WO1992002611A1 - Fabrication de compositions detergentes solides, moulees et resistant au gonflement - Google Patents

Fabrication de compositions detergentes solides, moulees et resistant au gonflement Download PDF

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Publication number
WO1992002611A1
WO1992002611A1 PCT/US1991/005162 US9105162W WO9202611A1 WO 1992002611 A1 WO1992002611 A1 WO 1992002611A1 US 9105162 W US9105162 W US 9105162W WO 9202611 A1 WO9202611 A1 WO 9202611A1
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WIPO (PCT)
Prior art keywords
composition
mixture
cast
dual
swelling
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Application number
PCT/US1991/005162
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English (en)
Inventor
John J. Rolando
Stephen A. Morganson
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Ecolab Inc.
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Publication date
Application filed by Ecolab Inc. filed Critical Ecolab Inc.
Publication of WO1992002611A1 publication Critical patent/WO1992002611A1/fr

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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
    • C11D3/10—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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0052—Cast detergent 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
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/06—Phosphates, including polyphosphates
    • C11D3/062—Special methods concerning phosphates

Definitions

  • the invention relates to the manufacture of solid, cast cleaning compositions which tend to swell after casting. More specifically, the invention relates to the manufacture of solid, cast cleaning compositions which contain a hydratable chemical capable of forming various hydrated forms with significantly different delttr ⁇ t ⁇ es so as to avoid transformation of the hydratable chemical between the various hydrate forms after casting.
  • Solid blocks of alkaline detergent compositions are widely used for household and institutional dishwashing, laundering and general surface cleaning.
  • the manufacturing process employed to produce such solid cast blocks of detergent typically involves heating an aqueous emulsion of the individual components to form a molten melt, blending the molten melt to form a homogeneous mixture, and then casting, cooling and solidifying the homogeneous mixture within a container from which the composition is to be stored, shipped and dispensed.
  • alkaline builder such as an alkali metal carbonate and/or an alkali metal phosphate.
  • alkaline builders are known to be effective for maintaining the detergent solution at an alkaline pH and assisting in the removal of soils from various substrates.
  • Swelling of a solid, cast, detergent composition which contains a hydratable chemical capable of forming a high density and a low density hydrate may be significantly reduced by cooperatively controlling both the concentration of the dual hydratable chemical, based upon the amount of dual hydratable chemical and water, and the processing temperature so as to minimize formation of the higher density hydrate of the dual hydratable chemical during processing.
  • a process for preparing such a non-swelling, solid, cast, detergent composition comprises the step of combining (i) about 10 to about 50 wt% of a dual hydratable alkaline chemical capable of forming a high density and a low density hydrate under different conditions, (ii) about 10 to about 50 wt% water, and (iii) an effective detersive amount of an operative detergent component under conditions which consistently provide a substantially non-swelling cast composition.
  • Typical dual alkaline hydratable chemicals utilized in detergent compositions include specifically, but not exclusively, sodium carbonate and trisodium phosphate.
  • the processing temperature of a saturated solution of the sodium carbonate should be maintained below about 105°F with the concentration of sodium carbonate maintained below 46 wt%. Based upon the processing temperature required to produce a castable composition and the performance benefits obtained by incorporating a major proportion of sodium carbonate, the processing temperature is preferrably maintained between about 90° and 105°F with the concentration of the sodium carbonate maintained between about 32 and 46 wt%, based upon the sodiunj carbonate and water. - ⁇ "---
  • Figure 1 is a schematic diagram depicting a three- stage process useful for practicing the process of the present invention.
  • Figure 2 is a phase diagram for the various hydration states of sodium carbonate.
  • a “dual hydratable alkaline chemical” refers to those hydratable chemicals capable of forming at least one high density hydrate form and at least one low density hydrate form under different conditions wherein the highest density is at least 20% greater than the lowest density.
  • the erm "wt%" refers to the weight proportion based upon the total weight of the composition unless otherwise specified.
