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
• • 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
  • C11D10/00—Compositions of detergents, not provided for by one single preceding group
  • C11D10/04—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
  • C11D10/045—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap based on non-ionic surface-active compounds and soap
• • 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
• • 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
  • C11D1/66—Non-ionic compounds
  • C11D1/72—Ethers of polyoxyalkylene glycols

Definitions

• the present invention relates to a free-flowing granular detergent base composition of high bulk density having a surfactant system consisting essentially of fatty acid soap and nonionic surfactant, and a detergency builder system based on aluminosilicate.
• the composition of the invention which can be used alone or admixed with other detergent ingredients, combines efficient cleaning performance with a lack of environmentally questionable ingredients, has good powder properties, and dispenses surprisingly well into a drum-type automatic washing machine.
• the invention also relates to the preparation of the detergent base composition by densification of a spray-dried base powder in a high-speed mixer/granulator.
• a product having an exceptionally attractive appearance is obtained.
• EP 344 629A (Henkel), published on 6 December 1989, discloses a granular composition comprising aluminosilicate (45-75 wt%), fatty acid soap (1-6 wt%), acrylic and/or maleic polymer (1-12 wt%), optionally plus sodium sulphate and a small amount (up to 5 wt%) of nonionic surfactant.
• the granular material (65-90 wt%) may be used as a carrier for nonionic surfactant (10-35 wt%).
• EP 229 671A (Kao), JP 61 069 897A (Kao) and JP 61 064 798A (Kao) disclose the densification of spray-dried detergent powder, containing a high level of anionic non-soap surfactant and a relatively low level of aluminosilicate builder, in a high-speed mixer/granulator.
• EP 340 013A (Unilever), published on 2 November 1989, describes and claims high-bulk-density granular detergent compositions comprising moderate levels of anionic non-soap surfactant and moderate levels of aluminosilicate builder, and their preparation by densification of spray-dried base powder in a high-speed mixer/granulator.
• JP 62 086 099A discloses a granular soap-based detergent composition of high bulk density typically containing 40-55 wt% soap, 5-20 wt% nonionic surfactant (7-15 wt% exemplified) and 25-50 wt% builder.
• the powder is prepared by a non-tower process in which soap chips, nonionic surfactant and builders are disintegrated and mixed in a lateral-type mixer/granulator.
• the present invention provides a granular detergent base composition having a bulk density of at least 650 g/litre, which comprises:
• the invention also provides a process for the preparation of a detergent base composition as defined in the previous paragraph, which includes the steps of:
• the detergent base composition is a mixture of the detergent base composition
• the first subject of the present invention is a granular detergent base composition of moderate to high bulk density, having a surfactant system based on fatty acid soap and alkoxylated nonionic surfactant, and built with alkali metal aluminosilicate, at a relatively high level, and an organic sequestrant cobuilder.
• detergent base composition is intended to indicate a particulate composition that may be used as a detergent product in its own right, or alternatively may be admixed with other, separately prepared ingredients to form a more fully formulated detergent composition.
• the detergent base composition is a generally a substantially homogeneous particulate material.
• the invention is especially concerned with a spray-dried detergent base composition, which may or may not be subsequently densified.
• Compositions of the invention having bulk densities up to about 650 g/l have been successfully produced just by spray-drying, and these may be further densified by post-tower treatment in a high-speed mixer/granulator as indicated above.
• detergent base composition indicates the spray-dried primary product, plus any “base” ingredients (for example, nonionic surfactant, fatty acid soap) that for processing reasons may be withheld from the slurry and added after the tower.
• detergent base composition for preparation of the detergent base composition, it is within the scope of the invention for the liquid or liquefiable ingredients of the base composition - nonionic surfactant, and soap as fatty acid - to be incorporated by spray-on rather than via the slurry.
• detergent base composition includes those sprayed-on ingredients.
• detergent base composition indicates the spray-dried powder produced by step (1), plus any "base” ingredients introduced separately prior to or during the densification step (2).
