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
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/08—Silicates
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/10—Carbonates ; Bicarbonates
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
  • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/3757—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions
  • C11D3/3761—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions in solid 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/38—Products with no well-defined composition, e.g. natural products
  • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
• • 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
  • C11D3/38—Products with no well-defined composition, e.g. natural products
  • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
  • C11D3/38609—Protease or amylase in solid compositions only
• • 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
  • C11D3/3942—Inorganic per-compounds

Definitions

• the enzymes in the detergent are maintained in a minimum exposure to moisture or water, the enzymes will suffer a degradation during storage which will result in a product that will have a decreased activity.
• the initial water content of the components of the composition should be as low a level as possible, and this low water content must be maintained during storage, since water will deactivate the enzymes. This deactivation will cause a decrease in the initial activity of the detergent composition.
• the detergent After the detergent container is opened, the detergent will be exposed to the environment which contains moisture. During each instance that the detergent is exposed to the environment it could possibly absorb some moisture. This absorption occurs by components of the detergent composition absorbing moisture, when in contact with the atmosphere. This effect is increased as the container is emptied, since there will be a greater volume of air in contact with the detergent, and thus more available moisture to be absorbed by the detergent composition. This will usually accelerate the decrease in the activity of the detergent composition.
• the most efficient way to keep a high activity is to start with an initial high activity of enzyme and to use components in the dishwashing composition which do not interact with the enzyme or which have a low water affinity which will minimize any losses in activity as the detergent is being stored or used.
• Powdered detergent compositions which contain enzymes can be made more stable and to have a high activity, if the initial free water content of the detergent composition is less than 10 percent by weight, more preferably less than 9 percent by weight and most preferably less than 8 percent by weight. Furthermore, the pH of a 1.0 wt% aqueous solution of the powdered detergent composition should be less than about 11.5 more preferably less than 11.0, and most preferably less than 10.5. This low alkalinity of the dishwashing detergent should maintain the stability of the detergent composition which contains a mixture of enzymes, thereby providing a higher initial activity of the mixture of the enzymes and the maintenance of this initial high activity.
• a major concern in the use of automatic dishwashing compositions is the formulation of phosphate-free compositions which are safe to the environment while maintaining superior cleaning performance and dish care.
• the present invention teaches the preparation and use of powdered automatic dishwashing compositions which are phosphate-free and have superior cleaning performance and dish care.
• This invention is directed to producing powdered phosphate-free enzyme-containing automatic dishwashing detergent compositions that have an increased chemical stability and essentially high at wash operating temperatures of 40°C to 65°C, wherein the composition also can be used as a laundry pre-soaking agent. This is accomplished by controlling the alkalinity of the detergent composition and using a unique mixture of enzymes.
• An alkali metal silicate is used in the powdered dishwashing detergent compositions.
• the preferred builder system of the instant compositions comprises a mixture of sodium carbonate and/or sodium citrate and a low molecular weight polyacrylic polymer.
• powder in this invention includes within its definition tablets, soluble capsules and soluble sachet. It is also possible to use the instant compositions as a laundry presoaking powder.
• French Patent No. 2,102,851 to Colgate-Palmolive pertains to rinsing and washing compositions for use in automatic dishwashers.
• the compositions disclosed have a pH of 6 to 7 and contain an amylolytic and, if desired, a proteolytic enzyme, which have been prepared in a special manner from animal pancreas and which exhibit a desirable activity at a pH in the range of 6 to 7.
• German Patent No. 2,038,103 to Henkel & Co. relates to aqueous liquid or pasty cleaning compositions containing phosphate salts, enzymes and an enzyme stabilizing compound.
• US Patent No. 3,799,879 to Francke et al teaches a detergent composition for cleaning dishes, with a pH of from 7 to 9 containing an amylolytic enzyme, and in addition, optionally a proteolytic enzyme.
• US Patent No 3,827,938, to Aunstrup et al. discloses specific proteolytic enzymes which exhibit high enzymatic activities in highly alkaline systems. Similar disclosures are found in British Patent Specification No. 1,361,386, to Novo Terapeutisk Laboratorium A/S. British Patent Specification No. 1,296,839, to Novo Terapeutisk Laboratorium A/S, discloses specific amylolytic enzymes which exhibit a high degree of enzymatic activity in alkaline systems.
