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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/38—Cationic compounds
  • C11D1/645—Mixtures of compounds all of which are cationic
• • 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
  • C11D1/38—Cationic compounds
  • C11D1/52—Carboxylic amides, alkylolamides or imides or their condensation products with alkylene oxides
  • C11D1/525—Carboxylic amides (R1-CO-NR2R3), where R1, R2 or R3 contain two or more hydroxy groups per alkyl group, e.g. R3 being a reducing sugar rest
• • 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
  • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
• • 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
  • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
  • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/38—Cationic compounds
  • C11D1/62—Quaternary ammonium compounds

Definitions

• This invention concerns liquid premixes comprising certain nonionic surfactants, including fatty acid amides, which are suitable for further processing into detergent granules, especially for spraying on to prepared base granules to provide a finished granular detergent product.
• the polyhydroxy fatty acid amides are one class of nonionic surfactants which are currently being investigated for use in detergent compositions.
• One problem with this class of surfactants is that concentrated aqueous solutions containing them tend to precipitate and/or gel on storage, even at elevated temperatures (35-60°).
• low temperature storage of this family of amide surfactants is of great importance, since at elevated temperatures they are susceptible to degradation via hydrolysis of the amide bond to give the amine and the fatty acid.
• polyhydroxy fatty acid amides are stored below 35°C this degradation is negligible, i.e. less than 5-10% per year, but at elevated temperatures it becomes highly significant, rising to about 10% per month at 50°C and about 20-25% per month at 60°C.
• WO 9206160 published April 16th, 1992, describes aqueous compositions comprising polyhydroxy fatty acid amides and ethoxylated nonionic surfactants. Ratios between 1:5 and 5:1 are claimed.
• Non-aqueous premixes typically have high melting points (about 135°C for C16-18 glucose amide), and consequently for ease of processing it is necessary to depress the melting point of the amide by addition of suitable melting point depressants.
• Ethoxylated nonionic surfactants are suitable for this purpose if they are added at high levels, for example 2 parts ethoxylated nonionic to 1 part polyhydroxy fatty acid amide.
• WO9000189 published January 11th, 1990, describes a process of spraying nonionic surfactant premix on to a base powder. It is claimed that solubility and dispersibility are improved if the nonionic premix comprises from 1% to 40% of hydrophobic substance containing polar groups (such as fatty acid, fatty acid ester, fatty acid amide, fatty amine, fatty alcohol or quaternary ammonium compound). There is no mention of problems associated with high melting points of any of the hydrophobic substances.
• hydrophobic substance containing polar groups such as fatty acid, fatty acid ester, fatty acid amide, fatty amine, fatty alcohol or quaternary ammonium compound.
• borate functional materials have been suggested as melting point depressants for both aqueoues and non-aqueous premixes.
• EP592754 published April 20th, 1994, describes a liquid premix comprising polyhydroxy fatty acid amide and a borate functional material.
• the benefit claimed is that the premix does not solidify or gel at temperatures above about 20-30°C.
• borate functional materials may be unnecessary, or even undesirable in granular laundry detergents.
• the present invention addresses the problem of providing an alternative melting point depressant for use in non-aqueous liquid premixes comprising polyhydroxy fatty acid amide. It has been found that choline ester acts to reduce the melting point of a typical polyhydroxy fatty acid amide / ethoxylated nonionic premix. The presence of 10% by weight of choline ester reduces the melting point by about 12°C. The possibility of storage and handling at lower temperatures has the further benefit of handling higher concentrations of polyhydroxy fatty acid amide than would be possible without the melting point depressant, and additionally reduces the rate of product decomposition.
