ethyl-4-amino benzoate, polyethyleneimine polymers commercially available under the tradename Lupasol like Lupasol FG, G20,wfv, PR8515, WF, FC, G20, G35, G100, HF, P, PS, SK, SNA; the diaminobutane dendrimers Astramol®, polylysine, cross-linked polylysine, N,N'-bis-(3-aminopropyl)-1,3-propanediamine linear or branched; 1,4-bis-(3-aminopropyl) piperazine, and mixtures thereof.
• ethyl-4-amino benzoate polyethyleneimine polymers commercially available under the tradename Lupasol like Lupasol FG, G20,wfv, PR8515, WF, FC, G20, G35, G100, HF, P, PS, SK, SNA
• Even most preferred compounds are those selected from ethyl-4-amino benzoate, polyethyleneimine polymers commercially available under the tradename Lupasol like Lupasol FG, G20,wfv, PR8515, WF, FC, G20, G35, G100, HF, P, PS, SK, SNA; polylysine, cross-linked polylysine, N,N'-bis-(3-aminopropyl)-1,3-propanediamine linear or branched, 1,4-bis-(3-aminopropyl) piperazine, and mixtures thereof.
• Lupasol like Lupasol FG, G20,wfv, PR8515, WF, FC, G20, G35, G100, HF, P, PS, SK, SNA polylysine, cross-linked polylysine, N,N'-bis-(3-aminopropyl)-1,3-propanediamine linear or branched, 1,4-bis-(3-amin
• such most preferred primary and/or secondary amine compounds also provide fabric appearance benefit, in particular colour appearance benefit, thus providing a resulting amine reaction product with the dual properties of both fabric appearance benefit and delayed release of the active.
• the primary and/or secondary amine compound has more than one free primary and/or secondary amine group, several different active ingredients (aldehyde and/or ketone) can be linked to the amine compound.
• active ketone or active aldehyde it is meant any chain containing at least 1 carbon atom, preferably at least 5 carbon atoms.
• the active ketone or active aldehyde is respectively selected from a flavour ketone or aldehyde ingredient, a pharmaceutical ketone or aldehyde active, a biocontrol ketone or aldehyde agent, a perfume ketone or aldehyde component and mixtures thereof; most preferably a perfume ketone and/or aldehyde.
• Flavour ingredients include spices, flavor enhancers that contribute to the overall flavour perception.
• Pharmaceutical actives include drugs.
• Biocontrol agents include biocides, antimicrobials, bactericides, fungicides, algaecides, mildewcides, disinfectants, sanitiser like bleach, antiseptics, insecticides, insect and/or moth repellant, vermicides, plant growth hormones.
• Typical antimicrobials include Glutaraldehyde, Cinnamaldehyde, and mixtures thereof.
• Typical insect and/or moth repellants are perfume ingredients, such as citronellal, citral, N, N diethyl meta toluamide, Rotundial, 8-acetoxycarvotanacenone, and mixtures thereof.
• Other examples of insect and/or moth repellant for use herein are disclosed in US 4,449,987, 4,693,890, 4,696,676, 4,933,371, 5,030,660, 5,196,200, and "Semio Activity of Flavor and Fragrance molecules on various Insect Species", B.D. Mookherjee et al., published in Bioactive Volatile Compounds from Plants, ASC Symposium Series 525, R. Teranishi, R.G. Buttery, and H. Sugisawa, 1993, pp. 35-48.
• Perfume ketones components include components having odoriferous properties.
• the perfume ketone is selected from buccoxime; iso jasmone; methyl beta naphthyl ketone; musk indanone; tonalid/musk plus; Alpha-Damascone, Beta-Damascone, Delta-Damascone, Iso-Damascone, Damascenone, Damarose, Methyl-Dihydrojasmonate, Menthone, Carvone, Camphor, Fenchone, Alpha-lonone, Beta-lonone, Gamma-Methyl so-called lonone, Fleuramone, Dihydrojasmone, Cis-Jasmone, Iso-E-Super, Methyl-Cedrenyl-ketone or Methyl- Cedrylone, Acetophenone, Methyl-Acetophenone, Para-Methoxy-Acetophenone, Methyl-Beta-Nap
• the preferred ketones are selected from Alpha Damascone, Delta Damascone, Iso Damascone, Carvone, Gamma-Methyl-lonone, Iso-E-Super, 2,4,4,7-Tetramethyl-oct-6-en-3-one, Benzyl Acetone, Beta Damascone, Damascenone, methyl dihydrojasmonate, methyl cedrylone, hedione, and mixtures thereof.
• Perfume aldehyde components include components having odoriferous properties.
• the perfume aldehyde is selected from adoxal; anisic aldehyde; cymal; ethyl vanillin; florhydral; helional; heliotropin; hydroxycitronellal; koavone; lauric aldehyde; lyral; methyl nonyl acetaldehyde; P. T.
• aldehydes are selected from citral, 1-decanal, benzaldehyde, florhydral, 2,4-dimethyl-3-cyclohexen-1-carboxaldehyde; cis/trans-3,7-dimethyl-2,6-octadien-1-al; heliotropin; 2,4,6-trimethyl-3-cyclohexene-1-carboxaldehyde; 2,6-nonadienal; alpha-n-amyl cinnamic aldehyde, alpha-n-hexyl cinnamic aldehyde, P.T. Bucinal, lyral, cymal, methyl nonyl acetaldehyde, trans-2-nonenal, lilial, trans-2-nonenal, and mixture thereof.
• perfume ingredients some are commercial names conventionally known to one skilled in the art, and also includes isomers. Such isomers are also suitable for use in the present invention.