• the aforementioned prior art fails to provide a powdered automatic dishwashing detergent which is phosphate-free and contains a mixture of enzymes for the simultaneous degradation of both proteins and starches, wherein the combination of enzymes have a maximum activity at a pH of less than 11 to 12 as measured by Anson method and the powdered automatic dishwashing detergent has optimized cleaning performance in a temperature range of 40°C to 65°C.
• the present invention relates to powdered automatic dishwashing detergent compositions which comprise a nonionic surfactant, alkali metal silicate, a phosphate-free builder system, optionally a peroxygen compound with activator as a bleaching agent and a mixture of an amylase enzyme and a protease enzyme, wherein said dishwashing composition comprises in percent by weight : wherein the powdered automatic dishwashing detergent composition has a pH of less than 10.5 in the washing liquor at a concentration of 10 grams per liter of water and the powdered dishwashing detergent composition exhibits high cleaning efficiency for both proteins and starches at a wash temperature of 40°C to 65°C.
• the nonionic surfactants that can be used in the present powdered automatic dishwasher detergent compositions are well known. A wide variety of these surfactants can be used.
• the nonionic synthetic organic detergents are generally described as ethoxylated propoxylated fatty alcohols which are low-foaming surfactants and are possibly capped, characterized by the presence of an organic hydrophobic group and an organic hydrophilic group and are typically produced by the condensation of an organic aliphatic or alkyl aromatic hydrophobic compound with ethylene oxide and/or propyleneoxide. (hydrophilic in nature). Practically any hydrophobic compound having a carboxy, hydroxy, amido or amino group with a free hydrogen attached to the oxygen or the nitrogen can be condensed with ethylene oxide or propylene oxide or with the polyhydration product thereof, polyethylene glycol, to form a nonionic detergent. The length of the hydrophilic or polyoxy ethylene chain can be readily adjusted to achieve the desired balance between the hydrophobic and hydrophilic groups.
• Typical suitable nonionic surfactants are those disclosed in US Patent Nos. 4,316,812 and 3,630,929.
• the nonionic detergents that are used are the low-foaming polyalkoxylated lipophiles wherein the desired hydrophile-lipophile balance is obtained from addition of an hydrophilic poly-lower alkoxy group to a lipophilic moiety.
• a preferred class of the nonionic detergent employed is the poly-lower alkoxylated higher alkanol wherein the alkanol is of 9 to 18 carbon atoms and wherein the number of moles of lower alkylene oxide (of 2 or 3 carbon atoms) is from 3 to 15.
• the higher alkanol is a high fatty alcohol of 9 to 11 or 12 to 15 carbon atoms and which contain from 5 to 15 or 5 to 16 lower alkoxy groups per mole.
• the lower alkoxy is ethoxy but in some instances, it may be desirably mixed with propoxy, the latter, if present, usually being major (more than 50%) portion.
• the alkanol is of 12 to 15 carbon atoms and which contain about 7 ethylene oxide groups per mole.
• Useful nonionics are represented by the low foam Plurafac series from BASF Chemical Company which are the reaction product of a higher linear alcohol and a mixture of ethylene and propylene oxides, containing a mixed chain of ethylene oxide and propylene oxide, terminated by a hydroxyl group. Examples include Product A(a C 13 -C l5 fatty alcohol condensed with 6 moles ethylene oxide and 3 moles propylene oxide). Product B (a C 13 -C 15 fatty alcohol condensed with 7 mole propylene oxide and 4 mole ethylene oxide), and Product C (a C 13 -C 15 fatty alcohol condensed with 5 moles propylene oxide and 10 moles ethylene oxide). Particularly good surfactants are Plurafac LF132 and LF 231 which are capped nonionic surfactants. Another liquid nonionic surfactant that can be used is sold under the tradename Lutensol SC 9713.
• Synperonic nonionic surfactant from ICI such as Synperonic LF/D25 are especially preferred nonionic surfactants that can be used in the powdered automatic dishwasher detergent compositions of the instant invention.