  • hydratable chemicals frequently utilized in the formulation of detergent compositions are capable of forming-both a high density and a low density Kyc ⁇ rate under those conditions commonly encountered in the processing and orage of solid cast detergent compositions.
  • a list of such dual hydratable chemicals includes specifically, but not exclusively, the alkaline detergent builders sodium carbonate and trisodium phosphate. The hydrates and associated densities of these dual hydratable compounds are set forth below.
  • the higher density anhydrous and/or monohydrate forms of sodium carbonate begin to form under saturated conditions, such as encountered in the manufacture of solid cast detergent compositions, when either (i) the concentration of sodium carbonate, based upon sodium carbonate and water, is greater than about 32 wt% and the temperature of the composition exceeds about 105 C F, or (ii) the concentration of sodium carbonate, based upon sodium carbonate and water, is greater than about 46 wt%, regardless of temperature.
  • the presence of the anhydrous and/or monohydrate forms in the solid cast detergent composition can produce perceptible swelling of the composition during storage as the higher density anhydrous and monohydrate forms convert to the lower density heptahydrate and decahydrate forms during storage.
  • the process which we have developed to minimize the swelling commonly associated with certain solid cast detergent compositions includes the step of maintaining the processing temperature the concentration of the dual hydratable chemical within a range which prevents the formation of substantial quantities of the high density form of the dual hydratable chemical. Minimizing formation of the high density form during processing correspondingly reduces the concentration of high density hydratable chemical converting to the low density form during storage which corresponds to a reduction in swelling of the cast composition.
  • Maintaining the concentration of the dual hydratable chemical within the desired range throughout processing is fairly simple once the range is defined.
  • maintaining the processing temperature below that temperature at which a significant concentration of the high density hydrate form is developed can be complicated by the fact that the minimum temperature necessary for proper processing of typical solid cast deterger*; compositions containing significant quantities of a dual hydratable chemical (T processing ) can be only about 10° to about 60 C F below T conversion dependent upon the particular dual hydratable chemical and, with respect to sodium carbonate, must be maintained within about a 15°F range (between about 90 and 105°F) to prevent formation of the higher density hydrate forms.
  • the processing temperature may be closely controlled between T proc . folk ing and T conv . rsion by employing a means for actively cooling the product during processing and providing staged hydration of t_hg__d ⁇ al hydratable chemical. Effective control of the processing temperature requires implementation of both active cooling and staged hydration as each control measure is generally insufficient when use alone to control the temperature within the desired range.
  • Figure 1 depicts a triple-stage, semi-continuous process for producing a solid cast detergent composition which permits close control over the processing temperature.
  • the three-stage process includes the steps of (i) mixing the liquid components of the composition and a first portion of the dual hydratable chemical in a first mix tank 10 to form a base mixture, (ii) mixing a second portion of the dual hydratable chemical and the powdered components of the composition in a first feeder system 40 to form a powder premix, (iii) continuously directing a flow of the base mixture and the powder premix into a second mixing tank 20 equipped with a cooling jacket 25 to produce an intermediate mixture, (iv) continuously directing a flow of the intermediate mixture from the second mixing tank 20 and a final portion of the dual hydratable chemical from a second feeder system 50 into a third mixing tank 30 equipped with a cooling jacket 35 to produce the final mixture, (v) casting the final g mixture into molds 70, and (vi) actively cooling the cast mixture in a cooling system 60.
  • the flow rates into and out from the second tank 20 should be controlled to maintain the intermediate mixture within the second tank 20 for the minimum average time period necessary to result in substantially complete hydration of the dual hydratable chemical within the intermediate mixture before the intermediate mixt re is directed into the third tank 30.
  • the flow rates into and out from the third tank 30 should be controlled to maintain the final mixture within the third tank 30 for the minimum average time period necessary to produce a homogeneous final mixture.
  • An extended residence time within the third tank 30 can result in an increase in the viscosity of the final mixture which can interfere with casting of the composition ana cause the composition to solidify and adhere to the si ⁇ ewall of the third tank 30.
