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WO1998035010A1 - Composition particulaire d'additif de blanchiment a utiliser dans des compositions de detergent granulaires - Google Patents

Composition particulaire d'additif de blanchiment a utiliser dans des compositions de detergent granulaires Download PDF

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Publication number
WO1998035010A1
WO1998035010A1 PCT/US1998/002528 US9802528W WO9835010A1 WO 1998035010 A1 WO1998035010 A1 WO 1998035010A1 US 9802528 W US9802528 W US 9802528W WO 9835010 A1 WO9835010 A1 WO 9835010A1
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WO
WIPO (PCT)
Prior art keywords
additive composition
bleach
linear
alkyl group
activator
Prior art date
Application number
PCT/US1998/002528
Other languages
English (en)
Inventor
Robert Louis Bill
Scott William Capeci
Original Assignee
The Procter & Gamble Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by The Procter & Gamble Company filed Critical The Procter & Gamble Company
Publication of WO1998035010A1 publication Critical patent/WO1998035010A1/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
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3905—Bleach activators or bleach catalysts
    • C11D3/3935—Bleach activators or bleach catalysts granulated, coated or protected
    • 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0034—Fixed on a solid conventional detergent ingredient
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
    • 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
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites
    • 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
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2079—Monocarboxylic acids-salts thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3707—Polyethers, e.g. polyalkyleneoxides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3905—Bleach activators or bleach catalysts
    • C11D3/3907—Organic compounds
    • C11D3/3917—Nitrogen-containing compounds

Definitions

  • the invention generally relates to a particulate bleach additive composition, and more particularly, to a composition containing unsymmetrical acyclic imide bleach activators in particulate form for easy incorporation into granular detergent compositions.
  • the particulate bleach additive composition is particularly useful in laundry, automatic dishwashing and hard surface cleaning compositions.
  • BACKGROUND OF THE INVENTION The formulation of bleaching compositions which effectively removes a wide variety of soils and stains from fabrics under wide-ranging usage conditions remains a considerable challenge, especially in the laundry detergent industry. Challenges are also faced by the formulator of hard surface cleaning compositions and automatic dishwashing detergent compositions (ADD's), which are expected to efficiently cleanse and sanitize dishware, often under heavy soil loads.
  • ADD's automatic dishwashing detergent compositions
  • the challenges associated with the formulation of truly effective cleaning and bleaching compositions have been increased by legislation which limits the use of effective ingredients such as phosphate builders in many regions of the world.
  • Oxygen bleaching agents such as hydrogen peroxide
  • Oxygen bleaching agents have found particular acceptance in laundry products such as detergents, in automatic dishwashing products and in hard surface cleaners. Oxygen bleaching agents, however, are somewhat limited in their effectiveness. Some frequently encountered disadvantages include color damage on fabrics and surfaces.
  • oxygen bleaching agents tend to be extremely temperature rate dependent. Thus, the colder the solution in which they are employed, the less effective the bleaching action. Temperatures in excess of 60°C are typically required for effectiveness of an oxygen bleaching agent in solution.
  • bleach activators typically perhydrolyzable acyl compounds having a leaving group such as oxybenzenesulfonate, react with the active oxygen group, typically hydrogen peroxide or its anion, to form a more effective peroxyacid oxidant. It is the peroxyacid compound which then oxidizes the stained or soiled substrate material.
  • bleach activators are also somewhat temperature dependent. Bleach activators are more effective at warm water temperatures of from about 40°C to about 60°C. In water temperatures of less than about 40°C, the peroxyacid compound loses some its bleaching effectiveness.
  • activator materials should be safe, effective, and will preferably be designed to interact with troublesome soils and stains.
  • Various activators have been described in the literature. Many are esoteric and expensive. It has now been determined that certain selected bleach activators are unexpectedly effective in removing both hydrophilic and hydrophobic soils and stains from fabrics, hard surfaces and dishes. When formulated as described herein, bleach additive and bleaching compositions are provided using the selected bleach activators to remove soils and stains not only from fabrics, but also from dishware in automatic dishwashing compositions, from kitchen and bathroom hard surfaces, and the like, with excellent results.