• Postdosed ingredients that is to say, ingredients added after densification, do not form part of the detergent base composition.
• the base composition of the invention may be formulated entirely from environmentally unobjectionable ingredients while exhibiting efficient cleaning performance.
• Preferred compositions of the invention are substantially free of non-soap anionic surfactants, and yet exhibit cleaning performance comparable with that of conventional detergent powders on the market today based on sulphonate- or sulphate-type anionic surfactants.
• the base composition of the invention is also preferably free of phosphate builders. Efficient detergency building is provided by alkali metal aluminosilicate, in a relatively large amount, assisted by an organic sequestrant which is advantageously an environmentally preferred material free of nitrogen or phosphorus, in particular a non-polymeric polycarboxylate such as citrate.
• ingredients which have been the subject of possible objections on environmental grounds, and which are preferably substantially absent, are sodium sulphate, fluorescer, nitrogen- or phosphorus-containing sequestrants, and acrylic, maleic or acrylic/maleic polymers.
• the base composition of the invention is capable of providing very acceptable cleaning performance without the need for the inclusion of those ingredients.
• the composition has a bulk density of at least 650 g/litre and if desired may be compacted to bulk densities of 700 g/litre and above, and even to 750 g/litre and above, the compactness providing a further environmental benefit of reduced packaging requirements. Powder properties (flow, compressibility, resistance to caking) are good whether or not the composition is densified.
• densification does not have a detrimental effect on the ability of the composition to dispense from the drawer of a drum-type automatic washing machine.
• This behaviour is in marked contrast to that of conventional powders based on sulphonate- or sulphate type anionic surfactants; in general the dispensing of densified powders of conventional formulation is so poor that dosing via the dispenser drawer is not practicable and the manufacturer has to provide a special reusable dosing device or "shuttle". This is not universally acceptable to the consumer, and being generally of plastics material adds to the waste disposal problem.
• Densified detergent base powder of the invention produced by one specific process, described in more detail below, is also characterised by a large and uniform particle size and a regular (spherical) particle shape, giving it an especially attractive appearance, and reducing the amount of further handling (for example, sieving) required after densification.
• the base composition of the invention contains from 5 to 40 wt%, preferably from 5 to 30 wt%, more preferably from 5 to 20 wt% and desirably from 7 to 20 wt%, of fatty acid soap.
• the soap provides detergency, detergency building and foam control.
• This total will generally be a blend composed of soaps of different chain lengths, and of saturated and unsaturated soaps.
• Commercially available soaps suitable for use in the present invention include those derived from hardened or natural tallow, coconut oil, rapeseed oil, and mixtures of these. It is also possible, however, to manipulate the chain length distribution and the amount of unsaturation so as to maximise the efficiency of the final blend as surfactant and (to a lesser extent) as builder, while giving also giving optimum stability, and dissolution and dispersion properties.
• the soap may advantageously contain at least 40 wt% unsaturated soap. This is preferably in the form of oleate (singly unsaturated soap) rather than linoleate (doubly unsaturated soap) because the latter material can have a tendency to rancidity.
• a soap blend is advantageously chosen that has a Krafft point not higher than 50°C, and preferably not higher than 30°C, so that optimum dispersion of the soap throughout the wash liquor and dissolution during the wash cycle is ensured.
• GB 2 034 741B (Unilever) discloses a soap blend having a low Krafft temperature (below 25°C), derived from a C12 ⁇ 22 fatty acid mixture comprising
• One soap blend suitable for use in the base composition of the invention derived from tallow and coconut, contains 14 wt% C12 saturated soap, 40 wt% C18 saturated soap, and 46 wt% C18 unsaturated soap (oleate). This blend has a Krafft point of about 45°C and exhibits excellent dispersion, dissolution and detergency in the 60°C wash cycle.
• Another blend, especially suitable for very low temperature washing contains a higher proportion of short-chain saturated soap (39 wt%), and a lower proportion of longer-chain saturated soap (15 wt%), and has a Krafft point of about 12°C.