• Odor Detection Threshold should be lower than 1ppm, preferably lower than 10ppb - measured at controlled Gas Chromatography (GC) conditions such as described here below.
• GC Gas Chromatography
• This parameter refers to the value commonly used in the perfumery arts and which is the lowest concentration at which significant detection takes place that some odorous material is present, as referred to for example in "Compilation of Odor and Taste Threshold Value Data (ASTM DS 48 A)", edited by F. A.
• the Odor Detection Threshold is measured according to the following method : The gas chromatograph is characterized to determine the exact volume of material injected by the syringe, the precise split ratio, and the hydrocarbon response using a hydrocarbon standard of known concentration and chain-length distribution. The air flow rate is accurately measured and, assuming the duration of a human inhalation to last 0.02 minutes, the sampled volume is calculated.
• perfume components are those selected from : 2-methyl-2-(para-iso-propylphenyl)-propionaldehyde, 1-(2,6,6-trimethyl-2-cyclohexan-1-yl)-2-buten-1-one and/or para-methoxy-acetophenone.
• the level of active is of from 10 to 90%, preferably from 30 to 85%, more preferably from 45 to 80% by weight of the amine reaction product.
• Preferred amine reaction products are those which have a Dry Surface Odour Index as per given in co-pending application EP 98870155.3 given at page 29, line 26 to page 32 line 29, in which the specified unperfumed base for fabric sufaces and hard surfaces are respectively as follow: Composition for fabric surface test % by weight LAS 16 NaSKS-6 6 PB1 8 TAED 2.4 Carbonate 1 Sodium Carbonate 1 HEDP 0.4 SRP1 0.2 Photobleach 0.013 Citric acid 1.0 Protease 0.3 Lipase 0.1 Cellulase 0.1 Amylase 0.3 Zeolilte 3.0 TFAA 3.0 QAS1 2.5 Silicone antifoam 1.0 Misc/minors to balance to 100% Composition for hard surface test % by weight C12-14 EO 21 2 C12-14 EO 5 2.5 C9-11 EO 5 2.5 LAS 0.8 Na2CO3 0.2 Citric acid 0.8 Caustic acid 0.5 Fatty acid 0.5 SCS 1.5 Water &Misc/Minors to balance to 100%
• Most preferred amine reaction products are those resulting from the reaction of polyethyleneimine polymer like Lupasol polymers, BNPP, or TPTA with one or more of the following Alpha Damascone, Delta Damascone, Carvone, Gamma-Methyl-Ionone, Hedione, Florhydral, Lilial, Heliotropine, and 2,4-dimethyl-3-cyclohexen-1-carboxaldehyde.
• Still other preferred amine reaction products are those resulting from the reaction of Astramol Dendrimers with Carvone as well as those resulting from the reaction of ethyl-4-amino benzoate with one or more of the following 2,4-dimethyl-3-cyclohexen-1-carboxaldehyde, and trans-2-nonenal.
• Still another preferred amine reaction products are those resulting from the reaction of polylysine with one or more of the following Alpha Damascone, Delta Damascone, Carvone, and 2,4-dimethyl-3-cyclohexen-1-carboxaldehyde.
• Even most preferred amine reaction products are those from the reaction of Lupasol HF with Delta Damascone; LupasolG35 with Alpha Damascone; LupasolG100 with 2,4-dimethyl-3-cyclohexen-1-carboxaldehyde, BNPP or TPTA with Alpha and Delta Damascone; ethyl-4-amino benzoate with 2,4-dimethyl-3-cyclohexen-1-carboxaldehyde.
• Most preferred amine reaction products are those fulfilling the Dry Surface Odor Index as per given in co-pending application EP 98870155.3 given at page 29, line 26 to page 32 line 29.
• Another essential ingredient of the process invention is a carrier having a melting point of less than 30°C, preferably between minus 150°C and less than 30°C.
• a carrier having a melting point of less than 30°C, preferably between minus 150°C and less than 30°C.
• Typical of such carrier includes liquid as well as solid carrier material.
• the liquid carrier can be in any suitable physical form like hydrophobic or hydrophilic form.
• substantially water insoluble shall refer to a material that is not soluble in distilled (or equivalent) water, at 25.degree. C., at a concentration of 0.2% by weight, and preferably not soluble at 0.1% by weight (calculated on a water plus carrier weight basis).
• substantially water soluble shall refer to a material that is soluble in distilled (or equivalent) water, at 25.degree. C., at a concentration of 0.2% by weight, and are preferably soluble at 1.0% by weight.
• soluble “solubility” and the like, for purposes hereof, corresponds to the maximum concentration of carrier, as applicable, that can dissolve in water or other solvents to form a homogeneous solution, as is well understood to those skilled in the art.
• Typical of materials that are in hydrophobic form include ingredients useful in perfumery. Typical of such ingredients are the perfume raw materials, solvents, and mixtures thereof.
• Typical hydrophobic raw materials include the ketones or aldehydes like hexyl cinnamic aldehyde, hydrocarbons like Limolene, d-Limonene, esters like Hercolyn D, benzyl salicylate, hexyl salicylate, triethyl citrate, iso propyl myristate, or mixtures thereof, or hydrophobic perfume composition preferably incorporating one or more of these raw materials.
• Typical hydrophobic solvents include diethyl phthalate, ethers like butoxypropoxypropanol, and mixtures thereof. Also suitable for use herein are the finished perfume compositions which have hydrophobic properties.
• Typical of materials that are in hydrophilic form include alcohols like methanol, ethanol, dipropyleneglycol, water, nonionic surfactants as above described but having a melting point below 30C, or mixtures thereof.