• Neodol 25-7 and Neodol 23-6.5 are made by Shell Chemical Company, Inc.
• the former is a condensation product of a mixture of higher fatty alcohols averaging about 12 to 13 carbon atoms and the number of ethylene oxide groups present averages 6.5.
• the higher alcohols are primary alkanols.
• Other examples of such detergents include Tergitol 15-S-7 and Tergitol 15-S-9 (registered trademarks), both of which are linear secondary alcohol ethoxylates made by Union Carbide Corp.
• the former is mixed ethoxylation product of 11 to 15 carbon atoms linear secondary alkanol with seven moles of ethylene oxide and the latter is a similar product but with nine moles of ethylene oxide being reacted.
• nonionic detergent also useful in the present compositions as a component of the nonionic detergent are higher molecular weight nonionics, such as Neodol 45-11, which are similar ethylene oxide condensation products of higher fatty alcohols, with the higher fatty alcohol being of 14 to 15 carbon atoms and the number of ethylene oxide groups per mole being about 11.
• higher molecular weight nonionics such as Neodol 45-11, which are similar ethylene oxide condensation products of higher fatty alcohols, with the higher fatty alcohol being of 14 to 15 carbon atoms and the number of ethylene oxide groups per mole being about 11.
• Neodol 45-11 are similar ethylene oxide condensation products of higher fatty alcohols, with the higher fatty alcohol being of 14 to 15 carbon atoms and the number of ethylene oxide groups per mole being about 11.
• Such products are also made by Shell Chemical Company.
• the number of lower alkoxies will usually be from 40% to 100% of the number of carbon atoms in the higher alcohol, preferably 40 to 60% thereof and the nonionic detergent will preferably contain at least 50% of such preferred poly-lower alkoxy higher alkanol.
• the alkyl polysaccharides are surfactants which are also useful alone or in conjunction with the aforementioned surfactants and have those having a hydrophobic group containing from 8 to 20 carbon atoms, preferably from 10 to 16 carbon atoms, most preferably from 12 to 14 carbon atoms, and polysaccharide hydrophilic group containing from 1.5 to about 10, preferably from about 1.5 to 4, and most preferably from 1.6 to 2.7 saccharide units (e.g., galactoside, glucoside, fructoside, glucosyl, fructosyl, and/or galactosyl units). Mixtures of saccharide moieties may be used in the alkyl polysaccharide surfactants.
• the number x indicates the number of saccharide units in a particular alkyl polysaccharide surfactant.
• x can only assume integral values.
• any physical sample can be characterized by the average value of x and this average value can assume non-integral values.
• the values of are to be understood to be average values.
• the hydrophobic group (R) can be attached at the 2-, 3-, or 4-positions rather than at the 1- position, (thus giving e.g. a glucosyl or galactosyl as opposed to a glucoside or galactoside).
• attachment through the 1-position i.e., glucosides, galactosides, fructosides, etc.
• additional saccharide units are predominately attached to the previous saccharide unit's 2-position.
• Attachment through the 3-, 4-, and 6-positions can also occur.
• the preferred alkoxide moiety is ethoxide.
• Typical hydrophobic groups include alkyl groups, either saturated or unsaturated, branched or unbranched containing from about 8 to about 20, preferably from 10 to 16 carbon atoms.
• the alkyl group is a straight chain saturated alkyl group.
• the alkyl group can contain up to 3 hydroxy groups and/or the polyalkoxide chain can contain up to 30, preferably less than 10, most preferably 0, alkoxide moieties.
• Suitable alkyl polysaccharides are decyl, dodecyl, tetradecyl, pentadecyl, hexadecyl, and octadecyl, di-, tri-, tetra-, penta-, and hexaglucosides, galactosides, lactosides, fructosides, fructosyls, lactosyls, glucosyls and/or galactosyls and mixtures thereof.
• the alkyl monosaccharides are relatively less soluble in water than the higher alkyl polysaccharides. When used in admixture with alkylpolysaccharides, the alkyl monosaccharides are solubilized to some extent.