  • an average residence time within the second tank 20 of about 20 to about 30 minutes and an average residence time within the third tank 30 of about 2 to about 10 minutes will provide the desired results.
  • the final mixture should have a viscosity of about 3,000 to 10,000 cps as the mixture is cast into the containers 70.
  • a viscosity of less than about 3,000 cps can permit settling to occur within the composition while a viscosity of greater than about 10,000 cps hampers continued mixing of the final composition within the third tank 30 and complicates casting of the composition into the containers 70.
  • Mixing and casting of the composition can be achieved at viscosities in excess of about 10,000 cps but requires specialized equipment. During such staged processing, it must be remembered that the concentration of dual hydratable chemical must be maintained within that concentration range which prevents formation of the higher density hydrate forms at all times.
  • formation of a sodium carbonate containing detergent composition utilizing the triple-stage process outlined above requires that sufficient sodium carbonate be initially added into the base mixture to produce a base mixture containing at least 32 wt% sodium carbonate, based upon sodium carbonate and water in the composition.
  • the first portion of the dual hydratable chemical is exothermically hydrated by the water in the base mixture within the first mixing tank 10 where the heat generated by the exothermic reaction can be used to bring the temperature of the first mixture up to the processing temperature (T proc ⁇ sing ) .
  • the various factors which affect the amount of dual hydratable chemical which can and should be added into the base mixture include (i) the concentration range of the dual hydratable chemical within which the formation of substantial concentrations of the higher density hydrate form are preventing from developing, (ii) the heat of hydration of the particular hydratable chemical (kcal/ ole), (iii) the heat of reaction of any other chemical reaction occurring in the first mixture (kcal/mole), (iv) the moles of first mixture available to absorb the generated heat (moles), (v) the ratio of increase in temperature to increase in heat content for the first mixture ( c F/kcal), (vi) the initial temperature of the first mixture (°F), (vii) T conversio-1 for the particular dual hydratable chemical (°F), and (viii)
  • the second portion of the dual hydra£able chemical is exothe mically hydrated by the water in the base mixture within the second mixing tank 20. Since the base mixture added to the second mixing tank 20 is only about 10° to about 40°F below T conversion , most of the heat generated by addition of the second proportion of the dual hydratable chemical must be promptly removed to prevent the temperature of the intermediate mixture from increasing beyond the. 10° to 40°F cushion between the actual temperature (T actual ) and T con-7ersion .
  • various factors can affect the amount of dual hydratable chemical which may be added to the intermediate mixture include (i) the heat of hydration of the particular dual hydratable chemical (kcal/mole), (ii) the heat of reaction of any other chemical reaction occurring in the second mixture (kcal/mole), (iii) the moles of intermediate mixture available to absorb the generated heat (moles), (iv) the ratio of increase in temperature to increase in heat content for the intermediate mixture (°F/kcal), (iv) the initial temperature of the base mixture (°F), (v) T conversicm (°F), and (vi) the capacity of the second mixing tank 20 to remove heat from the intermediate mixture.
  • the third portion of the dual hydratable chemical is exother ically hydrated within the third mixing tank 30.
  • the intermediate mixture added to the third mixing tank 30 is only about 10° to about 40°F below T conversion , most of the heat generated by addition of the third proportion of the dual hydratable chemical must be promptly removed to p event the temperature of the intermediate mixture from increasing beyond the 10° to 40°F t cushion between the actual temperature (T act . ual ) and T conv , r ⁇ ion .
  • the solid cast detergent composition may be cast into a temporary mold from which it is subsequently transferred for packaging in a separate receptacle, or may be cast directly into the receptacle used for shipping and sale.
  • the composition is cast directly into the final container in order to eliminate the transfer step.
  • the process provides excellent control over the swelling associated with various solid cast detergent compositions.
  • the process can typically prevent greater than 3 vol% swelling in at least 95% of the blocks of solid cast detergent composition prepared by the process and is capable of preventing greater than a 2 vol% swelling in at least 98% of the blocks of solid cast detergent composition prepared by the processs.
