WO2001009273A2 - Procede de fabrication de compositions detergentes avec additifs - Google Patents

Procede de fabrication de compositions detergentes avec additifs Download PDF

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Publication number
WO2001009273A2
WO2001009273A2 PCT/US2000/020991 US0020991W WO0109273A2 WO 2001009273 A2 WO2001009273 A2 WO 2001009273A2 US 0020991 W US0020991 W US 0020991W WO 0109273 A2 WO0109273 A2 WO 0109273A2
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Prior art keywords
mixture
aqueous
surfactant
neutralized
weight
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PCT/US2000/020991
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English (en)
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WO2001009273A3 (fr
Inventor
Yousef Georges Aouad
Rodolfo Delgado
Andrew Peter Bakken
Original Assignee
The Procter & Gamble Company
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Application filed by The Procter & Gamble Company filed Critical The Procter & Gamble Company
Priority to BR0012949-6A priority Critical patent/BR0012949A/pt
Priority to MXPA02001202A priority patent/MXPA02001202A/es
Priority to EP00953784A priority patent/EP1203071B1/fr
Priority to US10/048,079 priority patent/US6777381B1/en
Priority to AT00953784T priority patent/ATE272106T1/de
Priority to DE60012537T priority patent/DE60012537D1/de
Priority to AU66175/00A priority patent/AU6617500A/en
Priority to JP2001514067A priority patent/JP2003506524A/ja
Publication of WO2001009273A2 publication Critical patent/WO2001009273A2/fr
Publication of WO2001009273A3 publication Critical patent/WO2001009273A3/fr

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    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/143—Sulfonic acid esters
    • 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0094—Process for making liquid detergent compositions, e.g. slurries, pastes or gels
    • 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
    • C11D17/0004—Non aqueous liquid compositions comprising insoluble particles
    • 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
    • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
    • C11D17/003—Colloidal solutions, e.g. gels; Thixotropic solutions or pastes
    • 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
    • C11D3/2003—Alcohols; Phenols
    • C11D3/2041—Dihydric alcohols
    • C11D3/2044—Dihydric alcohols linear
    • 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
    • C11D3/2068—Ethers
    • 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
    • C11D3/26—Organic compounds containing nitrogen
    • C11D3/33—Amino carboxylic acids
    • 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
    • C11D3/36—Organic compounds containing phosphorus
    • C11D3/361—Phosphonates, phosphinates or phosphonites
    • 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
    • C11D3/36—Organic compounds containing phosphorus
    • C11D3/364—Organic compounds containing phosphorus containing nitrogen
    • 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
    • C11D3/43—Solvents