• the use of alkyl monosaccharides in admixture with alkylpolysaccharides is a preferred mode of carrying out the invention. Suitable mixtures include coconut alkyl, di-, tri-, tetra-, and pentaglucosides and tallow alkyl tetra-, penta-, and hexaglucosides.
• the preferred alkyl polysaccharides are alkyl polyglucosides having the formula: wherein Z is derived from glucose, R is a hydrophobic group selected from the group consisting of alkyl, alkylphenyl, hydroxyalkylphenyl, and mixtures thereof in which said alkyl groups contain from 10 to 18, preferably from 12 to 14 carbon atoms; n is 2 or 3 preferably 2, r is from 0 to about 10, preferable 0; and x is from 1.5 to 8, preferably from 1.5 to 4, most preferably from 1.6 to 2.7.
• R 2 0H a long chain alcohol
• the alkylpolyglucosides can be prepared by a two step procedure in which a short chain alcohol (R 1 0H) an be reacted with glucose, in the presence of an acid catalyst to form the desired glucoside.
• the short chain alkylglucoside content of the final alkylpolyglucoside material should be less than 50%, preferably less than 10%, more preferably less than 5%, most preferably 0% of the alkylpolyglucoside.
• the amount of unreacted alcohol (the free fatty alcohol content) in the desired alkylpolysaccharide surfactant is preferably less than about 2%, more preferably less than 0.5% by weight of the total of the alkylpolysaccharide. For some uses it is desirable to have the alkyl monosaccharide content less than 10%.
• alkyl polysaccharide surfactant is intended to represent both the preferred glucose and galactose derived surfactants and the less preferred alkyl polysaccharide surfactants.
• alkyl polyglucoside is used to include alkyl- polyglycosides because the stereo chemistry of the saccharide moiety is changed during the preparation reaction.
• APG glycoside surfactant is APG 625 glycoside manufactured by the Henkel Corporation of Ambler, PA.
• APG 625 has: a pH of 6-8(10% of APG 625 in distilled water); a specific gravity at 25°C of 1.1 grams/ml; a density at 25°C of 9.1 kgs/gallons; a calculated HLB of 12.1 and a Brookfield viscosity at 35°C, 21 spindle, 5-10 RPM of 3,000 to 7,000 cps.
• the liquid nonaqueous nonionic surfactant is absorbed on a builder system which comprises a mixture of phosphate-free particles which is a builder salt and a low molecular weight polyacrylate type polymer such as a polyacrylate organic and/or inorganic detergent builders.
• a preferred solid builder salt is an alkali carbonate such as sodium carbonate or an alkali metal citrate such as sodium citrate or a mixture of sodium carbonate and sodium citrate. When a mixture of sodium carbonate and sodium citrate is used, a weight ratio of sodium citrate to sodium carbonate is 9:1 to 1:9, more preferably 3:1 to 1:3.
• builder salts which can be mixed with the sodium carbonate and/or sodium citrate are gluconates phosphonates and nitriloacetic acid salts.
• low molecular weight polyacrylates having a molecular weight of 1,000 to 100,000, more preferably 2,000 to 80,000.
• a preferred low molecular weight polyacrylate is Sokalan t mCP45 manufactured by BASF and having a molecular weight of 70,000.
• Another preferred low molecular weight polyacrylate is Acrysol t mLMW45ND manufactured by Rohm and Haas and having a molecularweightof4,500.
• Norasol t mWL2 comprises 26% LMW45ND sprayed on 74% soda ash.
• Sokalan t mCP45 is a copolymer of an acrylic acid and an acid anhydride. Such a material should have a water absorption at 38°C and 78 percent relative humidity of less than 40 percent and preferably less than 30 percent.
• the builder is commercially available under the tradename of Sokalan t mCP45. This is a partially neutralized copolymer of metacrylic acid and maleic anhydride sodium salt. Sokalan t mCP45 is classified as a suspending and anti-deposition agent. This suspending agent has a low hygroscopicity.
• Another builder salt is So- kalan t mCP5 having a molecular weight of 70,000.
• An objective is to use suspending and anti-redeposition agents that have a low hygroscopicity.