• Preferred carrier materials are selected from benzyl salicylate, diethyl phatalate, dipropylene glycol, methanol, ethanol, and mixtures thereof.
• the amine reaction product when the amine reaction product is only mixed with a carrier but not further processed, the amine reaction product will be present in an amount of from 1 to 75%, preferably 10 to 60%, more preferably 15 to 45% by weight of the processed reaction product. In this instance, the amount of carrier will be sufficient to add up to 100%. Of course, the processed amine reaction product may also contain minors but in quantities which will not exceed the amount of carrier material. Typically the carrier will be present in an amount of from 3 to 95%, preferably from 15 to 90% and most preferably from 45 to 85%, by weight of the processed amine reaction product.
• processed amine reaction product it is meant the resulting product of the amine reaction product with the carrier material.
• Processing of the amine reaction product with the carrier is done by thoroughly mixing the amine reaction product with the carrier.
• This mixing is done at the lowest possible temperature, i.e. just above the melting point of the carrier or at room temperature.
• the mixing step is carried out until a complete homogeneous mixture is obtained.
• homogeneous it is meant compositions which have similar appearance to the resulting composition of a 20g of amine reaction product mixed with 20g of methanol or 80g of diethylphtalate for 5 minutes by means of an Ultra Turrax , the temperature of mixing being room temperature.
• the obtained processed amine reaction product may then be suitable for spray on applications when use of a liquid carrier is made.
• a carrier with a melting point of less than 30 °C it may then be preferred to further process the mixture to form a coated particle like e.g. by adsorption of the mixture onto a solid, preferably porous coating.
• the coating will advantageously protect the processed amine reaction product from the aggressive chemicals present in wash water.
• the resulting coated particles can be in any form which is suitable for incorporation into liquid or powders, preferably powders, such as agglomerate, pellets, tablets, or mixtures thereof.
• Suitable coating agents for both solid, including paste, and liquid mixtures are substantially water-soluble solid binder or agglomerating agents.
• substantially water soluble shall refer to a material that is soluble in distilled (or equivalent) water, at 25°C., at a concentration of 0.2% by weight, and are preferably soluble at 1.0% by weight.
• a “solid” is defined as a material that is a solid at ambient temperatures, and so solid substantially water-soluble binder or agglomerating agent must have a melting point of at least 30°C, and preferably of at least 40°C.
• Suitable water-soluble binders or agglomerating agents include the water soluble organic polymeric compounds, water soluble monomeric polycarboxylates, or their acid forms, homo or copolymeric polycarboxylic acids or their salts in which the polycarboxylic acid comprises at least two carboxylic radicals separated from each other by not more that two carbon atoms, carbonates, bicarbonates, borates, phosphates, sulfate salts like sodium and magnesium sulfate, inorganic perhydrate salts including perborate like perborate monohydrate, percarbonate, silicates, starch, cyclodextrin, and mixtures of any of the foregoing.
• Suitable organic polymeric compounds suitable as coating agents include cellulose derivatives such as methylcellulose, carboxymethylcellulose, hydroxypropylcellulose and hydroxyethylcellulose, as well as carbohydrates like pectins, and gums. Further compounds are carbohydrates and derivatives such as fructose, xylose, galactose, galacturonic acid or glucose based polymers like inuline, dextran, xyloglucan, pectin or gums
• Suitable carboxylates containing one carboxy group include the water soluble salts of lactic acid, glycolic acid and ether derivatives thereof.
• Polycarboxylates containing two carboxy groups include the water-soluble salts of succinic acid, malonic acid, (ethylenedioxy) diacetic acid, maleic acid, diglycolic acid, tartaric acid, tartronic acid and fumaric acid, as well as the ether carboxylates and the sulfinyl carboxylates.
• Polycarboxylates containing three carboxy groups include, in particular, water-soluble citrates, aconitrates and citraconates as well as succinate derivatives such as the carboxymethyloxysuccinates described in British Patent No.
• Polycarboxylates containing four carboxy groups include oxydisuccinates disclosed in British Patent No. 1,261,829, 1,1,2,2-ethane tetracarboxylates, 1,1,3,3-propane tetracarboxylates and 1,1,2,3-propane tetracarboxylates.
• Polycarboxylates containing sulfo substituents include the sulfosuccinate derivatives disclosed in British Patent Nos. 1,398,421 and 1,398,422 and in U.S. Patent No. 3,936,448, and the sulfonated pyrolysed citrates described in British Patent No. 1,439,000.
• Alicyclic and heterocyclic polycarboxylates include cyclopentane-cis,cis,cis-tetracarboxylates, cyclopentadienide pentacarboxylates, 2,3,4,5-tetrahydrofuran - cis, cis, cis-tetracarboxylates, 2,5-tetrahydrofuran - cis - dicarboxylates, 2,2,5,5-tetrahydrofuran - tetracarboxylates, 1,2,3,4,5,6-hexane - hexacarboxylates and carboxymethyl derivatives of polyhydric alcohols such as sorbitol, mannitol and xylitol.
• Aromatic polycarboxylates include mellitic acid, pyromellitic acid and the phthalic acid derivatives disclosed in British Patent No. 1,425,343.
• the preferred polycarboxylates are hydroxycarboxylates containing up to three carboxy groups per molecule, more particularly citrates.
• Borate, as well as builders containing borate-forming materials that can produce borate under detergent storage or wash conditions can also be used but are not preferred at wash conditions less that about 50°C, especially less than about 40°C.
• carbonates are the alkaline earth and alkali metal carbonates, including sodium carbonate and sesqui-carbonate and mixtures thereof with ultra-fine calcium carbonate as disclosed in German Patent Application No. 2,321,001 published on November 15, 1973.