Definitions

  • the present invention relates to processes for making non-aqueous liquid laundry detergent products which contain an organic anhydrous solvent, an anionic sulfonated surfactant as well as other conventional detergent composition adjuvants and which are in the form of a Newtonian liquid, as well as the drying of (removing water from) detergent ingredients, especially polymers, surfactants and/or solvents, more especially polymers and surfactants for use in detergent compositions.
  • the present invention also provides a means of converting Newtonian liquids into non-Newtonian liquids and non-Newtonian liquids into Newtonian liquids.
  • Liquid laundry detergent products offer a number of advantages over dry, powdered or particulate laundry detergent products.
  • Liquid laundry detergent products are readily measurable, speedily dissolved in wash water, non-dustmg, are capable of being easily applied in concentrated solutions or dispersions to soiled areas on garments to be laundered and usually occupy less storage space than granular products.
  • liquid laundry detergents may have incorporated into their formulations materials which would deteriorate in the drying operations employed in the manufacture of particulate or granular laundry detergent products. Because liquid laundry detergents are usually considered to be more convenient to use than granular laundry detergents, they have found substantial favor with consumers
  • liquid laundry detergents have a number of advantages over granular laundry detergent products, there are also disadvantages entailed in using them as well.
  • laundry detergent composition components which may be compatible with each other m granular products may tend to interact or react with each other in a liquid, and especially in an aqueous liquid, environment.
  • Components such as surfactants, perfumes, b ⁇ ghteners and non-aqueous solvents can be especially difficult to incorporate into liquid laundry detergent products with an acceptable degree of compositional stability. Poor compositional stability may cause the detergent composition to be prematurely reacted into the wash liquor as well as create an ineffective, heterogeneous detergent composition during storage
  • Non-aqueous liquid laundry detergent compositions have been disclosed in Hepworth et al., U.S. Patent 4,615,820, Issued October 17, 1986; Schultz et al., U.S. Patent 4,929,380, Issued May 29, 1990; Schultz et al., U.S.
  • non-aqueous liquid laundry detergents come with their own set of disadvantages and problems.
  • the desirable advantage of having excellent compositional stability may mean simultaneously that the non-aqueous liquid laundry detergent will have poor solubility and dispersion properties in the wash liquor inside an automatic clothes washer.
  • non-aqueous liquids typically have awkward rheological properties, displaying a tendency known as "shear thickening", where the viscosity of the paste or liquid increases with an increasing shear rate making the paste difficult to pump, store and transport.
  • non-aqueous liquid laundry detergent compositions are difficult and expensive to manufacture.
  • a drying step requiring prolonged heating and stirring is necessary to eliminate the water, but not only is it difficult to consistently achieve the proper heating and stirring conditions in a manufactu ⁇ ng setting, but such drying operations may also have the effect of decomposing or evaporating individual components of the detergent composition.
  • the resulting difficulty and expense involved with working with such fluids has greatly reduced their utilization as laundry detergent compositions.
  • It is a benefit of the present invention is to provide a process which produces a liquid laundry detergent composition that is easy to handle in bulk. Since it does not display shear thickening, but is in fact a Newtonian fluid over a broad range of shear rates, it is considerably easier to store, pump and transport when compared with other non-aqueous liquids.
  • An additional benefit of the present invention is a process for drying (removing water from) detergent ingredients, especially polymers, surfactants and/or solvents, more especially polymers and surfactants for use m detergent compositions.
  • Such a process preferably comp ⁇ ses the steps of forming an aqueous detergent ingredient mixture and drying said mixture using an Agitated Thin Film Evaporator (ATFE).
  • ATFE Agitated Thin Film Evaporator
  • Yet a further benefit of the present invention is a process for converting Newtonian liquids into non-Newtonian liquids and non-Newtonian liquids into Newtonian liquids.
  • Such a process preferably comp ⁇ ses the steps of forming an aqueous Newtonian liquid mixture and drying said mixture using an Agitated Thm Film Evaporator (ATFE) such that a non-Newtonian liquid is produced.
  • the process preferably comp ⁇ ses the steps of forming an aqueous non- Newtonian liquid mixture and drying said mixture using an Agitated Thm Film Evaporator (ATFE) such that a Newtonian liquid is produced.
  • ATFE Agitated Thm Film Evaporator
  • An additional benefit of the present invention is to provide a process for prepa ⁇ ng non- aqueous liquid laundry detergent products which have excellent chemical and compositional stability as well as outstanding fabric laundering performance characteristics.
  • the processes produce non-aqueous liquid laundry detergent products that are readily soluble in a wash liquor.
  • a further benefit is to provide a process for combining aqueous solutions of detergent components and then drying them together to produce a liquid mixture with a water level lower than what could be achieved by combining non-aqueous solutions of the components.
  • Still yet a further benefit of the present invention is to provide a process for preparing anhydrous agglomerates, preferably comprising organic solvents, surfactants, other detergent adjunct ingredients and/or combinations thereof, wherein the process comprises the step of producing a binder, preferably an anhydrous binder, which is preferably a highly viscous, non- Newtonian solvent based mixture of preferably one or more organic solvents, one or more surfactants, one or more chelants and/or one or more polymers, preferably anhydrous liquid polymers
  • the anhydrous binder is formed by mixing an anionic material, preferably an anionic surfactant, more preferably linear alkylbenzene sulfonate, with a cationic material, preferably a cationic anhydrous liquid polymer.
  • the mixture is made in an aqueous phase in the presence of an organic solvent and then further d ⁇ ed using a drying process described herein, preferably using an Agitated Thm Film Evaporator (ATFE), to produce an anhydrous binder.
  • the anhydrous binder can then be combined with powders, such as citrates, carbonates, silicates, and the like, to form anhydrous agglomerates.
  • powders such as citrates, carbonates, silicates, and the like.
  • Such a process provides anhydrous agglomerates that do not require a further drying step after the agglomeration step.