• Copolymerized polyacids have this property, and particularly when partially neutralized.
• Acusol t m640ND provided by Rohm Haas is another useful suspending and anti-redepositing agent.
• aluminosilicates both of the crystalline and amorphous type.
• Various crystalline zeolites i.e. alumino-silicates
• alumino-silicates are described in British Patent No. 1,504,168, U.S. Patent No. 4,409,136 and Canadian Patent Nos. 1,072,835 and 1,087,477.
• An example of amorphous zeolites useful herein can be found in Belgium Patent No. 835,351.
• the zeolites generally have the formula
• x is 1, y is from 0.8 to 1.2 and preferably 1, z is from 1.5 to 3.5 or higher and preferably 2 to 3 and w is from 0 to 9, preferably 2.5 to 6 and M is preferably sodium.
• a typical zeolite is type A or similar structure, with type 4A particularly preferred.
• the preferred aluminosilicates have calcium ion exchange capacities of about 200 milliequivalents per gram or greater, e.g. 400 meq/g.
• the alkali metal silicates are useful anti-corrosion agents which function to make the composition anticorrosive to eating utensils and to automatic dishwashing machine parts.
• the preferred silicates are sodium disilicate (anhydrous), sodium disilicate (hydrated) and sodium metasilicate and mixtures thereof, wherein the preferred silicate is hydrated disilicate.
• any compatible anti-foaming agent can be used.
• Preferred anti-foaming agents are silicone anti-foaming agents. These are alkylated polysiloxanes and include polydimethyl siloxanes, polydiethyl siloxanes, polydibutyl siloxanes, phenyl methyl siloxanes, dimethyl silinated silica, trimethysilanated silica and trie- thylsilanated silica.
• a suitable anti-foaming agent is Silicone TP-201 from Union Carbide.
• Suitable anti-foaming agents are Silicone DB700 used at 0.2 to 1.0 percent by weight, sodium stearate used at a concentration level of 0.5 to 1.0 weight percent, and LPKN 158 (phosphoric ester) sold by Hoechst used at a concentration level of 0 to 1.5 weight percent, more preferably 0.1 to 1.0 weight percent.
• the perfumes that can be used include lemon perfume and other natural scents.
• any opacifier that is compatible with the remaining components of the detergent formulation can be used
• a useful and preferred opacifier is titanium dioxide at a concentration level of 0 to 1.0 weight percent.
• a key aspect is to keep the free water (non-chemically bonded water) in the detergent composition at a minimum. Absorbed and adsorbed water are two types of free water, and comprise the usual free water found in a detergent composition. Free water will have the affect of deactivating the enzymes.
• the detergent composition of the present invention includes a peroxygen bleaching agent at a concentration level of about 0 to about 20 weight percent, more preferably 0.5 to 17 weight percent and most preferably at 1.0 to 14 weight percent.
• the oxygen bleaching agents that can be used are alkali metal perborate, percarbonate, perphthalic acid, perphosphates, and potassium monopersulfate.
• a preferred compound is sodium perborate monohydrate.
• the peroxygen bleaching compound is preferably used in admixture with an activator at a concentration level of 1-5 wt. percent. Suitable activators are those disclosed in U.S. Patent No. 4,264,466 or in column 1 of U.S. Patent No. 4,430,244. Polyacetylated compounds are preferred activators. Suitable preferred activators are tetraacetyl ethylene diamine ("TAED”), pentaacetyl glucose and ethylidenebenzoate acetate.
• TAED tetraacetyl ethylene di
• the activator usually interacts with the peroxygen compound to form a peroxyacid bleaching agent in the wash water.
• the detergent formulation also contains a mixture of a proteolytic enzyme and an amylotytic enzyme and, optionally, a lipolytic enzyme that serve to attack and remove organic residues on glasses, plates, pots, pans and eating utensils.
• Proteolytic enzymes attack protein residues, lipolytic enzymes fat residues and amylolytic enzymes starches.
• Proteolytic enzymes include the protease enzymes subtilism, bromelin, papain, trypsin and pepsin.
• Amylolytic enzymes include amylase enzymes.
• Lipolytic enzymes include the lipase enzymes.