  • spraying the liquid activator onto detergent granules deposits the activator on the outer surface of the granules which is readily exposed to the moisture in the atmosphere, especially when the product is stored for extended periods of time prior to use.
  • the exposure to moisture or water prior to use renders the bleach activator compound unstable, and therefore, reduces its effectiveness when ultimately used.
  • This decreased shelf-life as a result of spraying the liquid activator onto the detergent composition is extremely undesirable and can have detrimental commercial effects on the product in which the activator is contained.
  • Attempts at embodying such liquid activators in particulate form have also failed in that the activity of the activator is not retained due to particles susceptibility to moisture. Additionally, embodying these liquid activators in particulate form at very high active levels has been difficult, as well.
  • a bleach activator additive which provides satisfactory performance on both hydrophilic and hydrophobic soils and stains, and which is safe, effective, and designed to interact with troublesome soils and stains.
  • a bleach additive composition having improved physical properties and performance even when incorporated into fully formulated detergent compositions.
  • the invention meets the aforementioned needs by providing a particulate bleach additive composition containing an unsymmetrical acyclic imide bleach activator compound (e.g. N-Methyl N-Nonyl Aceta ide or "NMA") which has optimum performance and physical properties.
  • an unsymmetrical acyclic imide bleach activator compound e.g. N-Methyl N-Nonyl Aceta ide or "NMA”
  • the particulate bleach additive composition can be incorporated into granular detergent compositions without detrimentally affecting the physical properties or the activity of the unsymmetrical acyclic imide bleach activator compound contained therein.
  • a particulate bleach additive composition comprises: (a) from about 1% to about 90% by weight of carrier particles; (b) from about 1% to about 70% by weight of a liquid bleach activator compound having the formula
  • R ⁇ is a C7-C13 linear or branched chain saturated or unsaturated alkyl group
  • R2 is a C 1 -Cg linear or branched chain saturated or unsaturated alkyl group
  • R3 is a C1 -C4 linear or branched chain saturated or unsaturated alkyl group
  • a particulate bleach additive composition comprises: (a) from about 1% to about 90% by weight of carrier particles; (b) from about 1% to about 70% by weight of a liquid bleach activator compound having the formula
  • R ⁇ is a C7-C13 linear or branched chain saturated or unsaturated alkyl group
  • R2 is a Cj-Cg linear or branched chain saturated or unsaturated alkyl group
  • R3 is a C1-C4 linear or branched chain saturated or unsaturated alkyl group
  • a binder system including (i) from about 0.5% to about 15% of C12-13 linear alkylbenzene sulfonate surfactant, (ii) from about 1% to about 25% of polyethylene glycol, (iii) from about 0.5% to about 10% of pelargonic acid, and (iv) from about 1% to about 25% of palmitc acid.
  • the bleach activator and the binder are coated in and onto the carrier particles.
  • a detergent composition comprises: (a) detergent granules containing a detersive surfactant and a builder; and (b) a particulate bleach additive composition including, by weight of the additive composition, (i) from about 1% to about 90% of carrier particles; (ii) from about 1% to about 70% of a liquid bleach activator compound having the formula
  • R ⁇ is a C7-C13 linear or branched chain saturated or unsaturated alkyl group
  • R2 is a Ci-Cg linear or branched chain saturated or unsaturated alkyl group
  • R3 is a C1-C4 linear or branched chain saturated or unsaturated alkyl group
  • (iii) from about 1% to about 75% of a liquid binder Die bleach activator and the binder are coated in and onto the carrier particles.
  • the invention also provides a method of laundering soiled fabrics comprising the steps of contacting the fabrics in an aqueous medium with an effective amount of a detergent composition as described herein.
  • One aspect of the invention involves a particulate bleach additive composition that unexpectedly possesses superior performance and physical properties even when incorporated into fully formulated detergent compositions. It is essential for the bleach additive composition to include carrier particles and a liquid bleach activator.
  • the binder can include one or more of several ingredients as detailed hereinafter.