  • These anhydrous agglomerates are useful in product forms including, but not limited to, liquid detergent products, especially anhydrous liquid detergent products, and in detergent tablet products.
  • a process for making and/or drying surfactants or combinations of surfactants and/or other detergent adjunct ingredients such as chelants, builders, buffers, rheology modifiers and the like.
  • Such a process comp ⁇ ses preparing a mixture of surfactants and/or other detergent adjuncts in an aqueous medium or a combination of aqueous and solvent media.
  • This preparation step may be achieved by mixing these materials in their neutralized aqueous and/or powder form or by co-neutralizing them in the presence or absence of a solvent batchwise or continuously in a dominant bath neutralization loop such as a Chemithon, Ballestra or Manro unit.
  • the drying step comp ⁇ ses feeding the prepared mixture into a drying device or equipment which is a batch or continuous drying equipment.
  • a drying device or equipment which is a batch or continuous drying equipment.
  • An example of batch drying equipment is a combination tank, preferably agitated, which can be heated under vacuum. The tank is operated at suitable vacuum and temperature such that water is stripped from the mixture.
  • An example of a continuous drying equipment is an Agitated Thin Film Evaporator (ATFE).
  • a suitable ATFE is commercially available from LCI Corporation
  • This process is also suitable for expanding hollow microspheres, such as EXPANCEL® microspheres.
  • EXPANCEL® microspheres As the hollow microspheres pass through the drying equipment (ATFE) the microspheres expand because the temperature of the ATFE is above the expansion temperature of the microspheres.
  • ATFE drying equipment
  • compositions produced according to the processes disclosed herein the above benefits which are novel to non-aqueous compositions and yet these process produce compositions that are typical of a non-aqueous liquid laundry detergent composition, viz a high surfactant activity and excellent additive stability
  • the process comprises a formation step in which an aqueous surfactant mixture is formed by mixing an anionic sulfonated surfactant, an organic solvent or carrier and a chelant and a drying step m which the aqueous surfactant mixture under vacuum to form a solvent-based surfactant paste containing less than about one percent, by weight, of water.
  • This process may be modified such that an individual ingredient can be processed, thereby producing a "dried" ingredient.
  • an anionic sulfonated surfactant could be d ⁇ ed via the drying step such that the anionic sulfonated surfactant final product contains less than about 1% by weight of water.
  • the aqueous surfactant mixture m the formation step contains from about 5% to about 85%o of an amomc sulfonated surfactant, from about 15% to about 95%> of an organic solvent, from about 0.001% to about 40% of a chelant and at least about 15% of water by weight of the aqueous surfactant mixture
  • the aqueous surfactant mixture in the formation step is a non- Newtonian fluid.
  • the solvent-based surfactant paste produced by the drying step is a Newtonian fluid and having a substantially constant viscosity withm the range of 100 cp to 100000 cp when measured at a temperature of 25 °C and with the shear rate range of from Is "1 to 1000 s "1 .
  • a preferred embodiment also includes mixing into the aqueous surfactant mixture other additives such as buffers, builders, nomonic surfactants, polymers and copolymers and other additives.
  • the present invention may also be practiced in a second aspect.
  • This embodiment comp ⁇ ses a neutralization step in which a neutralized mixture is formed by a continuous neutralization loop.
  • This neutralized mixture contains an acid form of an anionic surfactant, a base, an organic solvent, and a chelant
  • the neutralized mixture has a water content of at least about 5% by weight of the neutralized mixture and is a non-Newtonian fluid.
  • the molar ratio of the acid form of the anionic surfactant to the base is from about 1 : 1 to about 9: 1
  • a first portion of the neutralized mixture is then removed from the continuous neutralization loop and dried under vacuum to form a solvent-based surfactant paste having a water content of from about 0.2% to about 10% and which is in the form of a Newtonian fluid having a substantially constant viscosity within the range of 100 cp to 100000 cp when measured at a temperature of 25°C and withm the shear rate range of from 1 s ' to 1000 s ' while a second portion of the neutralized mixture is recirculated m the continuous neutralization loop
  • additional chelant and solvent may be added to the neutralized mixture after the neutralized mixture is removed from the neutralization loop
  • the present invention offers the advantage of prepa ⁇ ng a surfactant paste with only a trace amount of water and yet can incorporate many of the ingredients desirable for use in a laundry detergent composition such as bleach, bleach activators, builders, enzymes, whiteners and other additives. By minimizing the amount of water m the surfactant pastes or mixtures, one may maximize the activity of the surfactant paste. Furthermore, the present invention allows the manufacture of a high-active surfactant paste or mixtures in the form of a Newtonian Fluid that has a low viscosity and so is capable of being transported, stored and handled with ease.
  • FIG. 1 is a schematic representation of an apparatus for carrying out the process according to the invention.
  • FIG. 2 is a schematic representation of an apparatus for carrying out the process according to the invention
  • a “Newtonian fluid” is a fluid that withm a range of specified shear rates at a specified temperature the viscosity of the fluid has a substantially constant value.
  • non-Newtonian fluid refers to a fluid which cannot be charactenzed as a “Newtonian fluid.”
  • non-aqueous or “anhydrous” are used synonymously and both describe a fluid in which the water content is less than about 5%
  • the present invention describes a process for preparing non-aqueous liquid laundry detergents with additives by forming an aqueous surfactant mixture and then drying the mixture under a vacuum to form a non-aqueous solvent-based surfactant paste.
  • the processes of preparing non-aqueous liquid laundry detergent compositions with additives has many important parameters and incorporates many different ingredients and additives as well as numerous other preferable and optional process subparts which are desc ⁇ bed hereafter.
  • the formation step consists of adding several different ingredients 10, 12, 14 and 16 to a mixer 20 with an impeller stirrer 18 to form an aqueous surfactant mixture by mixing the formation step ingredients (desc ⁇ bed below) in the mixer. It is preferable that each of the ingredients be added in the form of a neutralized aqueous solution which is comprised of about 20% water, by weight.
  • a modified process in accordance to the present invention comprises processing individual ingredients instead of a mixture of ingredients.
  • the first ingredient 10 in the formation step is an aqueous surfactant mixture.