• the present invention provides storage-stable, pumpable fluid compositions which contain relatively high concentrations of polyhydroxy fatty acid amide surfactants. Moreover, the invention provides such fluid compositions using ingredients which are either innocuous in the finished detergent composition, or which can provide desirable benefits to said finished compositions. Accordingly, removal of such ingredients is not required.
• the invention concerns a concententrated liquid premix comprising polyhydroxy fatty acid amide of the formula: where R is C5-C31 hydrocarbyl, preferably straight-chain C7-C19 alkyl or alkenyl, R1 is C1-C8, preferably C1-C4 hydrocarbyl, and Z is polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least 2, preferably at least 3 hydroxyls directly connected to the chain, wherein the liquid premix further comprises from 1% to 30% , preferably from 5% to 10%, by weight of choline ester.
• polyhydroxy fatty acid amide is C12-C18 linear alkyl N-methyl glucamine at a level of at least 25% by weight, even more preferably from 50% to 80% by weight, and most preferably from 60% to 75% by weight.
• the molar ratio of the polyhydroxy fatty acid amide to the choline ester is from 20:1 to 2:1.
• liquid premix is essentially anhydrous.
• Preferred embodiments may, however comprise from 5% to 50% by weight of ethoxylated nonionic surfactant, and may also optionally comprise from 1% to 40% by weight of a solvent chosen from propylene glycol, ethanol, glycerine or mixtures thereof.
• the present invention also concerns a process of treating the liquid premix mentioned above to form granules by spraying the premix onto a preformed adsorbent detergent power.
• granules may be formed by agglomerating finely divided detergent powders in the presence of the premix, preferably in a high shear mixer.
• concentrate liquid premix herein is meant percentages of the polyhydroxy fatty acid amide typically in the range of at least 25% by weight, preferably 35% to 80% by weight, and most preferably from 45% to 75% by weight.
• pumpable herein is meant a viscosity below about 20 000 mPas, preferably below about 12 000 mPas.
• Viscosity is measured by means of a Brookfield Viscometer Model DVII with a Thermosel System. The viscosity of the systems is measured at 80°C.
• stable liquid premix herein is meant a homogeneous, fluid, nonbirefringent liquid. This can be estimated visually using polarised light, and can be confirmed using a microscope under polarised light. There should be no crystallisation or precipitation when a sample is examined by the naked eye.
• Polyhydroxy fatty acid amides may be produced by reacting a fatty acid ester and an N-alkyl polyhydroxy amine.
• the preferred amine for use in the present invention is N-(R1)-CH2(CH2OH)4-CH2-OH and the preferred ester is a C12-C20 fatty acid methyl ester. Most preferred is the reaction product of N-methyl glucamine with C12-C20 fatty acid methyl ester.
• N-methyl glucamine is reacted with a C12-C20 methyl ester.
• formulator of granular detergent compositions may find it convenient to run the amidation reaction in the presence of solvents which comprise alkoxylated, especially ethoxylated (EO 3-8) C12-C14 alcohols (page 15, lines 22-27).
• solvents which comprise alkoxylated, especially ethoxylated (EO 3-8) C12-C14 alcohols (page 15, lines 22-27).
• EO 3-8 alkoxylated
• C12-C14 alcohols page 15, lines 22-27
• Nonionic surfactant systems, and granular detergents made from such systems have been described in WO 92 6160, published on 16th April, 1992.
• This application describes (example 15) a granular detergent composition prepared by fine dispersion mixing in an Eirich RV02 mixer which comprises N-methyl glucamide (10%), nonionic surfactant (10%). Both of these patent applications describe nonionic surfactant systems together with suitable manufacturing processes for their synthesis, which have been found to be suitable for use in the present invention.
• the polyhydroxy fatty acid amide may be present in compositions of the present invention at a level of from 0% to 40% by weight of the detergent component or composition, preferably from 1% to 30% by weight, even more preferably from 1% to 20% by weight.
• Preferred choline ester derivatives having the following formula : wherein R is a C5 to C30 straight chain or branched chain alkyl or alkenyl, group and X is an anion, which makes the compound at least water-dispersible, preferably selected from the group consisting of halide, methyl sulfate, sulfate, and nitrate, preferably methyl sulfate, chloride, bromide or iodide. as well as those wherein the ester linkage in the above formula is replaced with a reverse ester, amide or reverse amide linkage.