  • the invention also provides detergent compositions used in laundry or dishwashing applications which include the particulate bleach additive composition of the invention. Such detergent compositions typically include granules containing a detersive surfactant and a builder.
  • the detergent compositions will also include a source of hydrogen peroxide as detailed more particularly hereinafter.
  • the carrier particles are selected from the group consisting of silicas, aluminosilicates and mixtures thereof. Particularly preferred carrier particles are precipitated silica particles and amorphous aluminosilicate particles. Most preferably, the carrier is precipitated silica particles which are commercially available from Huber Corporation under the trade name Zeothix 265. The precipitated silica particles preferably have a median particle size of from about 0.5 microns to about 10 microns. It should be understood that a wide variety of particulate carrier materials can be used beyond those specifically mentioned herein without deviating from the scope of the invention.
  • the additive composition requires a binder to be employed which is a hydrophilic material that is capable of binding particles together, and preferably in liquid form.
  • a binder which is a hydrophilic material that is capable of binding particles together, and preferably in liquid form.
  • surfactants include anionic surfactants such as linear alkylbenzene sulfonate and nonionic surfactants such as alkyl ethoxylated sulfates.
  • the binder provides a moisture and alkalinity barrier for the particulate bleach additive composition such that it does not degrade prior to use.
  • the binder system may employ an ingredient to "crispen” or otherwise impart hardness to the particles, such as polyethylene glycol, polyvinylpyrrolidone (PVP), polyvinylpyridine N-oxide (PVNO) or Copolymers of N-vinylpyrrolidone and N-vinylimidazole (PVPVI).
  • an ingredient to "crispen” or otherwise impart hardness to the particles such as polyethylene glycol, polyvinylpyrrolidone (PVP), polyvinylpyridine N-oxide (PVNO) or Copolymers of N-vinylpyrrolidone and N-vinylimidazole (PVPVI).
  • Another optional ingredient is an acidic coating which protects the bleach activator in the bleach additive composition from degradation as a result of exposure to alkalinity.
  • the preferred ingredient is palmitic acid.
  • Another similar material which is suitable for use herein is citric acid. Additionally, an ingredient which reduces friability or "chipping" of the resultant particulate bleach additive composition may be included. Such ingredients include, but are not limited to pelargonic acid, and C j 2_i3 linear alkylbenzene sulfonate.
  • the binder includes only from about 0.5% to about 15%, preferably from about 1.5% to about 10%, and most preferably from about 2.5% to about 6.0%, by weight of the bleach additive composition, of Cj2-13 linear alkylbenzene sulfonate surfactant.
  • the preferred binder system may also include from about 0.5% to about 10%, preferably from about 1% to about 10%, and most preferably from about 2% to about 5%, by weight of the bleach additive composition, of pelargonic acid.
  • Another ingredient in the preferred binder system is from about 1% to about 25%, preferably from about 3% to about 20%, and most preferably from about 5% to about 12%, by weight of the bleach additive composition, of palmitic acid.
  • the unsymmetrical acyclic bleach activators employed in the invention are unsymmetrical' acyclic imide bleach activators.
  • the unsymmetrical acyclic imide activators used in the present invention have the formula: (I)
  • R ] is a C7-C 13 linear or branched chain saturated or unsaturated alkyl group
  • R2 is a Cj-Cg linear or branched chain saturated or unsaturated alkyl group
  • R3 is a C 1-C4" linear or branched chain saturated or unsaturated alkyl group.
  • Preferred activators are those in which the R ⁇ is a C7-C ] j linear or branched saturated alkyl group, more preferably, R ⁇ is a C7-C 1 1 saturated alkyl group, R2 is a C1-C4 linear or branched saturated alkyl group and R3 is a C1 -C4 linear or branched chain saturated or unsaturated alkyl group. More preferably, R2 and R3 are C ⁇ -C4 linear saturated alkyl groups and even more preferably are the same.
  • activators according to the present invention are the N- alkanoyl-N-methyl acetamides.
  • the activators have the formula (I) wherein both R2 and R3 are methyl groups.