  • the final aqueous surfactant mixture will include, by weight, from about 5% to about 85%, more preferably from about 25% to about 75%, most preferably from about 40%> to about 60% of anionic sulfonated surfactant. Suitable anionic sulfonated surfactants are discussed m greater detail below.
  • the second ingredient 12 m the formation step is an organic solvent.
  • the final aqueous surfactant mixture will include, by weight, from about 15% to about 95%, more preferably from about 30% to about 70% , most preferably from about 40% to about 60% of an organic solvent. Suitable organic solvents are discussed in greater detail below.
  • the third ingredient 14 in the formation step is a chelant.
  • the final aqueous surfactant mixture will include, by weight, from about 0.001% to about 40%, more preferably from about 0.01% to about 4% , most preferably from about 0.1% to about 2% of a chelant. Suitable chelants are discussed in greater detail below.
  • the third ingredient 16 m the formation step is composed of optional detergent additives such as bleach, bleach activator, buffers, builders, enzymes, nomonic surfactants, whiteners, rheology modifiers, polymers and copolymers. These are discussed in greater detail below.
  • the aqueous surfactant mixture m the formation step contains, by weight, at least about 15%, more preferably from about 18% to about 50% of water.
  • the aqueous surfactant mixture m Step A may also contain other conventional detergent ingredients such as buffers, builders, nomonic surfactants, whiteners, rheology modifiers, polymers and copolymers and other additives, some of which are discussed in greater detail below.
  • the aqueous surfactant mixture is formed by mixing together all of the ingredients in step A (in any order) into a substantially uniform mixture, at a temperature of between about 25 °C and about 80°C, preferably at a temperature of between about 35°C and about 70°C and most preferably at a temperature of between about 45°C and about 60°C. Temperature control is important because if the temperature is too low, it will be difficult to process the mixture and if the temperature is too high there may be degradation of the solvent and/or the chelant component of the mixture.
  • the mixer 20 in the formation step is most preferably carried out in a standard mixer or crutcher
  • the speed of the mixer and the duration of the mixing step varies depending on the type of mixer and ingredients used Mixing should be done at a speed and for a time sufficient to achieve a homogenous aqueous surfactant mixture.
  • the aqueous surfactant mixture 22 is then by the action of a pump 24 pumped into a drying device 26 where the drying step takes place
  • the drying step of the process is drying the aqueous surfactant mixture under vacuum to form a solvent-based surfactant paste containing less than about one percent, by weight, of water.
  • This drying may be accomplished m any conventional evaporator, provided that the drying is performed under vacuum Suitable evaporators are illustrated in Perry's Chemical Engineering Handbook, 7th. Ed., 1997, McGraw- Hill, ppg. 11-108 to 11-111, "Evaporator Types and Applications", which is herein incorporated by reference.
  • a preferred evaporator is an agitated thm-film evaporator.
  • the drying step produces a solvent-based surfactant paste 30 which is a Newtonian fluid having a substantially constant viscosity withm the range of 100 cp to 100000 cp when measured at a temperature of 25°C and with the shear rate range of from 1 s "1 to 1000 s ⁇
  • the drying step also produces a combination of water vapor and other volatiles 28 which are subsequently condensed and the volatiles reclaimed
  • a neutralized mixture 58 is formed by a continuous neutralization loop.
  • Four components are continuously added to the neutralization loop: an acid form of an amomc sulfonated surfactant 40, a base 42, an organic solvent 44, and a chelant 46 into the loop.
  • a mixture of the components are formed as the components and mixture are circulated through a mixer 50 a pump 52 and a heat circulator 54.
  • Neutralization takes place as the base reacts with the acid form of the surfactant to produce a surfactant salt.
  • the resulting neutralized mixture has a water content of at least about 15% by weight of the neutralized mixture and is a non-Newtonian fluid.
  • a first portion of the neutralized mixture 56 is recirculated in the continuous neutralization loop while a second portion is removed from the continuous neutralization loop 58 by the action of a pump 60
  • additional organic solvent 62 or chelant 62 may be added to and mixed with the second portion of the neutralized mixture in a static mixer 66 with the resulting mixture 64 having a water content of from about 5% to about 50%, by weight
  • the resulting mixture is then further mixed in a static mixer 66
  • additional chelant 72 or organic solvent 72 may again be added to the second portion of the neutralized mixture and mixed in a static mixer 76 or a conventional mixer such as a crutcher 84
  • the molar ratio of the acid form of the amomc surfactant to the base is from about 1 1 to about 9 1 It is preferable that these ingredients be added in the form of an aqueous solution
  • the aqueous solution of the va ⁇ ous components which are added to the continuous neutralization loop (40, 42, 44, 46) will preferably comprise the following amounts of water: acid from of sulfonated surfactant from about 0.0%> to about 10.0% base from about 30% to about 90% organic solvent from about 0.0% to about 50% chelant from about 40% to about 95%
  • the second portion of the neutralized mixture is then dried under vacuum to form a solvent-based surfactant paste having a water content of from about 0.2% to about 10% and which is in the form of a Newtonian fluid having a substantially constant viscosity withm the range of 100 cp to 100000 cp when measured at a temperature of 25°C and within the shear rate range of from 1 s "1 to 1000 s "1 .
  • the drying operation is similar to that described above and may use the same equipment and process va ⁇ ables.
  • the processes described above offer the advantage of preparing a surfactant paste with only a trace amount of water yet incorporating many of the ingredients desirable for use in a laundry detergent composition such as builders, whiteners and other additives.
  • a surfactant paste By minimizing the amount of water in the surfactant pastes, one may maximize the activity of the surfactant paste.
  • the present invention allows the manufacture of a high-active surfactant paste m the form of a Newtonian Fluid that has a low viscosity and so is capable of being transported, stored and handled with ease.
  • the solvent-based surfactant pastes desc ⁇ bed above comprise the following ingredients hereafter desc ⁇ bed in seritam.
  • Anionic sulfonated surfactants are added to the processes described herein m the form of aqueous liquids.
  • Suitable anionic sulfonated surfactants include the water-soluble salts, preferably the alkali metal, ammonium and alkylolammonium salts, of organic sulfu ⁇ c reaction products having in their molecular structure an alkyl group containing from about 10 to about 20 carbon atoms and a sulfonic acid or sulfu ⁇ c acid ester group.
