Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/06—Phosphates, including polyphosphates
  • C11D3/062—Special methods concerning phosphates
• • 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
  • C11D17/0034—Fixed on a solid conventional detergent ingredient
• • 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

Definitions

• the present invention relates to an improved auto­matic dishwashing detergent powder with superior performance solubility, pourability, handling and storage characteristics and method for making and using same.
• automatic dishwashing detergent powders contain water soluble builder salt, water-soluble silicate, bleach, preferably a water-soluble chlorine bleaching agent, and water-soluble detergent which is usually an organic, low-­foaming (i.e. low "sudsing") non-ionic.
• the compositions are usually formulated with alkaline salts (i.e. sodium and potassium).
• alkaline salts i.e. sodium and potassium.
• the automatic dishwashing compositions In the normal environment in the dishwashing machine, the automatic dishwashing compositions generally yield a pH in the range of about 9.0 to 12.0 and more generally about 9.5 to 11.5.
• the alkaline builder salts which have been used are both of the inorganic type (e.g.
• pyrophosphates carbonates, silicates and so forth
• organic type e.g. amino­carboxylates such as trisodium nitrilotriacetate, tetrasodium ethylene diamine tetra-acetate, sodium citrate, sodium itaconate, sodium polymaleate, sodium inter polymaleates, such as maleic­acrylic (or vinyl) interpolymers, sodium oxydisuccinate and so forth.
• the builder generally function to increase the clean­ing action of the composition by supplying alkalinity and also by removing (i.e. "sequestering") ions which affect the action and efficiency of the organic detergent.
• the silicates which have been used are those wherein the Na2O:SiO2 ratio varies from 2:1 to 1:4 and more generally from about 1:1 to about 1:3.4, typically 1:1, 1:2 and 1:2.4.
• the bleach employed is generally a chlorine-yielding agent and has been used in varying amounts but generally to give available chlorine levels of from about 0.3% to about 10% and, more often, levels of about 1% to 5%.
• Typical bleaches are the inorganic types such as sodium, lithium and calcium hypochlorite, and chlorinated trisodium phosphate, as well as the organic forms such as the di- and tri- chlorocyanuric acids and their alkali (e.g. sodium and potassium) metal salts, N-chloracetyl urea, 1,3-dichloro-5,5-dimethylkydantion, etc.
• nonionic detergents in common usage have been any of the conventional hydrophobe moieties (e.g. C8 to C20 alcohols, phenols, amides, acids, etc.) reacted with ethylene oxide (or mixtures with other oxyalkylating agents such as propylene oxide or butylene oxide).
• Typical nonionics used have been n-dodecanol with 10 moles of ethylene oxide; tetradecyl alcohol-hexadecyl alcohol (1:1 weight ratio) with 5, 10, 15 or 20 moles of ethylene oxide; polyoxypropylenes condensed (i.e.
• non-ionic detergent disclosed as generally useful in auto­matic dishwashing compositions can be found in U.S. Patents 3314891, 3359207, 2677700, 2979528, 3036118, 3382176, 4115308 and 4411810.
• Automatic dishwashing detergents have been provided in two basic forms, as powders and as “liquids” (or semi-­liquids or pastes).
• the powders represent the “first generation”. They are simple to formulate, easy to dispense from machines which have, in the main , been designed to handle powders and not liquids; and because of the presence of the formulation "actives" in solid state, (and usually the components comprise separate and discrete particles), there is a minimum of inter­action among the composition ingredients.
• "Liquids,” the so-­called “second generation” of products in this area are more convenient to dispense from the package; also they are generally more soluble in water and therefore have less tendency to remain and/or leave residues in the machine dispenser cup. Phase separation leading to decreased homo­geneity and an exacerbation of component interaction are among some of the minuses of the liquid system.
• the present invention relates to an improved auto­matic dishwashing detergent in powder form which is highly efficacious, has superior stability, is phase stable and homogeneous and notwithstanding its powder characteristic has many of the advantages of the liquid systems i.e. dispensibility, pourability and solubility without, however, the problems and disadvantages often attending the use of liquid automatic dish­washing compositions.