• water-soluble phosphates are the alkali metal tripolyphosphates, sodium, potassium and ammonium pyrophosphate, sodium and potassium and ammonium pyrophosphate, sodium and potassium orthophosphate, sodium polymeta/phosphate in which the degree of polymerization ranges from about 6 to 21, and salts of phytic acid.
• Suitable silicates include the water soluble sodium silicates with an SiO 2 : Na 2 O ratio of from 1.0 to 2.8, with ratios of from 1.6 to 2.4 being preferred, and 2.0 ratio being most preferred.
• the silicates may be in the form of either the anhydrous salt or a hydrated salt.
• Sodium silicate with an SiO 2 : Na 2 O ratio of 2.0 is the most preferred silicate.
• Typical disclosure of cyclodextrin derivatives are disclosed in WO96/05358, U.S. Pat. Nos: 3,426,011, Parmerter et al., issued Feb. 4, 1969; 3,453,257; 3,453,258; 3,453,259; and 3,453,260, all in the names of Parmerter et al., and all issued July 1, 1969; 3,459,731, Gramera et al., issued Aug. 5, 1969; 3,553,191, Parmerter et al., issued Jan. 5, 1971; 3,565,887, Parmerter et al., issued Feb. 23, 1971; 4,535,152, Szejtli et al., issued Aug.
• partially water soluble coating agents may also be used as coating agent. These compounds are indeed less preferred because during the wash cycle the amine reaction product will still be at least partially coated and therefore can not display its full functionality of long lasting freshness on dry fabrics or hard surfaces.
• partially water soluble coating agents include the crystalline layered silicates.
• largely water insoluble builders include the sodium aluminosilicates.
• Crystalline layered sodium silicates have the general formula NaMSi x O x+1.y H 2 O wherein M is sodium or hydrogen, x is a number from 1.9 to 4 and y is a number from 0 to 20. Crystalline layered sodium silicates of this type are disclosed in EP-A-0164514 and methods for their preparation are disclosed in DE-A-3417649 and DE-A-3742043.
• x in the general formula above has a value of 2, 3 or 4 and is preferably 2.
• the most preferred material is ⁇ -Na 2 Si 2 O 5 , available from Hoechst AG as NaSKS-6.
• Suitable aluminosilicate zeolites have the unit cell formula Na z [(AlO 2 ) z (SiO 2 )y]. XH 2 O wherein z and y are at least 6; the molar ratio of z to y is from 1.0 to 0.5 and x is at least 5, preferably from 7.5 to 276, more preferably from 10 to 264.
• the aluminosilicate material are in hydrated form and are preferably crystalline, containing from 10% to 28%, more preferably from 18% to 22% water in bound form.
• the aluminosilicate ion exchange materials can be naturally occurring materials, but are preferably synthetically derived. Synthetic crystalline aluminosilicate ion exchange materials are available under the designations Zeolite A, Zeolite B, Zeolite P, Zeolite X, Zeoilte MAP, Zeolite HS and mixtures thereof. Zeolite A has the formula Na 12 [AlO 2 ) 12 (SiO 2 ) 12 ]. xH 2 O wherein x is from 20 to 30, especially 27. Zeolite X has the formula Na 86 [(AlO 2 ) 86 (SiO 2 ) 106 ]. 276 H 2 O.
• the amine reaction product when the amine reaction product is mixed with a carrier and further processed to form a coated particle, the amine reaction product will be present in an amount of from 1 to 75%, preferably 5 to 30%, more preferably 6 to 25% by weight of the processed reaction product in the produced particle.
• the coating agent will be present in an amount of from 10% to 95%, preferably from 30 to 90%, more preferably, 50 to 75% by weight of the particle of the processed amine reaction product.
• the amount of carrier will be sufficient to add up to 100%.
• the coated particle may also contain minors but in quantities which will not exceed either of the amount of carrier material or coating agent.
• Preferred coating materials are selected from carbonate, starch, cyclodextrin, sulfate salts, silicates, and mixtures thereof.
• the surface treatment of the particle can be carried out in a number of ways using equipment known in the art and the process may take in batch wise or continuous fashion.
• One method for applying the coating material involves agglomeration. Any conventional agglomerator/mixer may be used including, but not limited to pan, rotary drum and vertical blender types. Molten coating compositions may also be applied either by being poured onto, or spray atomized onto a moving bed of the mixture of amine reaction product with carrier.
• Another method for applying the coating is to pour the obtained mixture (so-called particle), as herein before described, onto the coating material and agglomerate it in a Braun Mixer. Care is also taken that the temperature during the mixing and/or coating step does not substantially exceed the melting point of the carrier material. For example, 50g of a mixture containing a hydrophobic perfume composition and 25g of the amine reaction product is poured at room temperature into a Braun Mixer containing 200g of starch. The mixing of the ingredients is carried out for about 5 minutes.
• the coated particle may be useful to remove the carrier.
• removal can be made by conventional techniques.
• One typical of these technique is vacuum drying.
• the original viscosity of the amine reaction product i.e. higher viscosity
• the coated particle can then be used as is for incorporation into the finished composition.
• the coated particle may also contain one or more additional ingredients like a surfactant for improved solubility or dispersability.
• a surfactant for improved solubility or dispersability.
• Typical of such surfactant are the anionic, nonionic, or cationic surfactants. a cationic, anion or non-ionic surfactant like.
• the weight ratio of such additional ingredient(s) to the coating agent is of up to 1:1.
• an additional coating on the coated particle can be provided, which depending on the nature of this additional coating will give improved storage stability, flowability and/or improved fabric substantivity of the coated particle.