  • alkyl is the alkyl portion of acyl groups.
  • alkyl is the alkyl portion of acyl groups.
  • these group of synthetic surfactants are the sodium and potassium alkyl benzene sulfonates in which the alkyl group contains from about 9 to about 15 carbon atoms, in straight or branched chain configuration, e.g., those of the type described in U.S. Pat. Nos. 2,220,099 and 2,477,383.
  • Especially valuable are linear straight chain alkyl benzene sulfonates m which the average number of carbon atoms in the alkyl group is from about 11 to 13, abbreviated as C u -C !3 LAS.
  • amomc surfactants herein are the sodium alkyl glyceryl ether sulfonates, especially those ethers of higher alcohols de ⁇ ved from tallow and coconut oil; sodium coconut oil fatty acid monoglyce ⁇ de sulfonates.
  • Other useful anionic surfactants herein include the water-soluble salts of esters of alpha- sulfonated fatty acids containing from about 6 to 20 carbon atoms in the fatty acid group and from about 1 to 10 carbon atoms m the ester group; water-soluble salts of 2-acyloxy-alkane-l- sulfomc acids containing from about 2 to 9 carbon atoms in the acyl group and from about 9 to about 23 carbon atoms in the alkane moiety; water-soluble salts of-olefin sulfonates containing from about 12 to 24 carbon atoms; and beta-alkyloxy alkane sulfonates containing from about 1 to 3 carbon atoms m the alkyl group and from about 8 to about 20 carbon atoms in the alkane moiety.
  • the acid salts are typically discussed and used, the acid neutralization can be performed as part of the fine dispersion mixing step.
  • Particularly preferred surfactants herein include linear alkylbenzene sulfonates containing from about 11 to 14 carbon atoms in the alkyl group; tallow alkyl sulfates; coconutalkyl glyceryl ether sulfonates; olefin or paraffin sulfonates containing from about 14 to 16 carbon atoms; alkyldimethylamme oxides wherein the alkyl group contains from about 11 to 16 carbon atoms; alkyl dimethylammomo propane sulfonates and alkyl dimethylammonio hydroxy propane sulfonates wherein the alkyl group contains from about 14 to 18 carbon atoms and mixtures thereof.
  • Specific preferred surfactants for use herein include: t ⁇ ethanolammonium C ⁇ -C 13 alkylbenzene sulfonate; sodium coconut alkyl glyceryl ether sulfonate; sodium coconut alkyl glyceryl ether sulfonate; the condensation product of a C ]2 -C !3 fatty alcohol with about 3 moles of ethylene oxide; 3-(N,N-d ⁇ methyl-N-coconutalkylammon ⁇ o)-2-hydroxypropane-l-sulfonate; 3- (N,N-d ⁇ methyl-N-coconutalkylammon ⁇ o)-propane-l -sulfonate; and mixtures thereof.
  • Non-surfactant Non-aqueous Organic Solvents may also comp ⁇ se one or more non- surfactant, non-aqueous organic solvents.
  • the detergent compositions of the present invention will contain from about 15% to about 95%, more preferably from about 30% to about 70%, most preferably from about 40% to about 60% of an organic solvent.
  • Such non-surfactant non-aqueous liquids are preferably those of low polarity.
  • "low-pola ⁇ ty" liquids are those which have little, if any, tendency to dissolve one of the preferred types of particulate material used in the compositions herein, i.e., the peroxygen bleaching agents, sodium perborate or sodium percarbonate.
  • Suitable types of low-pola ⁇ ty solvents useful in the non-aqueous liquid detergent compositions herein do include non-vicmal Ci-Cg alkylene glycols, alkylene glycol mono lower alkyl ethers, lower molecular weight polyethylene glycols, lower molecular weight methyl esters and amides, and the like.
  • a preferred type of non-aqueous, low-polarity solvent for use in the compositions herein comp ⁇ ses the non-vicmal C4-Cg branched or straight chain alkylene glycols. Mate ⁇ als of this type include hexylene glycol (4-methyl-2,4-pentaned ⁇ ol), 1,6-hexanediol, 1,3-butylene glycol and 1 ,4-butylene glycol. Hexylene glycol is the most preferred.
  • Another prefe ⁇ ed type of non-aqueous, low-polarity solvent for use herein comp ⁇ ses the mono-, di-, t ⁇ -, or terra- C2-C3 alkylene glycol mono C2-Cg alkyl ethers.
  • the specific examples of such compounds include diethylene glycol monobutyl ether, tetraethylene glycol monobutyl ether, dipropolyene glycol monoethyl ether, and dipropylene glycol monobutyl ether.
  • Diethylene glycol monobutyl ether, dipropylene glycol monobutyl ether and butoxy-propoxy-propanol (BPP) are especially preferred.
  • Compounds of the type have been commercially marketed under the tradenames Dowanol, Carbitol, and Cellosolve.
  • non-aqueous, low-polarity organic solvent useful herein comprises the lower molecular weight polyethylene glycols (PEGs). Such materials are those having molecular weights of at least about 150. PEGs of molecular weight ranging from about 200 to 600 are most preferred. Yet another preferred type of non-polar, non-aqueous solvent comp ⁇ ses lower molecular weight methyl esters. Such materials are those of the general formula: R*-C(0)-OCH3 wherein
  • R! ranges from 1 to about 18.
  • suitable lower molecular weight methyl esters include methyl acetate, methyl propionate, methyl octanoate, and methyl dodecanoate.
  • the non-aqueous, generally low-pola ⁇ ty, non-surfactant organic solvent(s) employed should, of course, be compatible and non-reactive with other composition components, e.g., bleach and/or activators, used in the liquid detergent compositions herein.
  • a solvent component is preferably utilized in an amount of from about 1% to 70% by weight of the liquid phase.
  • a non-aqueous, low-pola ⁇ ty, non-surfactant solvent will comprise from about 10%) to 60%) by weight of a structured liquid phase, most preferably from about 20% to 50% by weight, of a structured liquid phase of the composition.
  • Utilization of non-surfactant solvent in these concentrations in the liquid phase corresponds to a non-surfactant solvent concentration m the total composition of from about 1%> to 50% by weight, more preferably from about 5% to 40% by weight, and most preferably from about 10% to 30% by weight, of the composition.
  • the detergent compositions herein also contain a chelatmg agent which serves to chelate metal ions, e.g., iron and/or manganese, withm the non-aqueous detergent compositions herein.
  • the detergent compositions will contain from about 0.1% to about 10%, more preferably from about 0.5% to about 5%, most preferably from about 1%> to about 3% of a chelant.
  • Such chelatmg agents thus serve to form complexes with metal impurities in the composition which would otherwise tend to deactivate composition components such as the peroxygen bleaching agent.
  • Useful chelatmg agents can include amino carboxylates, phosphonates, ammo phosphonates, polyfunctionally-substituted aromatic chelatmg agents and mixtures thereof.
  • Other suitable chelants are disclosed in U.S. Pat. Nos. 5,712,242, issued January 27, 1998, to Aouad et al., which is incorporated herein by reference.
  • Ammo carboxylates useful as optional chelatmg agents include hylenediammetetraacetates, N-hydroxyethyl-ethylenediaminet ⁇ acetates, nit ⁇ lot ⁇ acetates, ethylene-diamme tetraprop ⁇ onates, t ⁇ ethylenetetraammehexacetates, diethylenet ⁇ ammepentaacetates, ethylenediammedisuccmates and ethanol diglycines.