• compositions of this invention comprise builder salt, generally alkaline builder salt, alkali-metal silicate, non-ionic surfactant and as a preferred optional ingredient, bleaching agent.
• the product is characterized by a base bead of builder salt having absorbed thereon the nonionic surfactant, said bead being admixed with the silicate and bleach (where used). Where other optional materials are used they, too, are conveniently post blended with the base beads.
• These materials may be alkali salts including builder salts anti-oxi­dants, dyes, pigments, fragrances, anti-foamers, fillers, se­questering agents, soil suspending agents, drainage improvers and the like.
• the present invention relates to an improved and superior automatic dishwahing detergent composition in powder form which is free flowing, non-caking, homogeneous, highly soluble and very low, if not entirely free of insolubles and residue when in use, and methods for making and using such compositions.
• the outstanding automatic dishwashing compositions which are provided are powders and comprise a base material on which is absorbed or "loaded” a detergent, and in admixture therewith an alkaline silicate and any other desired components.
• a bleaching agent and alkaline reacting compounds such as alkali carbonates, bicarbonates, borates, hydroxides and so forth.
• the base material which is the carrier for the surfact­ant is a spray-dried phosphate composition which also con­tains a small amount of a polymeric substance.
• the spray-dried base is generally characterized as a "base bead" although it may not necessarily be a bead in the usual geometric form.
• the absorbent base material is com­prised of a major portion of inorganic salts and generally and preferably phosphate material.
• Suitable phosphates include trisodium phosphate, sodium tripolyphosphate, monobasic sodium phosphate, dibasic sodium phosphate, dibasic sodium pyrophosphate, tetra sodium pyrophosphate, sodium hexametaphos­phate and the like.
• the corresponding potassium salts along with mixtures of sodium and potassium salts are useful.
• the base "bead” is prepared by spray-drying a slurry of the phosphate-containing composition. The processing of slurries and spray-drying them to form base beads is described in U.S. Patent 441429 to David Joshi and the entire disclosure of this patent is incorporated herein by reference thereto.
• the base material will generally comprise from about 50 to 95% alkali-metal polyphosphate.
• the base may comprise from about 50% to 99% of inorganic salts and again, preferably alkali metal polyphosphate. Minor amounts of moisture are almost invariable present and the water content may vary from a few or less percent (e.g. 0.5%, 1%, 2%, 3%) to 20% & more but more generally from about 5% to 15%, typically 6%, 8%, 10% and 12%.
• alkaline salts particularly sodium carbonate, sodium tetraborate and sodium silicate may be admixed with the phosphate in the crutcher before spray-drying.
• these materials are used in less than major amounts, generally from very small amounts e.g. 1%, 2%, 5%, up to larger quantities, typically 10%, 15%, 20%, 30%, 35% & 40%.
• silicate is used in the crutcher mix it is usually one of lesser alkalinity e.g. Na2O:SiO2 ratio of about 1:1.6 to 1:3.4 typically 1:2.4.
• a second essential component of the base bead is a water-soluble polymeric material such as sodium polyacrylate, which is the most preferred polymer salt.
• water-soluble polymers at least soluble in such salt form
• poly (hydroxy) aerylates copolymers and inter polymers of acrylic acid with other copolymerizable monomers (usually B-olefinically un­saturated)
• vinyl pyrrolidone vinyl acetate
• hydrolized polyvinyl acetate 75-95% polyvinyl alcohol
• acrylamide methyl vinyl ether and so forth
• Other polymers include water-soluble forms of starch and cellulose and particularly derivatives such as sodium carboxy methylcellulose and the like.
• Natural proteins are useful, too; examples include gelatin and the like.
• the useful materials are characterized by water-solubility and compatibility to form a base carrier suitable for loading the detergent in quantities from 1 to about 10% and where described up to quantities of 25-35%.