  • the process can typically prevent greater than a 3% decrease in the density of the composition in at least 95% of the blocks of cast detergent composition prepared by the process and is capable of preventing greater than a 2% decrease in the density of the composition in at least 98% of the blocks of cast detergent composition prepared by the process. It is noted that a % change in volume does not directly correspond to the same % change in density.
  • the solid cast detergent composition may include various other detergent components including (i) an alkaline source such as an alkali metal hydroxide, and/or an alkali metal silicate, (ii) a surfactant such as a sulfonate, an ethoxylated alky phenol, and/or a polyoxyalkylene oxide block copolymer, (iii) a chelating agent such as aminopolycarboxylic acid, a condensed phosphate, and/or a polyacrylic acid, (iv) a bleaching agent such as hydrogen peroxide, sodium hypochlorite and/or dichloroisocyanurate, (v) a defoamer such as a defoaming nonionic surfactant, (vi) an enzyme, and (vi) various aesthetically based additives such as dyes and perfumes.
  • an alkaline source such as an alkali metal hydroxide, and/or an alkali metal silicate
  • a surfactant such as
  • alkaline source refers to those alkaline compounds which are known to be useful as builders in detergent compositions for improving soil removal performance.
  • Typical sources of alkalinity include the sodium ⁇ ..d potassium hydroxides and the sodium and potassium silicates.
  • Sodium carbonate is also a typical source of alklainity in detergent compositions but is classified here as a dual hydratable chemical.
  • sources of alkalinity are commonly available in either aqueous or powdered form which are both generally useable A3 in formulating typical solid cast detergent compositions.
  • the alkaline source can also assist in solidification of the composition by fixing the free water present in the composition as water of hydration.
  • a second detergent component useful in a solid cast detergent composition is a surfactant.
  • Surfactants are those organic compounds which include both a hydrophilic and a hydrophobic moiety on the same molecule and therefore are able to assist in the performance of a detergent composition by enhancing wetting of the substrate, suspending removed contaminants, and various other functions.
  • anionic and nonionic surfactants providing various combinations of characteristics are commercially available from a number of sources. For a detailed discussion of surfactants see Kirk-Othmer, Encvclopdia of Chemical Technology, Second Edition, volume 19, pages 507-592.
  • a third detergent component useful in a solid cast detergent composition is a chelating/sequestering agent.
  • chelating agents are those molecules capable of coordinating the metal ions commonly found in natural water and thereby preventing the metal ions from interfering with the functioning of the other detersive component(s) of the composition.
  • Useful chelating agents include aminocarboxylic acids, condensed phosphates and polyacrylates.
  • Suitable aminocarboxylic acids include specifically, but not exclusively,
  • N-hydroxyethyliminodiacetic acid N-hydroxyethyliminodiacetic acid, nitrilotriacetic acid (NTA) , ethylenediaminetetraacetic acid (EDTA), N-hydroxyethyl-ethylenediaminetriacetic acid (HEDTA), and diethylenetriaminepentaacetic acid (DTPA) .
  • NTA nitrilotriacetic acid
  • EDTA ethylenediaminetetraacetic acid
  • HEDTA N-hydroxyethyl-ethylenediaminetriacetic acid
  • DTPA diethylenetriaminepentaacetic acid
  • Suitable condensed phosphates include specifically, but not exclusively phosphates such as sodium and potassium ortnophosphate, sodium and potassium pyrophosphate, sodium tripolyphosphate, and sodium hexametaphosphate.
  • the condensed phosphates can also assist in solidification of the composition by fij ⁇ ing the free water present in the composition as water of hydration.
  • Suitable polyacrylates include specifically, but not exclusively, polyacrylic acid, polymethacrylic acid, acrylic acid-methacrylic acid copolymers, hydrolyzed polyacrylamide, hydrolyzed polymethacrylamide, hydrolyzed polylamide-methacrylamide copolymers, hydrolyzed polyacrylonitrile, hydrolyzed polymethacrylonitrile, and hydrolyzed acrylonitrile- methacrylonitrile copolymers.