• the alkoxylated nonionic surfactant is the alkoxylated nonionic surfactant
• the base composition of the invention also contains from 5 to 35 wt%, preferably from 5 to 20 wt%, and more preferably from 5 to 15 wt%, of alkoxylated nonionic surfactant.
• Nonionic surfactants are well known to those skilled in the art, and include the C12 ⁇ 20 primary and secondary aliphatic alcohols ethoxylated with an average of from 3 to 20 moles of ethylene oxide per mole of alcohol. Especially preferred for use in the base composition of the invention are those with lower degrees of ethoxylation, for example, 3 to 8 moles of ethylene oxide per mole of alcohol.
• Nonionic surfactants of plant or animal origin for example, the ethoxylation products of tallow alcohol, hardened tallow alcohol, and coconut alcohol, may if desired be used in the base composition of the present invention.
• One preferred nonionic surfactant for use in the base composition of the invention is coconut alcohol ethoxylated with an average of from 3 to 8, preferably from 5 to 8, moles of ethylene oxide; optionally in combination with tallow or hardened tallow alcohol ethoxylated with an average of 6 to 10 moles of ethylene oxide.
• the principal detergency builder of the base composition of the invention is alkali metal aluminosilicate, present in a substantial amount: 20 to 60 wt%, preferably 25 to 60 wt%, more preferably from 30 to 50 wt%, calculated on an anhydrous basis.
• the alkali metal (preferably sodium) aluminosilicate builder may be crystalline or amorphous or a mixture thereof, and has the general formula 0.8-1.5 Na2O.Al2O3.0.8-6 SiO2.
• aluminosilicates contain 1.5-3.5 SiO2 units (in the formula above) and have a particle size of not more than about 100 ⁇ m, preferably not more than about 20 ⁇ m. Both amorphous and crystalline aluminosilicates can be made readily by reaction between sodium silicate and sodium aluminate, as amply described in the literature.
• Crystalline aluminosilicates are preferred for use in the present invention. Suitable materials are described, for example, in GB 1 473 201 (Henkel) and GB 1 429 143 (Procter & Gamble).
• the preferred sodium aluminosilicates of this type are the well-known commercially available zeolites A and X, and mixtures thereof.
• Especially preferred for use in the present invention is Type 4A zeolite.
• the aluminosilicate is assisted by an organic sequestrant cobuilder, preferably a material free of nitrogen or phosphorus, present in an amount of from 2 to 15 wt%, preferably from 5 to 10 wt%.
• organic sequestrant cobuilder preferably a material free of nitrogen or phosphorus
• the organic builder is preferably a water-soluble salt of a polycarboxylic acid, for example, alkali metal (preferably sodium) oxydisuccinate, tartrate monosuccinate, tartrate disuccinate, carboxymethyloxysuccinate, polyacetal carboxylate, or, most preferably, citrate.
• a polycarboxylic acid for example, alkali metal (preferably sodium) oxydisuccinate, tartrate monosuccinate, tartrate disuccinate, carboxymethyloxysuccinate, polyacetal carboxylate, or, most preferably, citrate.
• water-soluble salts of non-polymeric polycarboxylic acids are especially preferred.
• Water-soluble (preferably alkali metal) salts of citric acid for example, sodium citrate, are especially preferred.
• sodium citrate is used in an amount of from 5 to 10 wt%.
• Polymeric polycarboxylates especially acrylic, maleic and acrylic/maleic polymers, are also effective cobuilders and their use is not excluded from the scope of the invention, although the materials listed in the previous paragraph may be preferred on environmental grounds.
• sodium carbonate is advantageously present in an amount of up to 25 wt%, for example, from 2 to 25 wt%, preferably from 5 to 15 wt%. If the amount of fatty acid soap is 6 wt% or less, then the presence of 2 to 25 wt% sodium carbonate is an essential feature of the invention.
• base compositions containing more than 6 wt% of fatty acid soap to be free of sodium carbonate.