• the preferred amylase enzyme is available under the name Maxamyl, derived from Bacillus licheniformis and is available from Gist-brocades of the Netherlands available in the form of a prill having an activity of about 6,000 TAU/g.
• One of the preferred protease enzyme is available under the name Maxacal derived from Bacillus al- calophilus, and is supplied by Gist-brocades, of the Netherlands in a prill form (activity of about 329KADU/g.).
• Preferred enzyme activates per wash are Maxacal-300-700 KADU per wash and Maxamyl-2,000 to 4,000 TAU per wash.
• Another preferred protease enzyme is available under the name Maxatase derived from a novel Bacillus strain designated "PB92" wherein a culture of the Bacillus is deposited with the Laboratory for Microbiology of the Technical University of Delft and has a number OR-60, and is supplied by from Gist-Brocades, of the Netherlands in a prill form activity of about 40,000 DU/g.).
• Preferred enzyme activates per wash are Maxatase 250-600 KDU per wash.
• Maxapen 15, Maxapen 30 or Maxapen 42 are high alkaline mutant proteolytic enzyme derived from Bacillus alcalophylus, and is supplied by from Gist- Brocades, of the Netherlands in a prill form (activity of about 400,000 ADU/g.).
• Preferred enzyme activates per wash are Maxapem 15 or 42 of 50-100 MPU per wash or Maxapem 30 of 100-200 MPU per wash, and Maxamyl-4,000-8,000 TAU per wash,wherein the Maxapem 15,30 or 42 exhibits improved resistance to activated oxygen (perborate) agents which can be used in the instant composition.
• the alkali metal silicate which is a corrosion inhibitor, wherein sodium disilicate is preferred, will be present in an amount about 3 to about 40 percent by weight and more preferably about 4 to about 28 percent by weight.
• the opacifier will be present in an amount of about 0 to about 1.0 percent by weight, more preferably about 0.1 to about 7 percent by weight and most preferably about 0.4 percent by weight.
• the enzymes will be present in an amount in a prill form as supplied by Gist-Brocades at a concentration of about 0.8 to 22.0 percent by weight, more preferably about 0.9 to 20.0 percent by weight, and most preferably about 1.0 to about 18.0 percent by weight.
• the protease enzyme prills in the automatic dishwashing composition will comprise about 0.5 to about 15.00 percent by weight, more preferably about 0.7 to about 13.0 weight percent and most preferably about 0.8 to about 11.0 percent by weight.
• the amylase enzyme prills will comprise about 0.3 to about 8.0 percent by weight, more preferably about 0.4 percent to about 7.0 weight percent and most preferably about 0.5 to about 6.0 weight percent.
• the lipase enzyme will comprise about 0.00 to about 8.0 percent by weight of the detergent composition.
• a typical lipase enzyme is Lipolase 100 T from Novo Corporation.
• the lipase enzymes are especially beneficial in reducing grease residues and related filming problems on glasses and dishware.
• Another useful lipase enzyme is Amano PS lipase provided by Amano International Enzyme Co., Inc.
• perfumes will comprise about 0.1 to about 5.0 percent by weight of the detergent composition.
• One method of producing the powder detergent formulation having a bulk density of about 0.8 is to spray dry by any conventional means the nonionic surfactant and defoamer onto the perborate bleach compound and the builder salt.
• This spray dry materials can be used immediately, but it is preferred to age it for 24 hours.
• the spray dried materials are dry blended in any suitable conventional blender such as a tumble blender at about room temperature with the other ingredients of the composition until a homogenous blend is obtained.
• the weight ratio of the proteolytic enzyme to the amylolytic enzyme in prill form in the powdered automatic dishwasher detergent compositions is 6:1 to 1:1, and more preferably 4.5:1 to 1.1:1.
• the detergent composition can have a fairly wide ranging composition.
• the surfactant can comprise 1 to 15 percent by weight of the composition, and most preferably about 1 to 12 percent by weight.
• the anti-foaming agent will be present in an amount of about 0 to about 1.5 percent by weight, more preferably about 0.1 to about 1.2 percent by weight and most preferably about 0.1 to about 1 percent by weight.