  • the alkali metal salts of these materials are preferred
  • Ammo phosphonates are also suitable for use as chelatmg agents in the compositions of this invention when at least low levels of total phosphorus are permitted in detergent compositions, and include ethylenediammetetrakis (methylene-phosphonates) as DEQUEST.
  • these ammo phosphonates do not contain alkyl or alkenyl groups with more than about 6 carbon atoms
  • Prefe ⁇ ed chelatmg agents include hydroxy-ethyldiphosphonic acid (HEDP), diethylene t ⁇ amme penta acetic acid (DTP A), ethylenediamme disuccimc acid (EDDS) and dipicohmc acid (DP A) and salts thereof.
  • the chelatmg agent may, of course, also act as a detergent builder during use of the compositions herein for fabric laundermg bleach g.
  • the chelatmg agent if employed, can comprise from about 0.1% to 4% by weight of the compositions herein. More preferably, the chelatmg agent will comprise from about 0.2% to 2%> by weight of the detergent compositions herein.
  • the acid from of a surfactant reacts with a neutralization base.
  • a neutralization base Any base which adequately neutralizes the acid form of the surfactant is suitable.
  • Preferred neutralization bases include the alkali metal carbonates, alkali metal hydroxides and alkali metal phosphates, e.g., sodium carbonate, sodium hydroxide, sodium polyphosphate.
  • the present detergent compositions can, and preferably will, contain various other optional components.
  • Such optional components are added to the detergent compositions in the form of dilute aqueous solutions, (a) Organic Detergent Builders
  • Another possible type of additional particulate material which can be suspended in the non- aqueous liquid detergent compositions herein comprises an organic detergent builder mate ⁇ al which serves to counteract the effects of calcium, or other ion, water hardness encountered during laundermg bleachmg use of the compositions herein.
  • Such materials include the alkali metal, citrates, succinates, malonates, fatty acids, carboxymethyl succmates, carboxylates, polycarboxylates and polyacetyl carboxylates
  • Specific examples include sodium, potassium and lithium salts of oxydisuccmic acid, melhtic acid, benzene polycarboxy c acids and citric acid
  • organic phosphonate type sequestering agents such as those which have been sold by Monsanto under the Dequest tradename and alkanehydroxy phosphonates. Citrate salts are highly preferred
  • Suitable organic builders include the higher molecular weight polymers and copolymers known to have builder properties
  • mate ⁇ als include appropriate polyacryhc acid, polymaleic acid, and polyacrylic/polymaleic acid copolymers and their salts, such as those sold by BASF under the SOKALANTM which have molecular weight ranging from about 5,000 to 100,000.
  • Another suitable type of organic builder comprises the water-soluble salts of higher fatty acids, i.e , "soaps".
  • these include alkali metal soaps such as the sodium, potassium, ammonium, and alkylolammomum salts of higher fatty acids containing from about 8 to about 24 carbon atoms, and preferably from about 12 to about 18 carbon atoms.
  • Soaps can be made by direct saponification of fats and oils or by the neutralization of free fatty acids.
  • Particularly useful are the sodium and potassium salts of the mixtures of fatty acids derived from coconut oil and tallow, i.e., sodium or potassium tallow and coconut soap.
  • insoluble organic detergent builders can generally comprise from about 2% to 20% by weight of the compositions herein. More preferably, such builder material can comprise from about 4%> to 10% by weight of the composition.
  • the detergent compositions herein may also optionally contain one or more types of inorganic detergent builders beyond those listed hereinbefore that also function as alkalinity sources.
  • optional inorganic builders can include, for example, alummosilicates such as zeolites. Alummosihcate zeolites, and their use as detergent builders are more fully discussed m Corkill et al., U.S. Patent No. 4,605,509; Issued August 12, 1986, the disclosure of which is incorporated herein by reference.
  • crystalline layered silicates such as those discussed m this '509 U.S. patent, are also suitable for use in the detergent compositions herein.
  • optional inorganic detergent builders can comprise from about 2% to 15%> by weight of the compositions herein.
  • the polymers and copolymers of the present invention may be chosen from a wide range of organic polymers, some of which also may function as builders to improve detergency Included among such polymers may be mentioned sodium carboxy-lower alkyl celluloses, sodium lower alkyl celluloses and sodium hydroxy-lower alkyl celluloses, such as sodium carboxymethyl cellulose, sodium methyl cellulose and sodium hydroxypropyl cellulose, polyvinyl alcohols (which often also include some polyvinyl acetate), polyacrylamides, polyacrylates, polyaspartates, polyv ylpyrrohdones and various copolymers, such as those of maleic and acrylic acids. Molecular weights for such polymers vary widely but most are withm the range of 2,000 to 100,000.
  • Polymeric polycarboxyate builders are set forth in U.S. Pat. No. 3,308,067, Diehl, issued Mar. 7, 1967. Such materials include the water-soluble salts of homo-and copolymers of aliphatic carboxyhc acids such as maleic acid, ltacomc acid, mesacomc acid, fuma ⁇ c acid, acomtic acid, citraconic acid and methylenemalonic acid.
  • copolymers of maleic and acrylic acid having a molecular weight of from 2000 to 100000, carboxymethyl cellulose and mixtures thereof.
  • concentration of the aqueous solutions of the polymer or copolymer is not critical m the present invention. However, it is convenient to use solutions which are readily available commercially.
  • anhydrous liquid polymers preferably cationic anhydrous liquid polymers.
  • anhydrous liquid polymers are known to those of ordinary skill in the art.
  • Aqueous solutions having a concentration of from 5%> to 60% of the polymer or copolymer are suitable, (d) Optional Brighteners, Suds Suppressors, and/or Dyes
  • the detergent compositions herein may also optionally contain conventional b ⁇ ghteners, suds suppressors, bleach catalysts, dyes and/or perfume materials.
  • Such b ⁇ ghteners, suds suppressors, sihcone oils, bleach catalysts, dyes and perfumes must, of course, be compatible and non-reactive with the other composition components in a non-aqueous environment. If present, b ⁇ ghteners suds suppressors, dyes and or perfumes will typically comprise from about 0.0001% to 2% by weight of the compositions herein.
  • Suitable bleach catalysts include the manganese based complexes disclosed in US 5,246,621, US 5,244,594, US 5,114,606 and US 5,114,611.
  • This process is comprised of two key steps.
  • raw materials m form of aqueous solutions are combined at a typical batch size of 2400 lb.
  • the water is removed from the aqueous feed stock.
  • BPP n-butoxy propoxy propanol
  • LAS linear alkyl benzene sulfonate