• One typical example is polyvinyl alcohol.
• the finished compositions aspect of the invention comprises the incorporation of the hereinbefore described processed amine reaction product together with one or more laundry or cleaning ingredient in a finished composition.
• Laundry compositions of the invention which also encompass compositions providing color care, are suitable for use in any steps of the domestic treatment, that is as a pre-treatment composition, as a wash additive as a composition suitable for use in the rinse-cycle of the laundry cycle or applied on a dryer-sheet.
• multiple applications can be made such as treating the fabric with a pre-treatment composition of the invention and also thereafter with a composition of the invention suitable for use in the rinse cycle and/or suitable for use as a dryer-sheet.
• the incorporation of the processed amine reaction product is conveniently made depending on its end form by either by spraying when in sprayable liquid form, or dry-addition when in coated form.
• Laundry compositions encompass laundry detergent compositions, including liquid, solid form like powdered, tablets as well as softening compositions including rinse added softening composition as well as dryer added softening compositions.
• compositions incorporating the processed amine reaction product will normally contain from 0.001 to 25%, more preferably from 0.02 to 10%, and most preferably from 0.05 to 5% of the processed product on a composition weight basis.
• the finished composition is a detergent composition, more preferably in solid form.
• the detergent composition comprises a clay.
• compositions of the invention may preferably contain a clay, preferably present at a level of from 0.05% to 40%, more preferably from 0.5% to 30%, most preferably from 2% to 20% by weight of the composition.
• clay mineral compound as used herein, excludes sodium aluminosilicate zeolite builder compounds, which however, may be included in the compositions of the invention as optional components.
• One preferred clay may be a bentonite clay.
• Highly preferred are smectite clays, as for example disclosed in the US Patents No.s 3,862,058 3,948,790, 3,954,632 and 4,062,647 and European Patents No.s EP-A-299,575 and EP-A-313,146 all in the name of the Procter and Gamble Company.
• smectite clays herein includes both the clays in which aluminium oxide is present in a silicate lattice and the clays in which magnesium oxide is present in a silicate lattice.
• Typical smectite clay compounds include the compounds having the general formula Al 2 (Si 2 O 5 ) 2 (OH) 2 .nH 2 O and the compounds having the general formula Mg 3 (Si 2 O 5 ) 2 (OH) 2 .nH 2 O. Smectite clays tend to adopt an expandable three layer structure.
• Suitable smectite clays include those selected from the classes of the montmorillonites, hectorites, volchonskoites, nontronites, saponites and sauconites, particularly those having an alkali or alkaline earth metal ion within the crystal lattice structure.
• Sodium or calcium montmorillonite are particularly preferred.
• Suitable smectite clays are sold by various suppliers including English China Clays, Laviosa, Georgia Kaolin and Colin Stewart Minerals.
• Clays for use herein preferably have a particle dimension of from 10nm to 800nm more preferably from 20nm to 500 mm, most preferably from 50nm to 200 mm.
• Particles of the clay mineral compound may be included as components of agglomerate particles containing other detergent compounds.
• the term "largest particle dimension" of the clay mineral compound refers to the largest dimension of the clay mineral component as such, and not to the agglomerated particle as a whole.
• Substitution of small cations, such as protons, sodium ions, potassium ions, magnesium ions and calcium ions, and of certain organic molecules including those having positively charged functional groups can typically take place within the crystal lattice structure of the smectite clays.
• a clay may be chosen for its ability to preferentially absorb one cation type, such ability being assessed by measurements of relative ion exchange capacity.
• the smectite clays suitable herein typically have a cation exchange capacity of at least 50 meq/100g.
• U.S. Patent No. 3,954,632 describes a method for measurement of cation exchange capacity.
• the crystal lattice structure of the clay mineral compounds may have, in a preferred execution, a cationic fabric softening agent substituted therein.
• a cationic fabric softening agent substituted therein Such substituted clays have been termed 'hydrophobically activated' clays.
• the cationic fabric softening agents are typically present at a weight ratio, cationic fabric softening agent to clay, of from 1:200 to 1:10, preferably from 1:100 to 1:20.
• Suitable cationic fabric softening agents include the water insoluble tertiary amines or dilong chain amide materials as disclosed in GB-A-1 514 276 and EP-B-0 011 340.
• a preferred commercially available "hydrophobically activated" clay is a bentonite clay containing approximately 40% by weight of a dimethyl ditallow quaternary ammonium salt sold under the tradename Claytone EM by English China Clays International.
• the clay is present in an intimate mixture or in a particle with a humectant and a hydrophobic compound, preferably a wax or oil, such as paraffin oil.
• humectants are organic compounds, including propylene glycol, ethylene glycol, dimers or trimers of glycol, most preferably glycerol.
• the particle is preferably an agglomerate.
• the particle may be such that the wax or oil and optionally the humectant form an encapsulate on the clay or alternatively, the clay be a encapsulate for the wax or oil and the humectant. It may be preferred that the particle comprises an organic salt or silica or silicate.
• the clay is preferably mixed with one or more surfactants and optionally builders and optionally water, in which case the mixture is preferably subsequently dried.
• a mixture is further processed in a spray-drying method to obtain a spray dried particle comprising the clay.
• the flocculating agent is also comprised in the particle or granule comprising the clay.
• the intimate mixture comprises a chelating agent.
• compositions of the invention may contain a clay flocculating agent, preferably present at a level of from 0.005% to 10%, more preferably from 0.05% to 5%, most preferably from 0.1% to 2% by weight of the composition.
