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
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/2075—Carboxylic acids-salts thereof
  • C11D3/2086—Hydroxy carboxylic 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/66—Non-ionic compounds
  • C11D1/72—Ethers of polyoxyalkylene glycols
• • 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
  • C11D1/66—Non-ionic compounds
  • C11D1/83—Mixtures of non-ionic with anionic 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
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
  • C11D17/065—High-density particulate detergent compositions
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—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
  • 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
  • C11D1/146—Sulfuric 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
  • 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

Definitions

• EP 544 492A discloses detergent powders of high bulk density comprising an organic surfactant system (ethoxylated nonionic surfactant plus primary alcohol sulphate), zeolite builder, and other optional ingredients.
• the ethoxylated nonionic surfactant which is the predominant component (at least 60 wt%) of the surfactant system, has a degree of ethoxylation not exceeding 6.5, preferably from 3 to 6.5 and more preferably from 4 to 5.5.
• This high-performance surfactant system gives excellent detergency, and the use of relatively high levels of zeolite allows the formulation of free-flowing powders containing high levels of these mobile surfactants.
• Citrates are well known as detergency builders used to supplement zeolites. Their use in zeolite-built powders is disclosed, for example, in EP 313 143A, EP 313 144A, EP 448 297A and EP 448 298A (Unilever); GB 1 408 678,
• EP 1310A, EP 1853B, EP 326 208A, EP 456 315A and WO 91 15566A Procter & Gamble
• DE 2 336 182C Lion
• GB 2 095 274B Coldgate
• the present invention accordingly provides a particulate detergent composition which is not the direct product of a spray-drying process, the composition having a bulk density of at least 650 g/1 and comprising:
• ethoxylated nonionic surfactant which is a primary C 8 -C 18 alcohol having an average degree of ethoxylation within the range of from 5.2 to 8.0
• nonionic surfactant which is an ethoxylated primary C 8 -C 18 alcohol having an average degree of ethoxylation within the range of from 5.2 to 8.0 to improve the delivery and dissolution characteristics of a particulate detergent composition having a bulk density of at least 650 g/1 which is not the direct process of a spray-drying process and which comprises: (a) from 15 to 50 wt% of a surfactant system consisting essentially of
• the high bulk density particulate detergent compositions of the invention contain as essential ingredients:
• compositions are preferably made by mixing and granulation processes that do not involve spray-drying.
• the invention also encompasses compositions that have been prepared by spray-drying and subsequently subjected to a granulation, densification or similar treatment that removes or reduces the porosity typical of a spray-dried powder.
• compositions of the invention are characteristically of low particle porosity.
• the particles Preferably have a void volume not exceeding 10 wt%, more preferably not exceeding 5 wt%, and desirably as low as possible. Void volume may be measured by mercury porosimetry.
• the essential ingredient of the surfactant system is an ethoxylated alcohol nonionic surfactant having an average alkyl chain length of C 8 -C 18 and an average degree of ethoxylation within the range of from 5.2 to 8.0.
• the nonionic surfactant preferably has an alkyl chain length of C 12 -C 16 , more preferably from C 12 -C 14 .
• the average degree of ethoxylation is preferably within the range of from 6 to 7.5, more preferably from 6.5 to 7.5, and most preferably is about 7.
• the desired degree of ethoxylation may be achieved, for example, by using a single commercial material having a nominal degree of ethoxylation of 7; for example coconut alcohol 7EO (eg Kolb's Inbentin* or DAC's Lorodac*), average degree of ethoxylation 6.9; or Synperonic* A7 from ICI, degree of ethoxylation 6.9 (* indicates Trade Mark).
• nonionic surfactant used in the compositions of the invention may comprise commercial nonionic surfactant having a nominal average degree of ethoxylation of 7 (55- 100 wt%, preferably 60-100 wt%), optionally in combination with commercial nonionic surfactant having a nominal average degree of ethoxylation of 3 .(0-45 wt%, preferably 0-40 wt%) .
• the ethoxylated nonionic surfactant may be the sole surfactant in the compositions of the invention.
• primary alcohol sulphate may also be present.
• the ethoxylated nonionic surfactant preferably constitutes from 30 to 90 wt% of the surfactant system, more preferably from 40 to 70 wt%; and the.
• PAS preferably constitutes from 10 to 70 wt%, more preferably from 30 to 60 wt%, of the surfactant system.
• the whole composition contains at least 5 wt% of PAS.
• the PAS suitably has a chain length in the C 8 -C 18 range, preferably C 12 -C 16 . If desired, mixtures of chain lengths may be used as described and claimed in EP 342 917A (Unilever) .
• PAS of vegetable origin and more especially PAS from coconut oil (cocoPAS)
• cocoPAS coconut oil
• the PAS is preferably present in sodium salt form.
• compositions of the invention contain no more than 5 wt% (based on the whole composition) of alkylbenzene sulphonates, and more preferably contain none.
• the detergent compositions of the invention contain an alkali metal, preferably sodium, aluminosilicate builder.
• Sodium aluminosilicates may generally be incorporated in amounts of from 10 to 70% by weight (anhydrous basis) , preferably from 25 to 50 wt%.
• the alkali metal aluminosilicate may be either crystalline or amorphous or mixtures thereof, having the general formula:
• the preferred sodium aluminosilicates contain 1.5-3.5 Si0 2 units (in the formula above). Both the amorphous and the crystalline materials can be prepared readily by reaction between sodium silicate and sodium aluminate, as amply described in the literature.
• the zeolite may be the commercially available zeolite 4A now widely used in laundry detergent powders.
• the zeolite builder incorporated in the compositions of the invention is maximum aluminium zeolite P (zeolite MAP) as described and claimed in EP 384 070A (Unilever) .
• Zeolite MAP is defined as an alkali metal aluminosilicate of the zeolite P type having a silicon to aluminium ratio not exceeding 1.33, preferably within the range of from 0.90 to 1.33, and more preferably within the range of from 0.90 to 1.20.
• zeolite MAP having a silicon to aluminium ratio not exceeding 1.07, more preferably about 1.00.