• a low level of water-soluble alkali metal silicate preferably sodium silicate not more than 5 wt% - may be included in order to provide protection against corrosion of metal washing machine parts, to increase alkalinity, and to provide powder structure.
• the amount of sodium silicate does not exceed 2 wt%.
• Powder structuring may also be assisted by the inclusion of succinic acid and/or a water-soluble (preferably alkali metal) salt thereof, more preferably sodium succinate, as described and claimed in EP 61 295B (Unilever).
• a water-soluble (preferably alkali metal) salt thereof more preferably sodium succinate, as described and claimed in EP 61 295B (Unilever).
• An amount of up to 5 wt% (calculated as succinic acid) is sufficient, and preferably the amount does not exceed 2.5 wt% calculated as succinic acid or 3.5 wt% calculated as sodium succinate.
• the base composition of the invention may also contain other conventional minor ingredients. As previously indicated, however, the base composition of the invention preferably does not contain materials which have been the subject of doubts or objections on environmental grounds.
• the base composition of the invention is suitable for use in its own right as a non-bleaching, non-enzymatic detergent composition. If desired, however, further ingredients may be admixed with the base composition to provide additional performance benefits.
• ingredients that may be admixed include peroxy bleach systems, proteolytic enzymes, lipolytic enzymes, amylolytic enzymes, fabric softening granules, and perfumes.
• a suitable peroxy bleach system consists of an inorganic persalt, for example, sodium perborate tetrahydrate, sodium perborate monohydrate or sodium percarbonate, in combination with a bleach precursor, for example, tetraacetylethylenediamine (TAED).
• TAED tetraacetylethylenediamine
• a bleach stabiliser hereinavy metal sequestrant
• the peroxy bleach system is suitably present in an amount of from 5 to 30 wt%, preferably from 5 to 15 wt%.
• Preferred fabric softening granules are those comprising clay and nonionic surfactant in a weight ratio of from 2:3 to 20:1, as described and claimed in EP 287 343A and EP 287 344A (Unilever). These are suitably present in an amount such that the amount of clay in the final composition is within the range of from 1.5 to 35 wt%, preferably from 4 to 15 wt%, the nonionic surfactant specifically associated with the clay being accounted for within the total amount of nonionic surfactant already specified.
• the detergent base composition of the invention may be prepared by any suitable process, but processes involving spray-drying are of especial interest.
• spray-drying may be employed without post-treatment.
• the preferred process for the preparation of the base composition of the invention consists of two main steps: spray-drying an aqueous slurry to produce a powder of conventional bulk density, followed by densification in a high-speed mixer/granulator.
• the soap, aluminosilicate, organic builder, and (if present) sodium carbonate, sodium silicate and sodium succinate are all suitable for incorporation into the base composition via the slurry, although it may be desirable to incorporate these materials in part at a later stage of the process, before or during densification.
• the addition of liquid or liquefiable ingredients during densification so that they can act as binders or granulating aids may be beneficial.
• Nonionic surfactant may be included in the slurry and/or added at a later stage in the process, for example, sprayed on before or during densification; generally nonionic surfactant having a relatively low degree of ethoxylation is not included in the slurry, but the incorporation of a low level of nonionic surfactant in the slurry aids processing.
• soap may if desired be incorporated wholly or in part by spray-on of the corresponding fatty acid before or during densification.
• aluminosilicate and/or sodium carbonate if present, during densification; or to postdose additional aluminosilicate, sodium carbonate or other inorganic solids after densification.
• the high-speed mixer/granulator The high-speed mixer/granulator
• Densification of the base powder is preferably effected by means of a high-speed mixer/granulator having both a stirring action and a cutting action.
• the stirrer and the cutter may be operated independently of one another, and at separately variable speeds.
• Such mixers are capable of combining a high energy stirring input with a cutting action, but can also be used to provide other, gentler stirring regimes with or without the cutter in operation. They are thus highly versatile and flexible pieces of apparatus.
• the high-speed mixer/granulator is a bowl-shaped batch mixer which more preferably has a substantially vertical stirrer axis.
