Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/2093—Esters; Carbonates
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/22—Carbohydrates or derivatives thereof
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
  • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/3723—Polyamines or polyalkyleneimines
• • 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
• • 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 act 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 from 30°C to 135°C.
• the present invention is a process for making particles of amine reaction product of a compound containing a primary amine functional group and an active ketone or aldehyde containing component, and which comprises the steps of:
• the amine reaction product for use herein is a product of reaction between a compound containing a primary amine functional group and an active ketone or aldehyde containing component, so called hereinafter "amine reaction product”.
• primary amine it is meant a component which carries at least one primary amine and/or amide function.
• the primary amine compound is also characterized by an Odour Intensity Index of less than that of a 1% solution of methylanthranilate 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.
• Preferred B carriers are inorganic or organic carriers.
• 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.
• 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 organic polymeric compounds suitable for mixing with primary amine compound herein include polyethylene glycols, and derivatives thereof, particularly those of molecular weight 1000-10000, more particularly 2000 to 8000 and most preferably about 4000.
• the alkyl ethoxylate condensation products of aliphatic alcohols with from about 1 to about 150 moles of ethylene oxide are suitable for use herein.
• the alkyl chain of the aliphatic alcohol can either be straight or branched, primary or secondary, and generally contains from 6 to 22 carbon atoms.
• Particularly preferred are the condensation products of alcohols having an alkyl group containing from 8 to 20 carbon atoms with from about 25 to about 150 moles of ethylene oxide per mole of alcohol, preferably 50 to 100, more preferably 80 moles of ethylene oxide per mole of alcohol.
• the preferred alkylpolyglycosides have the formula R2O((CnH2n)O)t(glycosyl) x wherein R2 is selected from the group consisting of alkyl, alkylphenyl, hydroxyalkyl, hydroxyalkylphenyl, and mixtures thereof in which the alkyl groups contain from 10 to 18, preferably from 12 to 14, carbon atoms; n is 2 or 3; t is from 0 to 10, preferably 0, and X is from 1.3 to 8, preferably from 1.3 to 3, most preferably from 1.3 to 2.7.
• the glycosyl is preferably derived from glucose.
• Fatty acid amide surfactants suitable for use herein are those having the formula: R 6 CON(R 7 ) 2 wherein R 6 is an alkyl group containing from 7 to 21, preferably from 9 to 17 carbon atoms and each R 7 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 hydroxyalkyl, and -(C 2 H 4 O) x H, where x is in the range of from 1 to 3.
• 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 the produced particle. In this instance, the amount of carrier will be sufficient to add up to 100%. Of course, the particle may also contain minors but in quantities which will not exceed the amount of carrier material.
• the carrier will be present in an amount of from 3 to 95%, preferably from 15 to 80% and most preferably from 25 to 75%, by weight of the produced particles in the processed amine reaction product.
• 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.
• 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 80g of TAE80 for 5 minutes by means of an Ultra Turrax, the temperature of mixing being of about 70°C.
• 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.
• the preferred polycarboxylates are hydroxycarboxylates containing up to three carboxy groups per molecule, more particularly citrates.
• 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.
• 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.
• 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 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.
• Preferred coating materials are selected from carbonate, starch, cyclodextrin, and mixtures thereof.
• 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 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.
• the finished composition is a detergent composition, more preferably in solid form.
• compositions incorporating the processed amine reaction product will normally contain from 0.1 to 25%, more preferably from 0.2 to 10%, and most preferably from 0.5 to 5% of the processed product on a composition weight basis.
• the preferred detergent composition will, 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.
• 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.
• 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 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 G100 was dried using the following procedure: 20 g of the Lupasol solution was dried at the rotating evaporator during several hours. The obtained residue, still containing about 4.5 g of H 2 O, was azeotropically distilled at the rotating evaporator using toluene. The residue was then placed in the desiccator dried at 60 °C (using P 2 O 5 as water absorbing material). On basis of the obtained weight we concluded that the oil contained less then 10 % H 2 O. On basis of the NMR-spectra we concluded that this is probably less then 5 %. This dried sample was then used in the preparation of ⁇ -amino ketones.
• Lupasol G35 or Lupasol HF is used instead of Lupasol G100.
• amine reaction product is processed as hereinbefore described.
• 20g of amine reaction product as above synthesised is mixed in an Ultra Turrax containing 80g of carrier, e.g. TAE80 for 5 minutes, the temperature of mixing being of about 70°C, 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 resulting mixture is maintained at a temperature substantially equal to the melting point of the carrier material. Once the mixture is at a suitable temperature, it is 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.
• 150g of a mixture containing TAE80 and 20% of the amine reaction product is poured at 60°C into a Braun Mixer containing 300g of carbonate.
• the mixing of the ingredients is carried out for about 5 minutes. Care is also taken that the temperature during the mixing does not exceed 65°C. Again, temperature and time will depend on the nature of the coating agent but are conventional step to skilled man.