• Such polymers are useful in amounts of from about 0.5% to about 10% and preferably from about 1% to 8%. Typical usage would be 1.5%, 2%, 2.5%, 3%, and 4%, especially with sodium poly­acrylate.
• the molecular weights of the synthetic polymers may vary from several hundred to several million, e.g. 600; 1200; 2000; 5000; 150,000; 500,000; 1,000,000; 5,000,000 and the like.
• the based bead After the based bead has been prepared, it is used as an absorbent or carrier for the detergent.
• the latter are preferably non-ionic surfactants which, in liquid form are sprayed on to the base beads.
• the more desirable non-ionic detergent materials are generally pasty to waxy at room temper­ature or at least sprayable as a liquid at somewhat elevated temperatures e.g. 30°C, 40°C, 60°C, 80°C and 100°C.
• the nonionic detergent materials comprise any of the class designated as nonionic and generally comprises the oxyalhylated derivatives (preferably oxyethyl or mixed oxpropyl-­oxyethyl) of hydrophobic base moieties of about C8 to C30 carbon content of such functional types as alcohols, thioalcohols, esters, acids and amides.
• the preferred compounds are oxyethy­lated and mixed oxypropylated-oxyethylated aliphatic alcohols of C10 to C18.
• the non-ionic detergents are the preferred types because of their physical characteristics; liquifiable and sprayable as well as low foaming; one of the major character­istics of a detergent which adversely affects the cleaning ef­ficacy of the dishwashing composition is a high level of foam. This is due primarily to the fact that the cleaning action is proportional to the force of the jets of water impinging on the dishes, etc., and high levels of foam and thick or dence foam reduce this force and thusly the cleaning action.
• R hydrogen or C10 to C18 alkyl and preferably linear alkyl.
• R is hydrogen the oxyalkyl groups are oxypropyl as a hydrophobe backbone with oxyethyl or oxyethyl and oxypropyl terminating groups.
• Illustrative compounds include:
• the amount of nonionic may range from a few percent up to 35 to 40% on a weight for weight basis. It is preferred to at least about 3 to 4%. Typical amounts would be 4%, 6%, 8% and in some embodiments 20%, 25% and 30%. Where high non-ionic loading is desired, then it is preferred to utilize some of the formula in organic polyphosphate as post added anhydrous (or very low moisture content e.g. 1%, 2% or 3%).
• silicate at least as a major replacement for the polymer if not as only a minor replacement for the polymer materials, and the silicate where employed in this invention for its alkalinity and anti-corrosive benefits is best utilized as a post added component.
• silicates which are used in the compositions of the present invention and particularly those which are post added as powders comprise any of the commercially available alkali silicates available as powders, wherein the Na2O to to SiO2 molar ratio varies from 2:1 to 1:4 and preferably varies from 1:1 to 1:3.5.
• Typical and most preferred silicates are sodium and potassium silicates where the Na2O to SiO2 molar ratio varies from 1:1 to 1:2.5 and especially the metasilicates (1:1 ratio).
• the physical form of the particulate silicate may be any form i.e. any density, porosity, shape and particle size.
• densities may range from a bulk density of 0.3 to one of 1.5 and preferably 0.4 or 0.5 to 0.7 or 0.8, 0.9 or 1.0.
• Typical particle sizes for the post added silicates may be a product of 20, 30, 40, 50, 60 mesh.
• a commercially available product with 80-85% or more between 40 & 60 mesh is very useful.
• a product with 84% between 10 & 65 mesh is excellent.
• One additional and particularly outstanding char­acteristic and feature of one aspect of the the compositions of this invention is their relative low bulk density as compared to the usual commercial products.
• commercial products may have densities of the order of 0.8 those of the present invention may be made having 20 to 50% less density.
• the silicates used may be in the form of beads, hollow or otherwise, finely divided powder, regular and irregular and diverse shaped particles. Particularly pre­ferred silicates are available as Metsobeads from PQ Corpor­ation and Britesil LD24. Mixtures of any of the foregoing may also, of course, be used.