• the calcium binding capacity of zeolite MAP is generally at least 150 mg CaO per g of anhydrous material.
• compositions of the invention also contain as an essential ingredient a water-soluble salt of citric acid, preferably sodium citrate.
• the citrate salt is present in an amount of from 5 to 40 wt%, preferably from 10 to 35 wt%, more preferably from 15 to 30 wt%. Especially good results have been obtained from compositions containing from 20 to 25 wt%.
• citrate salt sodium citrate
• the percentages refer to the dihydrate.
• compositions in accordance with the invention may contain sodium carbonate, to increase detergency and to ease processing.
• Sodium carbonate may generally be present in amounts ranging from 1 to 60 wt%, preferably from 2 to 40 wt%, and most suitably from 2 to 13 wt%.
• compositions free of alkali metal carbonate are also within the scope of the invention.
• the compositions also advantageously contain fatty acid soap, as a powder structurant, suitably in an amount of from 1 to 5 wt%.
• ingredients which may be present in the base powder include fluorescer; sodium silicate; and antiredeposition agents such as cellulosic polymers, for example, sodium carboxy ethyl cellulose.
• bleach components such as sodium perborate or percarbonate, bleach activators and bleach stabilisers; sodium carbonate; proteolytic and lipolytic enzymes; dyes; foam control granules; coloured speckles; perfumes; and fabric softening compounds. This list is not intended to be exhaustive.
• compositions of the invention are of high bulk density and are preferably prepared by non-tower (non-spray-drying) processes in which solid and liquid ingredients are mixed and granulated together.
• non-tower non-spray-drying
• Such powders have relatively non-porous particles and may be especially prone to delivery, dispersion and dissolution problems in use.
• mixing and granulation are carried out in a high-speed mixer/granulator having both a stirring and a cutting action.
• the high-speed mixer/granulator also known as a high-speed mixer/densifier, may be a batch machine such as the Fukae (Trade Mark) FS, or a continuous machine such as the L ⁇ dige (Trade Mark) Recycler CB30. Suitable processes are described, for example, in EP 544 492A, EP 420 317A and EP 506 184A (Unilever) .
• the inorganic builders and other inorganic materials are granulated with the surfactants, which act as binders and granulating or agglomerating agents. Any optional ingredients as previously mentioned may be incorporated at any suitable stage in the process.
• Fatty acid soap may be prepared by in situ neutralisation with sodium hydroxide solution during the mixing and granulation process.
• any PAS present may be already neutralised, that is to say in salt form, when dosed into the high-speed mixer/granulation, or alternatively may be added in acid form and neutralised in situ.
• PAS and nonionic surfactant may be introduced in the form of a homogeneous liquid blend, as described in EP 265 203A and EP 507 402A (Unilever) .
• EP 420 317A and EP 506 184A (Unilever) disclose a different process wherein PAS acid, which is a liquid, is mixed and reacted with a solid inorganic alkaline material, such as sodium carbonate, in a continuous high-speed mixer. The resulting granule or "adjunct" is then dosed into another high-speed mixer with the nonionic surfactants and solid ingredients. All these processes are suitable for the preparation of compositions of the invention.
• bleach ingredients (bleaches, bleach precursor, bleach stabilisers), proteolytic and lipolytic enzymes, coloured speckles, perfumes and foam control granules are most suitably admixed (postdosed) to the dense homogeneous granular product - the base powder - after it has left the high ⁇ speed mixer/granulator.
• the citrate salt may suitably be among the postdosed ingredients.
• the particulate detergent compositions of the invention have bulk densities of at least 650 g/1, preferably at least 770 g/1, and more preferably at least 800 g/1.
• Test 1 cage test
• a 50 g powder sample was introduced into the cylindrical vessel which was then closed.
• the vessel was attached to the agitator arm which was then moved down to a position such that the top of the cylindrical vessel was just below the surface of the water. After a 10 second delay, the apparatus was operated for 15 rotation/rest cycles.
• the delivery device was attached in an upright position (opening uppermost) to an agitator arm positioned above water.
• the device could be moved vertically up and down through a distance of 30 cm, the lowest 5 cm of this travel being under water.
• Each up or down journey had a duration of 2 seconds, the device being allowed to rest 5 cm under water for 4 seconds at the lowest position, and at the highest position being rotated through 100° and allowed to rest in the resulting tilted orientation for 2 seconds before redescending. 5 litres of water at a temperature of 20°C were used.
• a washing machine test was also used to determine the extent that insoluble residues were deposited on washed articles.
• the machine used was a Siemens Siwamat (Trade Mark) Plus 3700 front-loading automatic washer.
• a 100 g dose of powder was placed in a flexible delivery device as described previously.
• the delivery device was placed inside a black cotton pillowcase having dimensions of 30 cm by 60 cm, taking care to keep it upright, and the pillowcase was then closed by means of a zip fastener.
• the pillowcase containing the (upright) delivery device was then placed on top of a 3.5 kg dry cotton washload in the drum of the washing machine.
• the machine was operated on the "heavy duty cycle" at a wash temperature of 40°C, using water of 15° French hardness and an inlet temperature of 20°C.
• the pillowcase was removed, opened and turned inside out, and the level of powder residues on its inside surfaces determined by visual assessment using a scoring system of 1 to 5: a score of 5 corresponds to a residue of approximately 75 wt% of the powder, while 1 indicates no residue.
• a panel of five assessors was used to judge each pillowcase and allot a score. With each powder the wash process was carried out ten times and the scores were averaged over the ten repeats.
• Comparative Example A and Example 1 contained sodium citrate; Comparative Example A contained 7EO and 3EO nonionic surfactants, while Example 1 was a similar formulation containing only 7EO nonionic surfactant to the same total level. Comparative Examples B and C were two similar compositions containing no sodium citrate.
• Nonionic 3EO 8.05 - 7.35 -
• Test 3 (score 1-5) 1.0 0.4 1.0 1.5
• composition gave zero residues when dosed via the dispenser drawer of three different automatic washing machines (Phillips, Zanussi, Siemens) .