  • Such polyacrylates also function to thicken the detergent composition and thereby assist in solidification.
  • any chemical compound capable of chemically breaking a ci gated double bond and/or capable of modifying a resonating atom or group of atoms so as to interfere with resonation may be effective as a bleach.
  • the five categories of bleaching materials include: (i) chlorine, (ii) hypochlorites and chloramines, (iii) hydrogen peroxide and other peroxy compounds, (iv) chlorite and chlorine dioxide, and (v) reducing agents.
  • the preferred bleaching agent for use in laundry, warewashing and hard surface cleaners are those bleaches capable of liberating an active halogen sjoecies, such as -Cl, -Br, -OC1 and -OBr, under those conditions normally encountered in the cleansing processes.
  • the preferred halogen releasing compounds typically include the alkali metal dichloroisocyanurates, chlorinated trisodiumphosphate, the alkali metal hypochlorides, monochloramine and dichloramine.
  • Bleaching agents are generally deactived when placed in an alkaline environment such as found within solid cast detergent compositions containing an alkaline source. Accordingly, additional steps may be required to maintain activity of a bleaching agent within a solid cast detergent composition. See, for example. United States Patents Nos. 4,657,784 and 4,681,914.
  • a fifth detergent component useful in a solid cast detergent composition is a defoamant.
  • Typical defoamants are those compounds having a hydrophilic/hydrophobic balance suitable for reducing the stability of foam.
  • the hydrophobicity is typically provided by an oleophilic moiety such as an aromatic alkyl or aralkyl group or an oxypropylene group or chain.
  • the hydrophilicity is typically provided by an oxyethylene group or chain or an es er group.
  • the most frequently utilized defoamers include the phosphate esters and the nonionic organic surface-active polymers (surfactants) having both a hydrophobic groups or block and a hydrophilic ester-groups or block such as a nonylphenol ethoxylate.
  • a sixth detergent component useful in a solid cast detergent composition is an enzyme effective for catalyzing the break down of various contaminating compounds commonly found on the substrate(s) to be cleaned.
  • Commonly employed enzymes include the protei ses which are capable of catalyzing the hydro" " -sis of pro*--sinaceous materials, amylases which are c jable of catylizing the hydrolysis of polysaccharrides, and lipases which are capable of catylizing the hydrolysis of fats.
  • detergent components may be incorporated into the detergent composition so long as they do not meaningfully interfere with solidification of the compo ' ion nor with maintenance of the processing T-aram*...ers within those established for preventing the formation of the more dense hydrate form of dual hydratable chemical.
  • Such components may include such compounds as bactericides, brightening agents, antiredeposition agents, inorganic salts, dyes and fragrances.
  • a solid cast detergent composition based upon sodium carbonate may be prepared in accordance with the three-stage process described above by (-) including in the base mixture, with preferred ranges provided in / / brackets, (a) about 10 to 20 wt% [12 to 16 wt%], based upon the final mixture, sodium carbonate, (b) about 20 to 40 wt% [25 to 35 wt%], based upon the final mixture, " water, (c) about 0 to 5 wt% [2 to 5 wt%], based upon the final mixture, polycarboxylic acid, (d) about 0 to 5 wt% [1 to 3 wt%], based upon the final mixture, sodium hydroxide, and (e) about 0 to 5 wt% [2 to 5 wt%], based upon the final mixture, surfactant; (-) including in the powder ⁇ re ix, with preferred ranges provided between brackets, (aa) about 4 to 10 wt% [5 to 6 wt,
  • the sodium tripolyphosphate is preferrably added in hydrated form to prevent the sodium tripolyphosphate from competing with the sodium carbonate for water of hydration within the composition.
  • the solid cast detergent composition may be conveniently dispensed from a spray-type dispenser such as those disclosed in United States Patents Nos. 4,426,326, 4,569,780, 4,569,781 and 4,687,121.
  • spray-type dispensers function by supporting a solid block of material upon a screen above a spray nozzle and directing a water spray from the spray nozzle through the screen and into contact with an exposed surface of the solid block so as to dissolve a portion of the solid block of material and form a concentrated solution which is immediately directed to the point of use.