  • N-alkanoyl-N-methyl acetamides have the formula:
  • Rl ⁇ N Me I Me where Ri is C7-C1 1 linear saturated alkyl group. Particularly preferred are N- octanoyl-N-methyl acetamide (when Ri is C7), N-nonanoyl-N-methyl acetamide (when R ⁇ is Cg), N-decanoyl-N-methyl acetamide (when Ri is CQ) and N-dodecanoyl-N- methyl acetamide (when R ⁇ is C j 1 ).
  • the solubility of the compound decreases.
  • the activators of the present invention are ideally soluble for optimum performance of the activators, it is preferred that the number of carbon atoms in the activator compound be such that the activator compound displays satisfactory solubility profiles.
  • the sum of the carbons in Ri , R2 and R3 is preferably less than 19 and more preferably less than 15.
  • the unsymmetrical acyclic imide bleach activators used in the present invention provide superior bleaching ability and performance over the bleach activators of the prior art.
  • the unsymmetrical acyclic imide bleach activators of the present invention provide both hydrophobic and hydrophilic bleaching agents in aqueous solutions. This is believed to be due to the fact that perhydrolysis can occur at either of the carbonyl groups in the activator. Thus, any molecule of the activators of formula (I) would undergo perhydrolysis in an aqueous solution to form either a bleaching agent (R ] C(0)OOH) having hydrophobic properties and a bleaching agent (R3C(0)OOH) having hydrophilic properties when R ⁇ and R3 are defined as above.
  • the bleaching agent may of course be protonated or deprotonated depending upon the in-use pH.
  • a bleaching solution will then include both the hydrophilic bleaching agent and the hydrophobic bleaching agent.
  • the bleaching capabilities of a mixed activator system hydrophobic and hydrophilic
  • Elimination of mixed activator systems may provide enormous potential benefits by eliminating the significant expense of an additional bleach activator.
  • the bleach activators of formula (I) are liquids at or above room temperature.
  • the process of the instant invention involves producing a particulate bleach additive composition via initially blending a liquid bleach activator with carrier particles to form a powder which contains the bleach activator.
  • the carrier particles are comprised of a particulate carrier material selected from the group consisting of silicas, aluminosilicates and mixtures thereof.
  • Particularly preferred carrier particles are precipitated silica particles and amorphous aluminosilicate particles.
  • the carrier particles are precipitated silica particles which are commercially available from Huber Corporation under the trade name Zeothix 265.
  • the precipitated silica particles preferably have a median particle size of from about 0.5 microns to about 10 microns.
  • the blending step can be carried forth in any conventional stirred vessel such as a Cuisinart Food Processor, Eirich Type R Mixer, Lodige CB or KM mixer.
  • a preferred embodiment of the process entails mixing the liquid bleach activator and carrier particles in a weight ratio of from 1 : 10 to about 10: 1, preferably at a weight ratio of about 1 : 1.
  • the powdered activator is either granulated or agglomerated with a binder to form the particulate bleach additive composition.
  • the binder as well as the liquid bleach activator are detailed hereinafter.
  • a preferred embodiment of the process entails mixing the binder and powdered activator in a weight ratio of from 1 : 10 to about 5: 1, preferably at a weight ratio of about 1 :3.
  • the granulation step of the process can be carried forth in a dome granulator, e.g. commercially available from LCI Co ⁇ oration under the trade name Laboratory Dome Granulator Model DG-L1.
  • Other granulation equipment which can be used include extruders, extructors, roll compactors and the like.
  • the process may include a spheronization step following the granulation step to "round" the particles, and thereby improve the flow properties of the resulting particulate bleach additive composition.
  • Such an optional process step may be carried forth in equipment commercially available from LCI Corporation sold under the trade name Marumerizer.
  • the agglomeration step can be carried forth in equipment including but not limited to Eirich R type mixers commercially available from Eirich Machines, Inc., Schugi Granulators available from Hosokawa Bepex and sold under the trade name Flex-O-Mix, mixer/densifiers available from L ⁇ dige (Germany) sold as Lodige CB or KM mixers, e.g., L ⁇ dige CB 30 Recycler.