• the clay flocculating agent functions such as to bring together the particles of clay compound in the wash solution and hence to aid their deposition onto the surface of the fabrics in the wash. This functional requirement is hence different from that of clay dispersant compounds which are commonly added to laundry detergent compositions to aid the removal of clay soils from fabrics and enable their dispersion within the wash solution.
• Preferred as clay flocculating agents herein are organic polymeric materials having an average weight of from 100,000 to 10,000,000, preferably from 150,000 to 5,000,000, more preferably from 200,000 to 2,000,000.
• Suitable organic polymeric materials comprise homopolymers or copolymers containing monomeric units selected from alkylene oxide, particularly ethylene oxide, acrylamide, acrylic acid, vinyl alcohol, vinyl pyrrolidone, and ethylene imine. Homopolymers of, on particular, ethylene oxide, but also acrylamide and acrylic acid are preferred.
• EP-A-299,575 and EP-A-313,146 in the name of the Procter and Gamble Company describe preferred organic polymeric clay flocculating agents for use herein.
• the weight ratio of clay to the flocculating polymer is preferably from 1000:1 to 1:1, more preferably from 500:1 to 1:1, most preferably from 300:1 to 1:1, or even more preferably from 80:1 to 10:1, or in certain applications even from 60:1 to 20:1.
• Inorganic clay flocculating agents are also suitable herein, typical examples of which include lime and alum.
• the flocculating agent is preferably present in a detergent base granule such as a detergent agglomerate, extrudate or spray-dried particle, comprising generally one or more surfactants and builders.
• Effervescent means may also be optionally used in the compositions of the invention.
• Effervescency as defined herein means the evolution of bubbles of gas from a liquid, as the result of a chemical reaction between a soluble acid source and an alkali metal carbonate, to produce carbon dioxide gas, i.e. C 6 H 8 O 7 + 3NaHCO 3 ⁇ Na 3 C 6 H 5 O 7 + 3CO 2 ⁇ + 3H 2 O
• Suitable alkali and/ or earth alkali inorganic carbonate salts herein include carbonate and hydrogen carbonate of potassium, lithium, sodium, and the like amongst which sodium and potassium carbonate are preferred.
• Suitable bicarbonates to be used herein include any alkali metal salt of bicarbonate like lithium, sodium, potassium and the like, amongst which sodium and potassium bicarbonate are preferred.
• the choice of carbonate or bicarbonate or mixtures thereof may be made depending on the pH desired in the aqueous medium wherein the granules are dissolved.
• the inorganic alkali and/ or earth alkali carbonate salt of the compositions of the invention comprises preferably a potassium or more preferably a sodium salt of carbonate and/ or bicarbonate.
• the carbonate salt comprises sodium carbonate, optionally also a sodium bicarbonate.
• the inorganic carbonate salts herein are preferably present at a level of at least 20% by weight of the composition. Preferably they are present at a level of at least 23% or even 25% or even 30% by weight, preferably up to about 60% by weight or more preferably up to 55% or even 50% by weight.
• detergent granules such as agglomerates or spray dried granules.
• an effervescence source is present, preferably comprising an organic acid, such as carboxylic acids or aminoacids, and a carbonate. Then it may be preferred that part or all of the carbonate salt herein is premixed with the organic acid, and thus present in an separate granular component.
• Preferred effervescent source are selected from compressed particles of citric acid and carbonate optionally with a binder; and particle of carbonate, bicarbonate and malic or maleic acid in weight ratios of 4:2:4.
• the dry add form of citric acid and carbonate are preferably used.
• the carbonate may have any particle size.
• the carbonate salt in particular when the carbonate salt is present in a granule and not as separately added compound, the carbonate salt has preferably a volume median particle size from 5 to 375 microns, whereby preferably at least 60%, preferably at least 70% or even at least 80% or even at least 90% by volume, has a particle size of from 1 to 425 microns.
• the carbon dioxide source has a volume median particle size of 10 to 250, whereby preferably at least 60 %, or even at least 70% or even at least 80% or even at least 90% by volume, has a particle size of from 1 to 375 microns; or even preferably a volume median particle size from 10 to 200 microns, whereby preferably at least 60 %, preferably at least 70% or even at least 80% or even at least 90% by volume, has a particle size of from 1 to 250 microns.
• the carbonate salt when added as separate component, so to say 'dry-added' or admixed to the other detergent ingredients, the carbonate may have any particle size, including the above specified particle sizes, but preferably at least an volume average particle size of 200 microns or even 250 microns or even 300 microns.
• the carbon dioxide source of the required particle size is obtained by grinding a larger particle size material, optionally followed by selecting the material with the required particle size by any suitable method.
• percarbonate salts may be present in the compositions of the invention as a bleaching agent, they are not included in the carbonate salts as defined herein.
• the preferred detergent composition will, also preferably contain a bleach precursor, a source of alkaline hydrogen peroxide necessary to form a peroxyacid bleaching species in the wash solution and preferably will also contain other components conventional in detergent compositions.
• preferred detergent compositions will incorporate one or more of surfactants, organic and inorganic builders, soil suspending and anti-redeposition agents, suds suppressors, enzymes, fluorescent whitening agents, photoactivated bleaches, perfumes, colours, and mixtures thereof.
• composition of the invention may take a variety of physical form including liquid, gel, foam in either aqueous or non-aqueous form, granular and tablet forms.
• a packaged composition comprising the processed product of the invention or composition of the invention.
• the packaged composition is a closed packaging system having a moisture vapour transmission rate of less than 20g/m 2 /24 hours. Typical disclosure of such a package can be found in WO 98/40464.
• Still another preferred package is a spray dispenser.