  • the concentration of sodium carbonate in the product between the permissible range of 32 and 46 wt% can have a substantial effect upon the dispensing rate of the product in a spray-type " dispenser.
  • Product having a higher concentration of sodium carbonate is less water soluble and hence dispenses slower while product having a lower concentration of sodium carbonate is more water soluble and hence dispenses faster.
  • a base solution containing the components set forth in Table 1 was prepared in a 1000 gallon mixing tank equipped with a variable speed, pitched blade turbine agitator and a water cooling jacket. The temperature of the base solution within the 1000 gallon tank was
  • a blend of the powdered components set forth in Table 1 was prepared in a Ribbin Blender.
  • the powdered blend was generally maintained at about room temperature which is set forth in Table 2.
  • the base solution and the powdered premix were then fed continuously into a 150 gallon tank equipped with a variable speed, pitched blade turbine agitator and a water cooling jacket at the flow rates set forth in Table 2 to produce an intermediate mixture.
  • the flow rate of the base mixture was calculated by measuring the weight loss from the 1000 gallon tank over time.
  • the flow rate of the powdered premix was established by feeding the powdered premix through an Acrison w powder feeder. The two streams reacted exothermically as the dual hydratable chemical in the powdered premix was hydrated by the water in the base mixture.
  • the temperature of the intermediate mixture within the 150 gallon tank was maintained within the temperature range set forth in Table 2 by actively cooling the intermediate mixture with the cooling jacket.
  • the volume of intermediate mixture within the 150 gallon tank was maintained within the range set forth in Table 2 throughout the process until the supply of base solution and/or powdered premix was depleted.
  • the flow rate of the intermediate mixture was estimated by maintaining a constant volume of final mixture in the 40 gallon tank and measuring the flow rate of the final mixture out of the 40 gallon tank.
  • the flow rate ,of the dual hydratable chemical fed in the third stage addition was established by feeding the dual hydratable chemical through an AcrisonTM powder feeder. The two streams reacted exothermically as the dual hydratable chemical was hydrated by the water in the base mixture.
  • the temperature of the final mixture within the 40 gallon tank was maintained within the temperature range set forth in Table 2 by actively cooling the final mixture with the cooling jacket.
  • the volume of final mixture maintained within the 40 gallon tank was within the range set forth in Table 2 throughout the process until the supply of intermediate solution was depleted.
  • the final mixture in the 40 gallon tank was cast into approximately 8 pound blocks within a polypropylene bottle utilizing a SimplexTM piston filler.
  • the cast product was then cooled within a cooling water spray tunnel.
  • the temperature of the cooling water and the duration of cooling within the tunnel are set forth in Table 3.
  • NPE 9 .5 Nonylphenol ethoxylate having an average of 9.5 ethylene units per nonylphenol.
  • LAS 90F -y A 90% active flaked linear alkyl benzene sulfonate sodium salt available from Witco Chemical, Stepen Chemical, Pilot Chemical and Vista Chemical. STPP Sodium tripolyphosphate.
  • Esp 6 . 0T A protease enzyme available from Novo.

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Abstract

Procédé de fabrication d'une composition détergente moulée et solide qui comprend un produit chimique hydratable pouvant être combiné avec de l'eau dans différentes conditions pour prendre au moins deux formes hydratées distinctes de densités différentes, telles que le carbonate de sodium, de manière à empêcher le gonflement de la composition moulée. Le procédé permet de contrôler la concentration du produit chimique hydratable en fonction de la quantité du produit chimique hydratable et d'eau, ainsi que la température du mélange tout au long du procédé afin de minimiser la production de la forme hydratée la plus dense du produit chimique hydratable.