  • Eirich R type mixers commercially available from Eirich Machines, Inc.
  • Schugi Granulators available from Hosokawa Bepex and sold under the trade name Flex-O-Mix
  • mixer/densifiers available from L ⁇ dige (Germany) sold as Lodige CB or KM mixers, e.g., L ⁇ dige CB 30 Recycler.
  • the residence time of the powdered activator in both the granulation step and the agglomeration step will be from about 0.2 minutes to about 15 minutes.
  • the residence time will vary depending upon the actual number of granulating or agglomerating mixers used and the other operating parameters of the equipment.
  • the temperature of the liquid activator is preferably from about 50°C to about 70°C, and the binder is added while preferably at from about 65°C to about 95°C. In this way, a particulate bleach additive composition having unexpectedly superior flow properties and performance is produced which can be admixed with other detergent compositions such as those used in conventional laundering operations.
  • one or more additional process steps may be used in the process invention to enhance the properties of the particulate bleach additive composition.
  • the granulated or agglomerated bleach additive produced may be dried in a conventional fluid bed dryer or other known drying apparatus.
  • the particulate bleach additive composition may be cooled in a fluid bed cooler. Both of these optional processing steps enhance the physical properties of the particulate bleach additive compositions.
  • liquid bleach activator is mixed with a liquid h>drophilic material so as to enhance the solubility of the bleach activator in the aqueous washing solution to which it is ultimately added.
  • a liquid h>drophilic material is suitable for use herein, one convenient liquid would be a nonionic surfactant.
  • the median particle size of the bleach additive composition may be beneficial to target the median particle size of the bleach additive composition so as to facilitate incorporation into fully formulated detergent products and/or further impros e ph> sical properties such a free flow and reduce particle size segregation during storage.
  • the median particle size it is preferable for the median particle size to be in a range from about 500 microns to about 1000 microns, and most preferably from about 700 microns to about 800 microns. This can be accomplished by conventional sieving and grinding (for the oversized particles) and recycling (for the undersized particles) processing steps.
  • the admixed ingredients such as the particulate bleach additive composition produced by the present invention are incorporated after the base granules and/or agglomerates containing the common ingredients are formed.
  • detergent granules can be formed in a spray-drying tower which contain a detersive surfactant and builder to which liquid adjunct ingredients such as perfumes, some enzymes, some optical brighteners and the like are added via spraying.
  • the dry admixed ingredients such as the particulate bleach additive composition are admixed with the fully formulated detergent composition.
  • Such a process is also envisioned by the instant process invention.
  • the particulate bleach additive compositions of the invention can be incorporated into fully formulated laundry, hard surface cleaning, and automatic dishwashing compositions.
  • the particulate bleach additive of the present invention as described above are generally employed in combination with a source of hydrogen peroxide in the fully formulated compositions.
  • Levels of particulate bleach additive in the fully formulated compositions may vary widely, e.g., from about 0.1% to about 90%, by weight of the composition, although lower levels, e.g., from about 0.1% to about 30%, or from about 0.1% to about 20% by weight of the composition are more typically used.
  • the source of hydrogen peroxide herein is any convenient compound or mixture which under consumer use conditions provides an effective amount of hydrogen peroxide. Levels may vary widely and are typically from about 0.1% to about 70%, more typically from about 0.2% to about 40% and even more typically from about 0.5% to about 25%, by weight of the bleaching compositions herein.
  • the source of hydrogen peroxide used herein can be any convenient source, including hydrogen peroxide itself.
  • perborate e.g., sodium perborate (any hydrate but preferably the mono- or tetra-hydrate), sodium carbonate peroxyhydrate or equivalent percarbonate salts, sodium pyrophosphate peroxyhydrate, urea peroxyhydrate, or sodium peroxide can be used herein. Mixtures of any convenient hydrogen peroxide source can also be used.
  • a preferred percarbonate bleach comprises dry particles having an average particle size in the range from about 500 micrometers to about 1,000 micrometers, not more than about 10% by weight of said particles being smaller than about 200 micrometers and not more than about 10% by weight of said particles being larger than about 1,250 micrometers.