• the builder system which is preferably sodium carbonate and/or sodium citrate is present in an amount of 2 to 40 percent by weight, more preferably 4 to 40 percent by weight and most preferably 5 to 30 percent by weight.
• the builder system also preferably contains the low molecular weight polyacrylate type polymer at a concentration level of about 0 to 20 weight percent, more preferably 1.0 to 17 weight percent and most preferably a to 17 weight percent.
• One method of producing the powder detergent formulation having a bulk density of 0.8 is to spray dry by any conventional means the nonionic surfactant and defoamer onto the perborate bleach compound and the builder salt.
• This spray dry materials can be used immediately, but it is preferred to age it for 24 hours.
• the spray dried materials are dry blended in any suitable conventional blender such as a tumble blender at about room temperature with the other ingredients of the composition until a homogenous blend is obtained.
• compositions also can be produced as low density powders according to the procedure as set forth in U.S. Patent 4,931,203, wherein these powders have a bulk density less than the bulk density of the bulk density of the standard powders which have a bulk density of about 0.8 kg/liter.
• the concentrated powdered nonionic automatic dishwashing detergent compositions of the present invention disperses readily in the water in the dishwashing machine.
• the presently used home dishwashing machines have a measured capacity for 80 cc or 90 grams of detergent. In normal use, for example, for a full load or dirty disches 60 grams of powdered detergent are normally used.
• the normal operation of an automatic dishwashing machine can involve the following steps or cycles washing, rinse cycles with cold water and rinse cycles with hot water.
• the entire wash and rinse cycles require about 60 minutes.
• the temperature of the wash water is 40°C to 65°C and the temperature of the rinse water is 55°C to 65°C.
• the wash and rinse cycles use 4 to 7.5 liters of water for the wash cycle and 4 to 7.5 liters of water for the hot rinse cycle.
• the highly concentrated powdered automatic dishwashing detergent compositions exhibit excellent cleaning properties and because of the high concentration of the detergent in the composition, the detergent is not totally consumed during the wash cycle or totally eliminated during the rinse cycle such that there is a sufficient amount of detergent remaining during the rinse cycle to substantially improve the rinsing.
• the washed and dried dishes are free of undesirable traces, deposits or film due to the use of hot water in the rinse cycle.
• the instant compositions do not contain clays such as bentonites and laponites; the addition of these types of clay to the instant composition would cause an increased spotting of glassware during the washing cycle.
• the concentrated powdered nonionic surfactant detergent composition was formulated from the following ingredients in the amounts specified according to the previously defined and described dry blending process.
• Formulas (A-I) of Example 1 were tested in a European style Philips 664 Dishwasher working at 55°C with a charge of 15.0 grams per wash of the Formulas (A-I) and 3 mi./per wash of commercial Galaxy rinse aid sold by Colgate-Palmolive Co.
• the load of items placed in the dishwasher consisted of 6 plates soiled with 3.0 grams of a mixture of 12.0 grams of porridge oats with 188 grams of water and 3 plates soiled with 0.4 grams of calcium chloride denaturated egg yolk and three plates soiled with 5 grams of a microwave oven baked mixture of 177 grams of egg yolk with 50 grams of margarine and 3 cups soiled with tea after overglaze removal wherein all the plates and cups were dried prior to being placed in the dishwasher.
• the pH of the washing bath and the formulation were measured.
• the hardness of the rinse water was 38 (C a C0 3 ) ppm.
• Each formulation was evaluated for spotting and filming. The results were evaluated on a scale of 1 to 10 with the higher number being the better result.
• compositions of the invention were evaluated for performance according to the following laboratory test methods.
• Oatmeal soil was prepared by boiling 24 grams of Quaker oats in 400 ml of tap water for ten minutes and then homogenized with a high shearing device (Ultrawax). Three grams of this mixture was spread as thin film onto 7.5 inch china plates. The plates were aged for 2 hours at 80°C, and then stored overnight at room temperature. Hardened egg soil was prepared by mixing egg yolk with an equal amount of 2.5N calcium chloride solution. 0.4 grams of this mixture was applied as a thin crosswise film to the usable surface of 7.5 inch china plates. Microwave-egg soil was prepared by mixing hot egg yolk and cooked margarine with a homogenizer (Ultraturax device).