• mixers of the Fukae (Trade Mark) FS-G series manufactured by Fukae Powtech Kogyo Co., Japan are essentially in the form of a bowl-shaped vessel accessible via a top port, provided near its base with a stirrer having a substantially vertical axis, and a cutter positioned on a side wall.
• the stirrer and cutter may be operated independently of one another, and at separately variable speeds.
• Another mixer found to be suitable for use in the batch process of the invention is the Lödige (Trade Mark) FM series batch mixer ex Morton Machine Co. Ltd., Scotland. This differs from the mixers mentioned above in that its stirrer has a horizontal axis.
• densification is generally effected by running the mixer at a relatively high speed using both stirrer and cutter; a relatively short residence time (for example, 5-8 minutes for a 35 kg batch) is generally sufficient.
• the final bulk density can be controlled by choice of residence time, and it has been found that the powder properties (flow, compressibility, resistance to caking) of the resulting granulate are optimum if the bulk density has been allowed to rise to at least 750 g/litre, preferably at least 800 g/litre.
• This process produces a dense, granular product of very uniform particle size and very regular, generally spherical particle shape which is exceptionally visually attractive.
• the average particle size is within the range of from 700 to 800 ⁇ m, the n -value being typically about 2.5; with only about 12 15 wt% oversize (>1000 ⁇ m) material and, more importantly, a very low level (typically only about 2-3 wt%) of "fines" (material ⁇ 180 ⁇ m).
• Particle porosity is generally less than 0.25, and preferably less than 0.20.
• the presence of a small amount of liquid binder may be required during the densification step.
• Water may be added for this purpose, or, as previously indicated, part of the nonionic surfactant and/or the soap (as fatty acid) may be withheld from the slurry and incorporated at this stage.
• the binder may be sprayed in while the mixer is running. If desired, the mixer may first be operated at a relatively slow speed while binder is added, before increasing the speed of the mixer to effect densification.
• the optimum granulation temperature in this type of process appears to be formulation-dependent.
• the densification process is suitably carried out at a controlled temperature somewhat above ambient, preferably above 30°C, more preferably from 30 to 45°C; however, with the type of formulation with which the present invention is concerned, the best results appear to be obtained when the granulation temperature does not exceed 30°C, and a temperature of about 25°C appears to be particularly favourable.
• a wider particle size distribution may be obtained, and it may be necessary to remove oversize granules and "fines" by sieving.
• the continuous mixer The continuous mixer
• densification is effected by means of a continuous high-speed mixer/granulator, preferably having a substantially horizontal stirring axis.
• the preferred mixer of this type is the Lödige (Trade Mark) CB 30 or CB 100 Recycler.
• This mixer consists essentially of a large static hollow cylinder with a central rotating shaft (stirring axis) carrying several different types of blades. It can be rotated at speeds of 100-2500 rpm, depending on the degree of densification and the particle size desired.
• the blades on the shaft provide a thorough mixing action of the solids and any liquids admixed at this stage.
• the mean residence time is somewhat dependent on the rotational speed of the shaft, the position of the blades and the weir at the exit opening, but in general a relatively short residence time of about 5 to 30 seconds is suitable.
• Alternative high-speed mixer/granulators of this general type include the Shugi (Trade Mark) Granulator and the Drais (Trade Mark) K-TPP 80 mixer.
• the particulate starting material (predensified detergent base composition) is preferably brought into, or maintained in, a deformable state. This may be induced in a number of ways, for example, by operating at a temperature of 45°C or above; however, when liquid ingredients such as water or nonionic surfactant are added to the particulate starting material, lower temperatures, for example, 35°C and above, may be employed.
• One simple method of ensuring that the particulate starting material is in a deformable state is to feed spray-dried base powder leaving the tower at a temperature of ⁇ 45°C directly into the high-speed mixer/granulator. If plant layout does not permit that, the powder may be cooled first, for example in an airlift, and then reheated after transportation to the high-speed mixer/granulator.