• the amount of silicate used may vary from a few percent to a significant and almost major amount such as 2%, 3% and 5% to 10%, 15%, 20%, 30% and 40%. Particularly preferred ranges are 5% to 25% and 5% to 15%.
• the optional bleach which, however, is highly desirable and preferred can be any of those conventionally used in auto­dish compositions.
• the chloride bleaches described earlier in the "Background of the Invention and Prior Art" section can also be used in this invention. Similar amounts may be used as e.g. 0.3% to about 10%, preferably 1% to 5% (by weight).
• oxygen bleaches such as sodium perborate mono­hydrate, sodium perborate tetrahydrate, sodium persulfate, sodium percarbonate and so forth. Oxygen bleach levels may range from about 2% to 40 or 50% and preferably from about 5% to 30%.
• bacteriocides enzymes e.g. boric acid anhydride
• sheeting agents e.g. talc, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin,
• TPP anhydrous sodium tripolyphosphate powder
• sodium polyacrylate powder is prepared at 45% solids level handled and spray dried as in Example 1 of Joshi U.S. Patent 4414129.
• the TPP comprises 89.55%, the polyacrylate 2.45% and the balance of 8% is moisture in the bead.
• the bead has a specific gravity of 0.5 and has considerable mechanical strength.
• the beads so produced are introduced into a rotary drum and post sprayed with a nonionic surfactant (liquefied) at a temperature of 120°F until 6% by weight of the nonionic has been "loaded” on the carrier beads.
• the non-ionic is a C12-C14 linear alcohol containing about 55% of random oxyethyl and oxypropyl groups (42 wt. % oxyethyl - 58 wt. % oxypropyl groups). These groups are introduced into the alcohol using a mixed ethylene oxide - propylene oxide stream.
• the beads at the time of spraying are at a temperature of about 100° to 105°F. (38 to 41°C).
• Example I is repeated except that the beads are loaded with 25% by weight of the non-ionic and the composition is varied somewhat to have the following components: WT. % Based Beads of Ex. 1 60.0 Sodium metasilicate* 12.0 Sodium carbonate of Ex. 1 10.0 Nonionic of Ex. 1 15.0 C1. bleach of Ex. 1 3.0 100.0% *the metasilicate used here is a high bulk density product (50 lbs/ft3)
• Example II is repeated except that the amount of base beads is only 50% (and, therefore, non-ionic is only 12.5%).
• the additional "hole” of 12.5% in the formula is filled with sodium tripolyphosphate (anhydrous) which is post mixed and blended into the formula with the metasilicate, carbonate and bleach.
• the usual equipment may be used. Examples include Patterson Kelly twin shell blender for bath operation and a Patterson Kelly Ziq-Zag blender for continuous processing.

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Citations (1)

• 1989
  • 1989-02-15 NZ NZ228002A patent/NZ228002A/en unknown
  • 1989-02-15 EP EP89102553A patent/EP0330060A3/fr not_active Withdrawn
  • 1989-02-16 ZA ZA891223A patent/ZA891223B/xx unknown
  • 1989-02-16 IL IL89309A patent/IL89309A/xx not_active IP Right Cessation
  • 1989-02-17 AU AU30050/89A patent/AU3005089A/en not_active Abandoned
  • 1989-02-20 PT PT89765A patent/PT89765A/pt not_active Application Discontinuation
  • 1989-02-21 MX MX015005A patent/MX169823B/es unknown
  • 1989-02-24 AR AR89313283A patent/AR243226A1/es active
  • 1989-02-24 BR BR898900843A patent/BR8900843A/pt not_active Application Discontinuation
  • 1989-02-24 NO NO89890802A patent/NO890802L/no unknown
  • 1989-02-24 CA CA000591996A patent/CA1326621C/fr not_active Expired - Fee Related
  • 1989-02-24 DK DK090389A patent/DK90389A/da not_active Application Discontinuation
  • 1989-02-27 JP JP1046367A patent/JPH01304200A/ja active Pending

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