  • a 36.25% active aqueous solution of [S, S] - ethylenediammo - N - N' - disuccinic acid (EDDS) chelant is added, and the resulting solution is mixed until it appears homogeneous.
  • the EDDS chelant is added to the other two components at room temperature, and contains a minimum of 99% S,S isomer of the total EDDS isomers and a minimum of 95% S,S isomer of the total ammo acid species.
  • the formula details for the resulting aqueous solution are summarized below.
  • the water is removed from the aqueous mixture m a 5.4 ft 2 steam-jacketed agitated thm film evaporator.
  • the aqueous solution is pumped at a rate of 115 kg/hr to the evaporator, operating at a temperature of 160°C and a pressure of 100 mm Hg.
  • the product exits the evaporator at a temperature of 120°C with a moisture content of 0.6%.
  • the product is then cooled m a plate and frame heat exchanger to 35°C. About 14% of the BPP evaporates with the water m the ATFE.
  • the remaining d ⁇ ed product composition is shown in Table 2.
  • the table indicates that LAB and Na 2 S0 4 are present in the dried product.
  • LAB is linear alkyl benzene (LAB) alcohol, it is left over from the sulphonation reaction which produces HLAS.
  • Na S0 is a by-product of the reaction between HLAS and NaOH which produces NaLAS.
  • the resulting detergent compositions produced were then analyzed as follows: in all examples, Karl Fischer analysis was used to determine amount of residual water.
  • a rotational rheometer, Ca ⁇ -med, supplied by TA Instruments, Delaware, USA was used to measure rheology.
  • Example 2 The HLAS was neutralized with 50% solution of NaOH while co-adding an organic solvent n-butoxy propoxy propanol ("n-BPP") produced by the Dow Chemical of Midland, Michigan and a 37% solution of the sodium salt of [S,S] - ethylenediammo - N - N' - disuccmic acid ("NaEDDS"). After neutralization the resulting mixture comprised, on a weight basis:
  • n-BPP organic solvent n-butoxy propoxy propanol
  • NaEDDS sodium salt of [S,S] - ethylenediammo - N - N' - disuccmic acid
  • the combined flow rate of all components into the neutralization loop at room temperature was 1.034kg/mm
  • the temperature of neutralization was 99°F while the temperature of the mixture exiting the loop was 95°F.
  • the mixture exiting the loop was non-Newtonian as shown in the figure below. Also shown is a figure particle size distribution as measured by a
  • Coulter LS particle size analyzer The mixture is then fed continuously at a rate of 120kg/hr into a 3ft 2 ATFE) operating at 160°C and 95mmHg.
  • the resulting dry material contained 0.45% water and behaved as a Newtonian fluid having a viscosity of 15,000 cP at room temperature as measured by a rotational rheometer. Also shown is a particle size distribution measurement of the dry mate ⁇ al
  • Example 3 HLAS was neutralized with 50% solution of NaOH while co-add g BPP After neutralization the resulting mixture comprised, on a weight basis.
  • the combined flow rate of all components into the neutralization loop at room temperature was 0.906kg/mm.
  • the temperature of neutralization was 99°F while the temperature of the mixture exiting the loop was 95°F.
  • the mixture exiting the loop was non-Newtonian as shown m the figure below.
  • the mate ⁇ al was further mixed in a tank with a solution of NaEDDS to give a composition similar to that in the above example.
  • the resulting rheology was also non- Newtonian.
  • the mixture was then fed continuously at a rate of 137kg/hr into a 3 ft 2 ATFE operating at 160°C and 95mmHg.
  • the resulting dry mate ⁇ al contained 0.77% water and behaved as a Newtonian fluid having a viscosity of 12,000 cP at room temperature as measured by a rotational rheometer. Also shown is a particle size distribution measurement of the dry material.
  • Example 4 HLAS was neutralized with 50% solution of NaOH while co-addmg BPP. After neutralization the resulting mixture comp ⁇ sed, on a weight basis:
  • the combined flow rate of all components into the neutralization loop at room temperature was 0.906kg/mm.
  • the temperature of neutralization was 99°F while the temperature of the mixture exiting the loop was 95°F
  • the mixture exiting the loop was non-Newtonian as shown m the figure below.
  • the mixture is then fed continuously at a rate of 170kg/hr into a 3ft 2 ATFE operating at 160°C and 95mmHg
  • the resulting dry material contained 0.7% water and behaved as a Newtonian fluid having a viscosity of 10,000cP at room temperature as measured by a rotational rheometer
  • a particle size distribution measurement of the dry material is also shown.
  • Example 5 A mixture was prepared comprising on a weight basis
  • Example 6 A mixture was prepared comp ⁇ smg, on a weight basis:
  • the resulting dry material contained 0.25% water.
  • LAS Pilot Chemical Co., Middletown, Ohio
  • the solution is mixed until it appears homogeneous.
  • an active aqueous solution of EDDS chelant is added to the aqueous mixture, and the resulting solution is mixed until it appears homogeneous.
  • the EDDS chelant is added to the other two components at room temperature, and contains a minimum of 99%> S,S isomer of the total EDDS isomers and a minimum of 95% S,S isomer of the total ammo acid species.
  • the water is removed from the aqueous mixture m a 5.4 ft 2 steam-jacketed agitated thm film evaporator such as the one supplied by LCI Corporation, Charlotte, North Carolina.
  • the aqueous solution is pumped at a rate of 115 kg/hr to the evaporator, operating at a temperature of 160°C and a pressure of 100 mm Hg
  • the product exits the evaporator at a temperature of 120°C with a moisture content of 0.6%.
  • the product is then cooled in a plate and frame heat exchanger to 35°C. About 14%) of the BPP evaporates with the water in the ATFE.
  • the remaining dried product composition comp ⁇ ses, on a weight basis.
  • Example 7 A mixture was prepared comprising, on a weight basis: Ingredient Amount (%)
  • Example 8 A mixture was prepared comp ⁇ smg, on a weight basis:
  • the mixture was then fed continuously at a rate of 130kg/hr into a 5.5ft 2 ATFE operating at 150°C and lOOmmHg.
  • the resulting dry material contained 0.7% water and had a Newtonian viscosity of 10,000cP.
  • Example 9 A 78% high active paste of the sodium salt of C ⁇ -C 13 fatty acid of linear alkylbenze sulfonate (NaLAS) was mixed with an organic solvent/carrier as well as a chelant to form the following mixture, on a weight basis:
  • the mixture was then fed continuously at a rate of 56.7kg/hr into a 5.5ft 2 ATFE operating at 120°C and 34mmHg.
  • the resulting dry material contained 0.31% water and had a Newtonian viscosity of 6400cP.
  • Example 10 A 78% high active paste of the sodium salt of C ⁇ -C 13 fatty acid of linear alkylbenze sulfonate (NaLAS) was mixed with an organic solvent/earner as well as a chelant to form the following mixture, on a weight basis:
  • NaLAS linear alkylbenze sulfonate
  • the mixture was then fed continuously at a rate of 65kg/hr into a 5.5ft 2 ATFE operating at 140°C and 55mmHg.
  • the resulting dry material contained 0.69% water and had a Newtonian viscosity of 2400cP.