• the present invention also relates to such compositions incorporated into a spray dispenser to create an article of manufacture that can facilitate treatment of fabric articles and/or surfaces with said compositions containing the amine reaction product and other ingredients (examples are cyclodextrins, polysaccharides, polymers, surfactant, perfume, softener) at a level that is effective, yet is not discernible when dried on the surfaces.
• the spray dispenser comprises manually activated and non-manual powered (operated) spray means and a container containing the treating composition. Typical disclosure of such spray dispenser can be found in WO 96/04940 page 19 line 21 to page 22 line 27.
• the articles of manufacture preferably are in association with instructions for use to ensure that the consumer applies sufficient ingredient of the composition to provide the desired benefit.
• compositions to be dispensed from a sprayer contain a level of amine reaction product of from about 0.01% to about 5%, preferably from about 0.05% to about 2%, more preferably from about 0.1% to about 1%, by weight of the usage composition.
• Also provided herein is a method for providing a delayed release of an active ketone or aldehyde which comprises the step of contacting the surface to be treated with a compound or composition of the invention, and thereafter contacting the treated surface with a material, preferably an aqueous medium like moisture or any other means susceptible of releasing the perfume from the amine reaction product.
• surface it is meant any surface onto which the compound can deposit. Typical examples of such material are fabrics, hard surfaces such as dishware, floors, bathrooms, toilet, kitchen and other surfaces in need of a delayed release of a perfume ketone and/or aldehyde such as that with litter like animal litter.
• the surface is selected from a fabric, a tile, a ceramic; more preferably is a fabric.
• delayed release is meant release of the active component (e.g perfume) over a longer period of time than by the use of the active (e.g., perfume) itself.
• ⁇ -amino ketone from Lupasol G100 (commercially available from BASF with a content of 50 % water, 50 % Lupasol G100 (Mw. 5000)) and ⁇ -Damascone (or ⁇ -Damascone) was prepared using any one of these three different procedures described as follows:
• Lupasol G35 or Lupasol HF is used instead of Lupasol G100.
• amine reaction product Processing of the amine reaction product with the carrier is done as hereinbefore described.
• 20g of amine reaction product as above synthesised is mixed with 10 to 80g of a carrier, e.g. hydrophobic perfume composition, dipropylene glycol, diethylphthalate in an Ultra Turrax until an homogenous mixture is obtained.
• a carrier e.g. hydrophobic perfume composition, dipropylene glycol, diethylphthalate in an Ultra Turrax until an homogenous mixture is obtained.
• the temperature of mixing is about room temperature, and the speed of the mixer is sufficient to maintain such temperature substantially constant. Temperature and time will depend on the nature of the carrier but are a conventional step to skilled man.
• the amount of carrier relative to the amine reaction product will depends on the desired sprayability and the end viscosity of the resulting mixture. In the examples of the present invention, the viscosity was below 500Cps, as measured on a rheometer, TA Instrument CSL 2 100 at a temperature of 25
• amine reaction product Processing of the amine reaction product with the carrier is done as hereinbefore described.
• 20g of amine reaction product as above synthesised is mixed in an Ultra Turrax containing 20g of carrier, e.g. methanol or perfume mixture or composition for 5 minutes, the temperature of mixing being to about room temperature, and the speed of the mixer being sufficient so as to maintain such temperature substantially constant.
• Temperature and time will depend on the nature of the carrier but are a conventional step to skilled man.
• the composition in % by weight of a typical hydrophobic perfume mixture is as follows: Citronellol 7 Geraniol 7 Linalool 7 Para Tertiary Butyl Cyclohexyl Acetate 10 Phenyl Ethyl Alcohol 19 Habanolide 4.5 Para Methoxy Acetophenone 1.5 Benzyl Acetate 4 Eugenol 2 Phenyl Ethyl Acetate 5 Verdyl Acetate 6 Verdyl Propionate 4 Hexyl Cinnamic Aldehyde 3 lonone Gamma Methyl 2 Methyl Cedrylone 10 P.T. Bucinal 7 Para Cresyl Methyl Ether 1
• the obtained processed amine reaction product from above is subsequently coated.
• the resulting mixture is maintained at a temperature substantially equal to the melting point of the carrier material and poured onto the coating material and agglomerated in an electrical mixer like a Braun Mixer. Care is also taken that the temperature during the mixing does not substantially exceed the melting point of the carrier material.
• 100g of a mixture containing the methanol or perfume mixture and 20g of the amine reaction product is poured at room temperature into a Braun Mixer containing 300g of carbonate. The mixing of the ingredients is carried out for about 5 minutes. Again, temperature and time will depend on the nature of the coating agent but are conventional step to skilled man.
• the coated particle may be desired to remove the methanol by vacuum distillation.