• PEI Polyethyleneimine with an average molecular weight of 1800 and an average ethoxylation degree of 7 ethyleneoxy residues per nitrogen HEDP 1,1 -hydroxyethane diphosphonic acid LAS Sodium linear C 11-13 alkyl benzene sulfonate TAS Sodium tallow alkyl sulfate CxyAS Sodium C 1x -C 1y alkyl sulfate C46SAS Sodium C 14 -C 16 secondary (2,3) alkyl sulfate CxyEzS Sodium C 1x -C 1y alkyl sulfate condensed with z moles of ethylene oxide CxyEz C 1x -C 1y predominantly linear primary alcohol condensed with an average of z moles of
• Alcalase Proteolytic enzyme having 5.3% by weight of active enzyme, sold by NOVO Industries A/S Cellulase Cellulytic enzyme, having 0.23% by weight of active enzyme, sold by NOVO Industries A/S under the tradename Carezyme Amylase Amylolytic enzyme, having 1.6% by weight of active enzyme, sold by NOVO Industries A/S under the tradename Termamyl 120T Lipase Lipolytic enzyme, having 2.0% by weight of active enzyme, sold by NOVO Industries A/S under the tradename Lipolase Lipase (1) Lipolytic enzyme, having 2.0% by weight of active enzyme, sold by NOVO Industries A/S under the tradename Lipolase Ultra Endolase Endoglucanase enzyme, having 1.5% by weight of active enzyme, sold by NOVO Industries A/S PB4 Sodium perborate tetrahydrate of nominal formula NaBO 2 .3H 2 O.H 2 O 2 PB1 Anhydrous sodium perborate bleach of nominal formula NaBO 2 .H 2 O 2 Percarbonate Sodium
• Photoactivated bleach (1) Sulfonated zinc phthlocyanine encapsulated in dextrin soluble polymer
• Photoactivated bleach (2) Sulfonated alumino phthlocyanine encapsulated in dextrin soluble polymer
• Brightener 1 Disodium 4,4'-bis(2-sulphostyryl)biphenyl
• Brightener 2 Disodium 4,4'-bis(4-anilino-6-morpholino-1 .3.5-triazin-2-yl)amino) stilbene-2:2'-disulfonate
• PEGx Polyethylene glycol, with a molecular weight of x (typically 4,000)
• PEO Polyethylene oxide with an average molecular weight of 50,000
• PVI Polyvinyl imidosole with an average molecular weight of 20,000
• Paraffin Paraffin oil sold under the tradename Winog 70 by Wintershall. NaBz Sodium benzoate. BzP Benzoyl Peroxide. SCS Sodium cumene sulphonate. BTA Benzotriazole. PH Measured as a 1% solution in distilled water at 20°C.
• PARP1 Processed amine reaction product of ethyl 4-aminobenzoate with 2,4-dimethyl-3-cyclohexen-1-carboxaldehyde as made from Synthesis example I, mixed with a carrier and agglomerated with TAE80 coating agent according to processing method above described.
• PARP2 Processed amine reaction product of Lupasol G35 with ⁇ -Damascone as made from Synthesis example III, mixed with a carrier and agglomerated with TAE100 coating agent according to processing method above described.
• PARP3 Processed amine reaction product of Lupasol HF with 6-Damascone as made from Synthesis example III, mixed with a carrier and agglomerated with TAE80 coating agent according to processing method above described.
• PARP4 Processed amine reaction product of BNPP with 6-Damascone as made from Synthesis example II, mixed with a carrier and agglomerated with PEG4000 coating agent according to processing method above described.
• PARP5 Processed amine reaction product of LupasolG100 with 2,4-dimethyl-3-cyclohexen-1-carboxaldehyde as made from Synthesis example III, mixed with a carrier and agglomerated with TAE80 coating agent according to processing method above described.
• PARP6 Processed amine reaction product of ethyl 4-aminobenzoate with trans-2-nonenal as made from Synthesis example I, mixed with a carrier and agglomerated with TAE80 coating agent according to processing method above described.
• PARP7 Processed amine reaction product of ethyl 4-aminobenzoate with trans-2-hexenal as made from Synthesis example I, mixed with a carrier and agglomerated with TAE80 coating agent according to processing method above described.