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Abstract

Selon l'invention, on a élaboré des procédés faisant intervenir un solvant organique et étant constitués de composants détergents présents dans des plages spécifiques de manière à produire une composition détergente liquide non aqueuse sans les inconvénients inhérents aux liquides non aqueux. Plus particulièrement, ce procédé permet de produire une composition détergente liquide facile à traiter en grande quantité qui présente une excellente stabilité sur le long terme, et qui est facilement soluble dans une liqueur de lavage.
PCT/US2000/020991 1999-08-03 2000-08-02 Procede de fabrication de compositions detergentes avec additifs WO2001009273A2 (fr)

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BR0012949-6A BR0012949A (pt) 1999-08-03 2000-08-02 Processo para fabricação de composições detergentes com aditivos
MXPA02001202A MXPA02001202A (es) 1999-08-03 2000-08-02 Un procedimiento para elaborar composiciones detergentes con aditivos.
EP00953784A EP1203071B1 (fr) 1999-08-03 2000-08-02 Procede de fabrication de compositions detergentes avec additifs
US10/048,079 US6777381B1 (en) 1999-08-03 2000-08-02 Process for making detergent compositions with additives
AT00953784T ATE272106T1 (de) 1999-08-03 2000-08-02 Verfahren zur herstellung von waschmittelzusammensetzungen mit additiven
DE60012537T DE60012537D1 (de) 1999-08-03 2000-08-02 Verfahren zur herstellung von waschmittelzusammensetzungen mit additiven
AU66175/00A AU6617500A (en) 1999-08-03 2000-08-02 A process for making detergent compositions with additives
JP2001514067A JP2003506524A (ja) 1999-08-03 2000-08-02 添加剤を有する洗剤組成物の製法

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Publication number Priority date Publication date Assignee Title
WO2003010264A1 (fr) * 2001-07-24 2003-02-06 The Procter & Gamble Company Procede ameliore de production de compositions detergentes contenant des additifs
WO2003010275A1 (fr) * 2001-07-24 2003-02-06 The Procter & Gamble Company Procedes de fabrication d'apprets anhydres structures a base de tensioactifs, detergents et compositions les contenant
WO2005087909A1 (fr) * 2004-02-11 2005-09-22 Stepan Company Production de tensioactifs a activite elevee ou a activite super elevee dans un neutraliseur sous vide
EP1931616A2 (fr) 2005-09-07 2008-06-18 Basf Se Procede de neutralisation
US8802799B2 (en) 2005-09-07 2014-08-12 Basf Se Neutralization process
EP2102141B1 (fr) 2005-09-07 2015-04-01 Basf Se Procede de neutralisation

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US7414858B2 (en) 2002-04-11 2008-08-19 Koninklijke Philips Electronics N.V. Method of manufacturing an electronic device

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WO1992009678A1 (fr) * 1990-11-26 1992-06-11 S.B. Chemicals Limited Compositions detergentes liquides
WO1998000516A1 (fr) * 1996-06-28 1998-01-08 The Procter & Gamble Company Preparation de compositions detergentes liquides non aqueuses contenant des particules, a phase liquide structuree a l'aide d'un tensioactif
WO1998000518A1 (fr) * 1996-06-28 1998-01-08 The Procter & Gamble Company Preparation de compositions detergents liquides non aqueuses contenant des particules, avec pretraitement des elements secs

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WO1992009678A1 (fr) * 1990-11-26 1992-06-11 S.B. Chemicals Limited Compositions detergentes liquides
WO1998000516A1 (fr) * 1996-06-28 1998-01-08 The Procter & Gamble Company Preparation de compositions detergentes liquides non aqueuses contenant des particules, a phase liquide structuree a l'aide d'un tensioactif
WO1998000518A1 (fr) * 1996-06-28 1998-01-08 The Procter & Gamble Company Preparation de compositions detergents liquides non aqueuses contenant des particules, avec pretraitement des elements secs

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003010264A1 (fr) * 2001-07-24 2003-02-06 The Procter & Gamble Company Procede ameliore de production de compositions detergentes contenant des additifs
WO2003010275A1 (fr) * 2001-07-24 2003-02-06 The Procter & Gamble Company Procedes de fabrication d'apprets anhydres structures a base de tensioactifs, detergents et compositions les contenant
US6740630B2 (en) 2001-07-24 2004-05-25 The Procter & Gamble Company Processes for making substantially anhydrous structured surfactant pastes and other detergent ingredients and compositions employing same
US6770613B2 (en) 2001-07-24 2004-08-03 The Procter & Gamble Company Process for making detergent compositions with additives
WO2005087909A1 (fr) * 2004-02-11 2005-09-22 Stepan Company Production de tensioactifs a activite elevee ou a activite super elevee dans un neutraliseur sous vide
EP1931616A2 (fr) 2005-09-07 2008-06-18 Basf Se Procede de neutralisation
US8802799B2 (en) 2005-09-07 2014-08-12 Basf Se Neutralization process
EP2102141B1 (fr) 2005-09-07 2015-04-01 Basf Se Procede de neutralisation
EP1940766B2 (fr) † 2005-09-07 2019-09-04 Basf Se Procede de neutralisation

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WO2001009273A3 (fr) 2001-09-13
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BR0012949A (pt) 2002-04-30
JP2003506524A (ja) 2003-02-18

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