  • the percarbonate can be coated with silicate, borate or water-soluble surfactants.
  • Percarbonate is available from various commercial sources such as FMC, Solvay and Tokai Denka.
  • the source of hydrogen peroxide and unsymmetrical bleach activator are typically at a ratio of from about 1 :3 to about 20: 1, as expressed on a basis of peroxide:activator in units of moles H2O2 delivered by the hydrogen peroxide source to moles bleach activator.
  • Fully formulated compositions including the particulate bleach additive composition typically will also comprise other adjunct ingredients to improve or modify performance. Typical, non-limiting examples of such ingredients are disclosed hereinafter.
  • Adjunct ingredients can include one or more materials for assisting or enhancing cleaning performance, treatment of the substrate to be cleaned, or to modify the aesthetics of the fully formulated composition in which the particulate bleach additive composition of the invention is included.
  • Usual detersive surfactants, builders and other adjuncts for detergent compositions are included in U.S. Pat. No. 3,936,537, Baskerville et al.
  • Adjuncts which can also be included in their conventional art- established levels for use (generally from 0% to about 20% of the detergent ingredients, preferably from about 0.5% to about 10%), include other active ingredients such as bleach catalysts, enzymes, enzyme stabilizers, color speckles, anti-tarnish and/or anti- corrosion agents, dyes, fillers, optical brighteners, germicides, alkalinity sources, hydrotropes, anti-oxidants, perfumes, dyes, solubilizing agents, clay soil removal/anti- redeposition agents, carriers, processing aids, pigments, fabric softeners, static control agents, solid fillers for bar compositions, etc.
  • active ingredients such as bleach catalysts, enzymes, enzyme stabilizers, color speckles, anti-tarnish and/or anti- corrosion agents, dyes, fillers, optical brighteners, germicides, alkalinity sources, hydrotropes, anti-oxidants, perfumes, dyes, solubilizing agents, clay soil removal/anti- redeposition agents, carriers, processing
  • Dye transfer inhibiting agents including polyamine N-oxides such as polyvinylpyridine N-oxide can be used.
  • Dye-transfer-inhibiting agents are further illustrated by polyvinylpyrrolidone and copolymers of N-vinyl imidazole and N-vinyl pyrrolidone.
  • suds boosters such as the C 1 n-C j alkanolamides can be incorporated into the compositions, typically at 1%-10% levels.
  • the C ⁇ -C ] 4 monoethanol and diethanol amides illustrate a typical class of such suds boosters.
  • suds boosters with high sudsing adjunct surfactants such as the amine oxides, betaines and sultaines noted above is also advantageous.
  • soluble magnesium salts such as MgCl2, MgS ⁇ 4, and the like, can be added at levels of, typically, 0.1%-2%, to provide additional suds and to enhance grease removal performance.
  • EXAMPLE I a. Preparation of n-Methyl Nonanoyl Amide A 50 L, 3-necked round-bottomed flask equipped with a 2 L pressure equalizing addition funnel, mechanical stirrer, argon inlet, thermometer, and reflux condenser is charged with methylamine (40 wt% in water, 8 L, 93 mol, 2.5 eq) and cooled in an ice/methanol bath to 10 °C. Nonanoyl chloride/diethyl ether (approximately 1 : 1 volume ratio) is mixed in the addition funnel and added to the aqueous methylamine at a rate slow enough to maintain reaction temperature below 30 °C.
  • methylamine 40 wt% in water, 8 L, 93 mol, 2.5 eq
  • Nonanoyl chloride/diethyl ether (approximately 1 : 1 volume ratio) is mixed in the addition funnel and added to the aqueous methylamine at a rate
  • the reaction is stirred slowly enough to allow the organic and aqueous layers to remain separate.
  • 2 L of diethyl ether is added directly to the reaction.
  • Nonanoyl chloride/diethyl ether is then added in higher ratio until 6.59 kg (37.3 mol) of nonanoyl chloride and 14 L of diethyl ether has been added.
  • the stirred reaction is allowed to slowly warm to room temperature overnight.