• the dishwasher load included each run six plates of oatmeal, three cups soiled with tea, one dish of white sauce, one dish of rice, four glasses soiled with tomato juice, four glasses soiled with cocoa, and four soiled with milk.
• Pieces of cutlery forks, knives and spoons, six each) were also included and soiled with porridge soil, rice and rice with cheese soils.
• the dishwasher load included six clean plates in the lower basket and six clean glasses in the upper basket.
• the soil load was consisting of 100 grams of a greasy soil mixture prepared by mixing mustard (42 weight %) white vinegar (33 wt. %), corn oil (15 wt. %), and lard (10 wt. %) altogether.
• glasses were scored in a viewing box for filming and spotting and under natural lighting for 966d aspect according to the same 0 (bad performance) to 10 (perfectly clean glasses) scale as for the so-called soil cleaning test with the aid of reference glasses.
• the concentrated powdered nonionic surfactant detergent composition was formulated from the following ingredients in the amounts specified according to the previously defined and described dry blending process.
• Formulas (A-N) of Example 111 were tested in a European style Philips 664 Dishwasher working at 55°C with a charge of 15.0 grams per wash of the Formulas (A-N) and 3 mi./per wash of commercial Galaxy rinse aid sold by Colgate-Palmolive Co.
• the load of items placed in the dishwasher consisted of 6 plates soiled with 3.0 grams of a mixture of 12.0 grams of porridge oats with 188 grams of water and 3 plates soiled with 0.4 grams of calcium chloride denaturated egg yolk and three plates soiled with 5 grams of a microwave oven baked mixture of 177 grams of egg yolk with 50 grams of margarine and 3 cups soiled with tea after overglaze removal wherein all the plates and cups were dried prior to being placed in the dishwasher.
• the pH of the washing bath and the formulation were measured.
• the hardness of the rinse water was 38 (C 2 CO 3 ) ppm.
• Each formulation was evaluated for spotting and filming. The results were evaluated on a scale of 1 to 10 with the higher number being the better result.
• compositions of the invention were evaluated for performance according to the following laboratory test methods.
• Oatmeal soil was prepared by boiling 24 grams of Quaker oats in 400 ml of tap water for ten minutes and then homogenized with a high shearing device (Ultrawax). Three grams of this mixture was spread as thin film onto 7.5 inch china plates. The plates were aged for 2 hours at 80°C, and then stored overnight at room temperature. Hardened egg soil was prepared by mixing egg yolk with an equal amount of 2.5N calcium chloride solution. 0.4 grams of this mixture was applied as a thin crosswise film to the usable surface of 7.5 inch china plates. Microwave-egg soil was prepared by mixing hot egg yolk and cooked margarine with a homogenizer (Ultraturax device).
• the dishwasher load included each run six plates of oatmeal, three cups soiled with tea, one dish of white sauce, one dish of rice, four glasses soiled with tomato juice, four glasses soiled with cocoa, and four soiled with milk.
• Pieces of cutlery forks, knives and spoons, six each) were also included and soiled with porridge soil, rice and rice with cheese soils.
• the dishwasher load included six clean plates in the lower basket and six clean glasses in the upper basket.
• the soil load was consisting of 100 grams of a greasy soil mixture prepared by mixing mustard (42 weight %) white vinegar (33 wt. %), corn oil (15 wt. %), and lard (10 wt. %) altogether.
• glasses were scored in a viewing box for filming and spotting and under natural lighting for 966d aspect according to the same 0 (bad performance) to 10 (perfectly clean glasses) scale as for the so-called soil cleaning test with the aid of reference glasses.
• the concentrated powdered nonionic surfactant detergent composition was formulated from the following ingredients in the amounts specified according to the previously defined and described dry blending process.

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• 1992
  • 1992-05-14 AU AU16305/92A patent/AU656375B2/en not_active Ceased
  • 1992-05-29 EP EP19920401474 patent/EP0516553A3/en not_active Withdrawn

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