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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)
• Health & Medical Sciences (AREA)
• Emergency Medicine (AREA)
• Inorganic Chemistry (AREA)
• Detergent Compositions (AREA)

Priority Applications (5)

Applications Claiming Priority (6)

Publications (1)

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Family Applications (1)

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Cited By (4)

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Citations (3)

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• 1994
  • 1994-04-26 ES ES94915116T patent/ES2107218T5/es not_active Expired - Lifetime
  • 1994-04-26 EP EP94915116A patent/EP0700427B2/en not_active Expired - Lifetime
  • 1994-04-26 DE DE69405735T patent/DE69405735T3/de not_active Expired - Fee Related
  • 1994-04-26 JP JP7500144A patent/JPH08511568A/ja active Pending
  • 1994-04-26 AU AU66485/94A patent/AU6648594A/en not_active Abandoned
  • 1994-04-26 HU HU9503374A patent/HUT74019A/hu unknown
  • 1994-04-26 CZ CZ953099A patent/CZ309995A3/cs unknown
  • 1994-04-26 SK SK1446-95A patent/SK144695A3/sk unknown
  • 1994-04-26 WO PCT/EP1994/001292 patent/WO1994028098A1/en not_active Application Discontinuation
  • 1994-04-26 PL PL31174994A patent/PL311749A1/xx unknown

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