  • NMA N-nonanoyl-N-methylacetamide
  • EXAMPLE II a Preparation of n-Methyl Nonanoyl Amide Under nitrogen pressure, 20.39 lbs. of liquid monomethyl amine (MMA) is pushed into a 25 gallon agitated pressure vessel. The pressure vessel is held at a pressure of about 25-40 PSIG after MMA addition. The vessel's agitator is started. 51.95 lbs. of pelargonic acid is added to the vessel over a 0.5 to 1 hour period through a diaphragm pump. The reactor temperature rises to about 60- 100 F and 50- 100 PSIG during acid addition. When all of the acid is in the reactor, heating is started while agitation continues. The reactor is raised to 325-330 °F .
  • MMA liquid monomethyl amine
  • the remaining MMA and water that resulted from the amidation reaction are removed in the glass lined reactor at 122 °F and less than about 10 mm Hg vacuum.
  • the reactor pressure is set at 100 mm Hg and 335.1 lbs.
  • acetic anhydride is pulled in from a drum on a weigh scale via a Teflon lined stainless steel hose.
  • the reactor is returned to atmospheric pressure by breaking vacuum with nitrogen. Heating and agitation are continued.
  • the reactor is heated to 248 °F and sampled hourly and the samples analyzed by gas chromatography (GC). After approximately 10 hours conversion to crude NMA is 87.2%.
  • GC gas chromatography
  • acetic anhydride is removed in the 100 gallon reactor at 122 °F and less than about 10 mm Hg vacuum. After the acetic anhydride is removed vacuum is broken with nitrogen.
  • a wash mixture made up of 95 lbs. of water 10 lbs. of sodium bicarbonate, and 35 lbs. of methanol is prepared. This mixture is added to the reactor, stirred for 1 hour and settled for 1 hour. The bottom layer is drained off.
  • a second wash mixture consisting of 95 lbs. water, 6 lbs. sodium bicarbonate, 4 lbs. sodium carbonate and 35 lbs. of methanol is prepared. This mixture is added to the reactor, stirred for 1 hour and settled for 1 hour. The bottom layer is drained off. The product is washed a third time with 140 lbs. of pure water. The bottom layer is drained off. The product is then fractionally distilled in the reactor at pressure less than 10 mm Hg.
  • EXAMPLE III Granulation Process 6.2 kg of NMA bleach activator made according to Example II is premixed with 4.2 kg of nonionic surfactant (Neodol 25-7 available from Shell Chemical Co.) to form the liquid activator mixture. 7.5kg of precipitated silica carrier particles commercially available from Huber Corporation under the trade name Zeothix 265 is charged to a Eirich R08 mixer. The Eirich mixer is operated at low speed (Pan - 28 rpm, Rotor - 600 RPM) for about 1 minute while the liquid activator mixture is added, after which the mixing is allowed to continue until a powdered activator is formed. A binder, which includes 1.9 kg of polyethylene glycol (M.W.
  • Polyethylene glycol (MW 4000) 8.2%
  • NMA bleach activator made according to Example II is premixed with 4.2 kg of nonionic surfactant (Neodol 25-7 available from Shell Chemical Co.) to form a liquid activator mixture.
  • 7.5 kg of precipitated silica commercially available from Huber Corporation under the trade name eothix 265 is charged to an Eirich mixer commercially available from Eirich Machines Inc. and sold under the trade name Eirich R08.
  • the Eirich mixer is operated at low speed (Pan - 28 rpm, Rotor - 600 RPM) for about 1 minute while the liquid activator mixture is added, after which the mixing is allowed to continue until a powdered activator is formed.
  • a binder which includes 1.9 kg of polyethylene glycol (M.W.
  • the bleach additive granules formed have the following formula: Bleach Additive Component % Weight
  • Polyethylene glycol (MW 4000) 8.2%
  • the above exemplified particulate bleach additive composition unexpectedly has superior bleach boosting performance as well as physical properties alone and when incorporated into fully formulated detergent compositions.