• the preferred choline-derivative cationic substances may be prepared by the direct esterification of a fatty acid of the desired chain length with dimethylaminoethanol, in the presence of an acid catalyst. The reaction product is then quaternized with a methyl halide, forming the desired cationic material.
• the choline-derived cationic materials may also be prepared by the direct esterification of a long chain fatty acid of the desired chain length together with 2-haloethanol, in the presence of an acid catalyst material. The reaction product is then used to quaternize. Trimethylamine, forming the desired cationic component.
• Suitable choline esters for use herein have the formula: wherein t is 0 or 1, y is from 1 to 20, and R and X are as defined above.
• the choline esters herein can be present at levels of from 0% to 50% by weight of the compositions, preferably from 1% to 30% by weight, even more preferably from 1% to 20% by weight.
• non-aqueous premixes of the present invention may be incorporated into granular laundry detergent compositions by any of the techniques known in the art. Granulation by agglomeration is one particularly preferred process. Spraying the premix onto a prepared base powder is an alternative preferred process.
• liquid premix of the present invention is intimately mixed with finely divided detergent powders, such as sodium aluminosilicate or other builders, in a high shear mixer, such as a Loedige® CB unit.
• Finely divided detergent powders such as sodium aluminosilicate or other builders
• a high shear mixer such as a Loedige® CB unit.
• Agglomerates may be finished in further mixing units, such as a Loedige® KM, or a fluidised bed.
• the choline ester is handled in a propylene glycol solvent in a ratio of 7 parts choline ester to 3 parts propylene glycol (Examples 1 to 3) or 3 parts alkyl ethoxylate (Examples 4 to 6).
• Example 1 Example 2 Example 3 C16-18 N-methyl glucamide 27 36 45 C12-15 alkyl ethoxylate (3EO) 63 54 45 C12-14 Choline Ester 7 7 7 Propylene glycol 3 3 3 Melting Point* (°C) 67 64 63 *Melting Point is determined my means of Differential Scanning Calorimetry (DSC)
• Example 4 Example 5 Example 6 C16-18 N-methyl glucamide 27 36 45 C12-15 alkyl ethoxylate (3EO) 63 54 45 C12-14 Choline Ester 7 7 7 C12-14 Alkyl ethoxylate (3EO) 3 3 3 3 Melting Point* (°C) 67 65 63 *Melting Point is determined my means of Differential Scanning Calorimetry (DSC)
• Each of the liquid premix compositions of Examples 1 to 3 and A to F were prepared by mixing the raw materials in the appropriate ratios.
• the compositions were maintained at a temperature above the indicated melting point during transportation and storage.
• the lower storage temperatures of Examples 1 to 3, compared to Examples A to F, resulted in slower rates of degradation of the premix.
• liquid premix compositions were then sprayed on to a detergent base powder that had been prepared by agglomeration (of surfactants, builders etc.) and dry mixing (of granular percarbonate bleach, citric acid, granular suds suppressor, granular bleach activator, granular carbonate and bicarbonate, enzymes and encapsulated perfume).
• the ratio was 1 part liquid premix to 9 parts detergent base powder.
• the temperature of the premix was reduced immediately before the spraying step to between 10° and 20°C below the indicated melting point so that crystallisation of the premix was starting to occur, but not to the extent that it would cause blockage of the nozzles.
• the spraying temperature was between 46°C and 50°C for Examples 1 to 3, and between 58°C and 62°C for Examples A to F (i.e a reduction of about 12°C in spraying on temperature).
• Example 1 to 3 resulted in free-flowing detergent compositions.
• Example A to F resulted in compositions with a significant amount of lumps and oversize particles (Example C being worse than Example A and F being worse than example D).
• Example 1 to 3 showed better stability of the heat sensitive components, such as enzymes, than Examples A to F.

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• Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Chemistry (AREA)
• Detergent Compositions (AREA)

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Cited By (15)

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Citations (5)

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• 1994
  • 1994-10-28 EP EP94203141A patent/EP0709449A1/de not_active Withdrawn
• 1995
  • 1995-10-12 WO PCT/US1995/013562 patent/WO1996013564A1/en not_active Ceased

Patent Citations (5)

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