PCT/US1991/005162 1990-08-06 1991-07-22 Fabrication de compositions detergentes solides, moulees et resistant au gonflement WO1992002611A1 (fr)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998030674A1 (fr) * 1997-01-13 1998-07-16 Ecolab Inc. Composition detergente stable et en bloc solide
WO1998030675A1 (fr) * 1997-01-13 1998-07-16 Ecolab Inc. Agent de liaison pour produit fonctionnel en bloc solide
WO2000005331A1 (fr) * 1998-07-20 2000-02-03 Henkel Kommanditgesellschaft Auf Aktien Procede de production de corps solides a utiliser comme detergent ou comme agent de traitement d'eaux usees
US6150324A (en) * 1997-01-13 2000-11-21 Ecolab, Inc. Alkaline detergent containing mixed organic and inorganic sequestrants resulting in improved soil removal
US6156715A (en) * 1997-01-13 2000-12-05 Ecolab Inc. Stable solid block metal protecting warewashing detergent composition
WO2009087540A1 (fr) 2008-01-04 2009-07-16 Ecolab Inc. Matrice de solidification utilisant un polymère d'acide polycarboxylique

Citations (2)

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Publication number Priority date Publication date Assignee Title
US4569780A (en) * 1978-02-07 1986-02-11 Economics Laboratory, Inc. Cast detergent-containing article and method of making and using
US4595520A (en) * 1984-10-18 1986-06-17 Economics Laboratory, Inc. Method for forming solid detergent compositions

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4569780A (en) * 1978-02-07 1986-02-11 Economics Laboratory, Inc. Cast detergent-containing article and method of making and using
US4595520A (en) * 1984-10-18 1986-06-17 Economics Laboratory, Inc. Method for forming solid detergent compositions

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6436893B1 (en) 1997-01-13 2002-08-20 Ecolab Inc. Alkaline detergent containing mixed organic and inorganic sequestrants resulting in improved soil removal
US6177392B1 (en) 1997-01-13 2001-01-23 Ecolab Inc. Stable solid block detergent composition
US8906839B2 (en) 1997-01-13 2014-12-09 Ecolab Usa Inc. Alkaline detergent containing mixing organic and inorganic sequestrants resulting in improved soil removal
AU724117B2 (en) * 1997-01-13 2000-09-14 Ecolab Inc. Binding agent for solid block functional material
WO1998030674A1 (fr) * 1997-01-13 1998-07-16 Ecolab Inc. Composition detergente stable et en bloc solide
US6156715A (en) * 1997-01-13 2000-12-05 Ecolab Inc. Stable solid block metal protecting warewashing detergent composition
WO1998030675A1 (fr) * 1997-01-13 1998-07-16 Ecolab Inc. Agent de liaison pour produit fonctionnel en bloc solide
US6258765B1 (en) 1997-01-13 2001-07-10 Ecolab Inc. Binding agent for solid block functional material
US6150324A (en) * 1997-01-13 2000-11-21 Ecolab, Inc. Alkaline detergent containing mixed organic and inorganic sequestrants resulting in improved soil removal
WO2000005331A1 (fr) * 1998-07-20 2000-02-03 Henkel Kommanditgesellschaft Auf Aktien Procede de production de corps solides a utiliser comme detergent ou comme agent de traitement d'eaux usees
AU2008346168B2 (en) * 2007-05-04 2013-08-22 Ecolab Inc. Solidification matrix using a polycarboxylic acid polymer
WO2009087540A1 (fr) 2008-01-04 2009-07-16 Ecolab Inc. Matrice de solidification utilisant un polymère d'acide polycarboxylique
EP2240564A1 (fr) * 2008-01-04 2010-10-20 Ecolab Inc. Matrice de solidification utilisant un polymère d'acide polycarboxylique
CN101896594A (zh) * 2008-01-04 2010-11-24 埃科莱布有限公司 使用聚羧酸聚合物的固化基质
EP2240564A4 (fr) * 2008-01-04 2012-08-01 Ecolab Inc Matrice de solidification utilisant un polymère d'acide polycarboxylique
EP2240564B1 (fr) 2008-01-04 2016-04-13 Ecolab Inc. Matrice de solidification utilisant un polymère d'acide polycarboxylique

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