• a B C Blown Powder Zeolite A 15.0 15.0 15.0 Sulfate 0.0 5.0 0.0 LAS 3.0 3.0 3.0 QAS - 1.5 1.5 DTPMP 0.4 0.2 0.4 EDDS - 0.4 0.2 CMC 0.4 0.4 0.4 MA/AA 4.0 2.0 2.0 Agglomerates LAS 5.0 5.0 5.0 TAS 2.0 2.0 1.0 Silicate 3.0 3.0 4.0 Zeolite A 8.0 8.0 8.0 Carbonate 8.0 8.0 4.0 Spray On Perfume 0.3 0.3 0.3 C45E7 2.0 2.0 2.0 C25E3 2.0 - - PARP2 0.4 0.2 - Dry additives Citrate 5.0 - 2.0 Bicarbonate - 3.0 - Carbonate 8.0 15.0 10.0 TAED 6.0 2.0 5.0 PB1 14.0 7.0 10.0 PEO - - 0.2 PARP3 1.2(c) 1.0 (c) 0.75(c) Bentonite clay - - 10.0 Protease 1.0 1.0 1.0
• composition in the form of a tablet, bar, extrudate or granule in accord with the invention A B C D E F G Sodium C 11 -C 13 alkylbenzenesulfonate 12.0 16.0 23.0 19.0 18.0 20.0 16.0 Sodium C 14 -C 15 alcohol sulfate 4.5 - - - 4.0 C 14 -C 15 alcohol ethoxylate (3) sulfate - - 2.0 - 1.0 1.0 1.0 1.0 Sodium C 14 -C 15 alcohol ethoxylate 2.0 2.0 - 1.3 - - 5.0 C 9 -C 14 alkyl dimethyl hydroxy ethyl quaternary ammonium salt - - 1.0 0.5 2.0 Tallow fatty acid - - - - 1.0 Sodium tripolyphosphate / Zeolite 23.0 25.0 14.0 22,0 20.0 10.0 20.0 Sodium carbonate 25.0 22.0 35.0 20.0 28.0 41.0 30.0 Sodium Polyacrylate (45%)
• detergent additive compositions were prepared according to the present invention : A B C LAS - 5.0 5.0 STPP 30.0 - 20.0 Zeolite A - 35.0 20.0 PB1 20.0 15.0 - TAED 10.0 8.0 - PARP1 1.0(c) - 0.5(c) PARP3 - 0.3(c) 0.1(c) Protease - 0.3 0.3 Amylase - 0.06 0.06 Minors, water and miscellaneous Up to 100%
• liquid dishwashing detergent compositions of density 1.40Kg/L were prepared according to the present invention : A B C D STPP 17.5 17.5 17.2 16.0 Carbonate 2.0 - 2.4 - Silicate 5.3 6.1 14.6 15.7 NaOCI 1.15 1.15 1.15 1.25 Polygen/carbopol 1.1 1.0 1.1 1.25 Nonionic - - 0.1 - NaBz 0.75 0.75 - - PARP3 0.4(c) 0.2(c) 0.1(c) 0.5(c) NaOH - 1.9 - 3.5 KOH 2.8 3.5 3.0 - pH 11.0 11.7 10.9 11.0 Sulphate, miscellaneous and water up to 100%
• liquid rinse aid compositions were prepared according to the present invention : A B C Nonionic 12.0 - 14.5 Nonionic blend - 64.0 - Citric 3.2 - 6.5 HEDP 0.5 - - PEG - 5.0 - SCS 4.8 - 7.0 Ethanol 6.0 8.0 - PARP1 1.6(c) - 1.0(c) PARP3 - 1.0(c) 0.1 (c) pH of the liquid 2.0 7.5 / Miscellaneous and water Up to 100%
• liquid dishwashing compositions were prepared according to the present invention : A B C D E C17ES 28.5 27.4 19.2 34.1 34.1 Amine oxide 2.6 5.0 2.0 3.0 3.0 C12 glucose amide - - 6.0 - - Betaine 0.9 - - 2.0 2.0 Xylene sulfonate 2.0 4.0 - 2.0 - Neodol C11E9 - - 5.0 - - Polyhydroxy fatty acid amide - - - 6.5 6.5 Sodium diethylene penta acetate - - 0.03 - - (40%) TAED - - - 0.06 0.06 Sucrose - - - 1.5 1.5 Ethanol 4.0 5.5 5.5 9.1 9.1 Alkyl diphenyl oxide disulfonate - - - - 2.3 Ca formate - - - 0.5 1.1 Ammonium citrate 0.06 0.1 - - - Na chloride - 1.0 - - - Mg chloride
• the following spray composition for cleaning of hard surfaces and removing household mildew was prepared according to the present invention : PARP3 0.4(c) Amylase 0.01 Protease 0.01 Na octyl sulfate 2.0 Na dodecyl sulfate 4.0 Na hydroxide 0.8 Silicate 0.04 Butyl carbitol 4.0 Perfume 0.35 Water/minors up to 100%
• lavatory cleansing block compositions were prepared according to the present invention.
• the following toilet bowl cleaning composition was prepared according to the present invention.
• pre-soak fabric conditioning and/or fabric enhancement compositions according to the present invention which can be suitably used in the laundry rinse cycle.
• the perfume 1, 2, and 3 have the following compositions: Perfume 1 2 3 Perfume Ingredients Wt.% Wt.% Wt.% Anisic aldehyde - - 2 Benzophenone 3 5 - Benzyl acetate 10 15 5 Benzyl salicylate 5 20 5 Cedrol 2 - - Citronellol 10 - 5 Coumarin - - 5 Cymal - - 3 Dihydromyrcenol 10 - 5 Flor acetate 5 - 5 Galaxolide 10 - - Lilial 10 15 20 Linalyl acetate 4 - 5 Linalool 6 15 5 Methyl dihydro jasmonate 3 10 5 Phenyl ethyl acetate 2 5 1 Phenyl ethyl alcohol 15 15 20 alpha-Terpineol 5 - 8 Vanillin - - 1 Total 100 100 100 100 100 100 100 100 100

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• 1999
  • 1999-07-08 EP EP99870146A patent/EP1067173A1/de not_active Ceased
• 2000
  • 2000-07-06 JP JP2001509451A patent/JP2003504350A/ja not_active Withdrawn
  • 2000-07-06 MX MXPA02000337A patent/MXPA02000337A/es active IP Right Grant
  • 2000-07-06 AU AU59160/00A patent/AU5916000A/en not_active Abandoned
  • 2000-07-06 WO PCT/US2000/018468 patent/WO2001004247A1/en active Application Filing

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