  • Bleaching compositions having the form of granular laundry detergents are exemplified by the following formulations. COMPONENT A B C D
  • Trisodium citrate 5.0 5.0 2.0 3.0 3.0
  • the above exemplified granular detergent compositions unexpectedly have superior cleaning performance as well as physical properties.

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Abstract

La présente invention concerne une composition particulaire d'additif de blanchiment à utiliser dans des produits détergents granulaires. La composition particulaire d'additif comprend (a) environ 1 % à 90 % en poids de particules supports; (b) environ 1 % à 70 % en poids d'un composé liquide activateur de blanchiment de formule (I) dans laquelle R1 représente un groupe alkyle saturé ou insaturé à chaîne linéaire ou ramifiée en C7-C13, R2 représente un groupe alkyle saturé ou insaturé à chaîne linéaire ou ramifiée en C1-C8 et R3 représente un groupe alkyle saturé ou insaturé à chaîne linéaire ou ramifiée en C1-C8 et R3 représente un groupe alkyle saturé ou insaturé à chaîne linéaire ou ramifiée en C1-C4; et (c) environ 1 % à 75 % d'un liant liquide. L'activateur de blanchiment et l'activateur liquide sont enrobés à l'intérieur des particules support et sur celles-ci.
PCT/US1998/002528 1997-02-10 1998-02-09 Composition particulaire d'additif de blanchiment a utiliser dans des compositions de detergent granulaires WO1998035010A1 (fr)

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US60/036,931 1997-02-10

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000050556A1 (fr) * 1999-02-25 2000-08-31 Henkel Kommanditgesellschaft Auf Aktien Procede de production d'une preparation a base de derives d'acetonitrile
WO2005107815A2 (fr) * 2004-05-03 2005-11-17 Nektar Therapeutics Al, Corporation Dérivés de polymères comprenant un point de ramification de type imide
WO2009065770A1 (fr) * 2007-11-21 2009-05-28 Henkel Ag & Co. Kgaa Granulat d'un ingrédient sensible d'un agent de lavage ou de nettoyage

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0098021A2 (fr) * 1982-06-30 1984-01-11 The Procter & Gamble Company Compositions pour le blanchiment
EP0106634A1 (fr) * 1982-10-08 1984-04-25 THE PROCTER & GAMBLE COMPANY Masses contenant des activateurs de blanchiment
EP0163331A1 (fr) * 1984-05-02 1985-12-04 THE PROCTER & GAMBLE COMPANY Composition granulaires détergent-agent de blanchiment
EP0195663A2 (fr) * 1985-03-20 1986-09-24 The Procter & Gamble Company Compositions pour le blanchiment

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0098021A2 (fr) * 1982-06-30 1984-01-11 The Procter & Gamble Company Compositions pour le blanchiment
EP0106634A1 (fr) * 1982-10-08 1984-04-25 THE PROCTER & GAMBLE COMPANY Masses contenant des activateurs de blanchiment
EP0163331A1 (fr) * 1984-05-02 1985-12-04 THE PROCTER & GAMBLE COMPANY Composition granulaires détergent-agent de blanchiment
EP0195663A2 (fr) * 1985-03-20 1986-09-24 The Procter & Gamble Company Compositions pour le blanchiment

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000050556A1 (fr) * 1999-02-25 2000-08-31 Henkel Kommanditgesellschaft Auf Aktien Procede de production d'une preparation a base de derives d'acetonitrile
WO2005107815A2 (fr) * 2004-05-03 2005-11-17 Nektar Therapeutics Al, Corporation Dérivés de polymères comprenant un point de ramification de type imide
WO2005107815A3 (fr) * 2004-05-03 2007-08-23 Nektar Therapeutics Al Corp Dérivés de polymères comprenant un point de ramification de type imide
US9085659B2 (en) 2004-05-03 2015-07-21 Nektar Therapeutics Polymer derivatives comprising an imide branching point
WO2009065770A1 (fr) * 2007-11-21 2009-05-28 Henkel Ag & Co. Kgaa Granulat d'un ingrédient sensible d'un agent de lavage ou de nettoyage

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