• the following detergent compositions were prepared: GG HH II 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 - - 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 2.0(c) 1.0(c) 0.75(c) Bentonite clay - - 10.0 Protease 1.0 1.0 1.0 Lipase 0.4
• liquid detergent formulations were prepared in accord with the invention (levels are aiven in Darts per weight): SS TT UU VV WW XX YY ZZ LAS 10.0 13.0 9.0 - 25.0 - - - C25AS 4.0 1.0 2.0 10.0 - 13.0 18.0 15.0 C25E3S 1.0 - - 3.0 - 2.0 2.0 4.0 C25E7 6.0 8.0 13.0 2.5 - - 4.0 4.0 TFAA - - - 4.5 - 6.0 8.0 APA - 1.4 - - 3.0 1.0 2.0 - TPKFA 2.0 - 13.0 7.0 - 15.0 11.0 11.0 Citric acid 2.0 3.0 1.0 1.5 1.0 1.0 1.0 1.0 1.0 1.0 Dodecenyl/tetradecenyl succinic acid 12.0 10.0 - - 15.0 - - - Rape seed fatty acid 4.0 2.0 1.0 - 1.0 - - 3.5 - Ethanol 4.0
• the following detergent additive compositions were prepared according to the present invention : AL AM AN 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 10.0(c) - 5.0(c) PARP3 - 4.0(c) 2.0(c) Protease - 0.3 0.3 Amylase - 0.06 0.06 Minors, water and miscellaneous Up to 100%
• the following tablet detergent compositions were prepared according to the present invention by compression of a granular dishwashing detergent composition at a pressure of 13KN/cm 2 using a standard 12 head rotary press: BF BJ BK BL BM BN STPP - 48.8 49.2 38.0 - 46.8 Citrate 26.4 - - - 31.1 - Carbonate - 4.0 12.0 14.4 10.0 20.0 Silicate 26.4 14.8 15.0 12.6 17.7 2.4 PARP1 3.0(c) - - - 5.0(c) - PARP2 - 2.0(c) - - - 4.0(c) PARP3 - - 2.0(c) 1(s) - - Protease 0.058 0.072 0.041 0.033 0.052 0.013 Amylase 0.01 0.03 0.012 0.007 0.016 0.002 Lipase 0.005 - - - - - PB1 1.6 7.7 12.2 10.6 15.7 - PB4 6.
• liquid dishwashing detergent compositions of density 1.40Kg/L were prepared according to the present invention : BO BP BQ BR 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 4.0(c) 2.0(c) 1.0(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 : BS BT BU 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 - PARP5 6.0(c) - 3.0(c) PARP3 - 2.0(c) 1.0(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 : BV BW BX BY BZ 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 - -
• liquid hard surface cleaning compositions were prepared according to the present invention : CA CB CD CE CF PARP1 8.0(c) - 6.0(s) - 4.0(c) PARP3 - 2.0(c) - 1.0(c) 0.5(c) Amylase 0.01 0.002 0.005 - - Protease 0.05 0.01 0.02 - - Hydrogen peroxide - - - 6.0 6.8 Acetyl triethyl citrate - - - 2.5 - DTPA - - - 0.2 - Butyl hydroxy toluene - - - 0.05 - EDTA 0.05 0.05 0.05 - - Citric / Citrate 2.9 2.9 2.9 2.9 1.0 - LAS 0.5 0.5 0.5 - - C12 AS 0.5 0.5 0.5 - - C10AS - - - - 1.7 C12(E)S 0.5 0.5 0.5 - - C12,13 E6.5 nonionic
• the following spray composition for cleaning of hard surfaces and removing household mildew was prepared according to the present invention : PARP3 4.0(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.
• the following dryer added fabric conditioner compositions were prepared according to the present invention : CV CW CX CY DEQA(2) - - - 50.0 DTMAMS - - 26.0 - SDASA 70.0 70.0 42.0 35.0 Neodol 45-13 13.0 13.0 - - Ethanol 1.0 1.0 - - PARP 3(c) 1.5 - 1.5 3.0 PARP 3(s) - 1.5 - - Perfume 0.75 0.75 1.0 1.5 Glycoperse S-20 - - - 10.0 Glycerol monostearate - - 26.0 - Digeranyl Succinate 0.38 0.38 - - Clay - - 3.0 - Dye 0.01 0.01 - - Minors to balance to 100%

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• 1999
  • 1999-02-15 EP EP99870029A patent/EP0971021A1/en not_active Withdrawn
  • 1999-07-12 AU AU48703/99A patent/AU4870399A/en not_active Abandoned
  • 1999-07-12 AT AT99932389T patent/ATE286962T1/de not_active IP Right Cessation
  • 1999-07-12 WO PCT/US1999/015679 patent/WO2000002986A2/en active IP Right Grant
  • 1999-07-12 BR BRPI9912023-2A patent/BR9912023B1/pt not_active IP Right Cessation
  • 1999-07-12 CA CA002335576A patent/CA2335576C/en not_active Expired - Fee Related
  • 1999-07-12 JP JP2000559208A patent/JP2002524573A/ja active Pending
  • 1999-07-12 ES ES99932389T patent/ES2237123T3/es not_active Expired - Lifetime
  • 1999-07-12 DE DE69923227T patent/DE69923227T2/de not_active Expired - Lifetime
  • 1999-07-12 AR ARP990103369A patent/AR019367A1/es not_active Application Discontinuation
  • 1999-07-12 CN CNB998085081A patent/CN1167780C/zh not_active Expired - Fee Related
  • 1999-07-12 EP EP99932389A patent/EP1144578B1/en not_active Expired - Lifetime

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