• the densified detergent base composition emerging from the Lödige Recycler should no longer be in a deformable state.
• the densification step is therefore preferably followed by a drying and/or cooling step. This may be carried out in any suitable manner, for example, using a fluid bed (drying) or an airlift (cooling).
• the amount of densification that can be achieved using the Lödige Recycler is generally rather less than that achievable using the batch process previously described. Bulk densities of 650-700 g/litre are however readily obtained.
• the densified composition may therefore be desirable, when operating continuously, to subject the densified composition to a further processing step: treatment in a moderate-speed mixer/granulator, suitably with a residence time of form 1 to 10 minutes, preferably from 2 to 5 minutes.
• a moderate-speed mixer/granulator suitably with a residence time of form 1 to 10 minutes, preferably from 2 to 5 minutes.
• the composition should be in a deformable state, so any drying and/or cooling should be carried out after this further step.
• This further step may be carried out in a Lödige KM 300 mixer, also known as the Lödige Ploughshare.
• This apparatus consists essentially of a hollow static cylinder having a central rotating shaft (stirring axis), on which various plough-shaped blades are mounted.
• the shaft can be rotated at speeds of from 40 to 160 rpm; optionally, one or more high-speed cutters may be used to prevent excessive agglomeration.
• Another mixer suitable for this process step is the Drais K-T 160.
• a continuous process for the production of a high bulk density detergent powder comprising the sequential use of a high-speed mixer/granulator and a moderate-speed mixer/granulator, followed by a drying and/or cooling step, is described and claimed in EP 367 339A (Unilever) published on 9 May 1990.
• small amounts of finely powdered solids for example, sodium aluminosilicate, may be added in the moderate-speed mixer/granulator and/or the high-speed mixer/granulator, as described in EP 390 251A (Unilever) published on 3 October 1990.
• the processes of the invention generally produce densified detergent base compositions having excellent flow properties.
• the dynamic flow rate typically exceeds 120 ml/s, and compressibility is less than 15% v/v.
• the batch densification process generally produces an improvement in powder properties.
• compositions of the invention in a drum-type front-loading automatic washing machine were determined by means of a standard test using a Philips (Trade Mark) AWB 126/7 washing machine using a 100 g powder dose and a water fill of 5 litres at 10°C or 20°C flowing in at a pressure of 0.5 bar, over a period of 1 minute.
• the powder remaining in the dispenser after that 1-minute period was removed, dried at 100°C for 12 hours, and weighed. This weight, in grams, represented the weight percentage of powder not dispensed into the machine (the residue). An average of at least four determinations was taken as the final result. It will be appreciated that this test is stringent, using a low water inlet temperature and flow rate, and a machine with a drawer-type dispenser that is especially vulnerable to high residues and clogging.
• a granular detergent base composition was prepared to the following formulation: % (final) % (base) Sodium soap (46 wt% unsaturated) 13.10 13.26
• Nonionic surfactant Tallow alcohol 8EO 3.75 3.80
• Zeolite 4A anhydrous basis 43.80 44.34 Sodium citrate 6.25 6.33 Sodium carbonate 6.25 6.33 Sodium succinate 2.61 2.64 Sodium silicate 0.90 0.91 Moisture 17.12 17.33 98.78 100.00
• the soap blend used was the sodium salt of a fatty acid mix composed of 14 wt% lauric acid, 40 wt% stearic acid, and 46 wt% oleic acid.
• the tallow alcohol 8EO, soap (as fatty acid), zeolite, sodium citrate, sodium carbonate, sodium succinate (as succinic acid) and sodium silicate were slurried with water and spray-dried to form a powder having a moisture content of about 18 wt%, including the water of hydration of the zeolite; this represents a free moisture content of about 7 wt%.
• the coconut alcohol 6.5EO was then sprayed on. The bulk density was about 300-550 g/litre.
• a 50 kg batch of this powder was then densified in a Fukae FS-100 high-speed mixer/granulator.
• the stirrer speed was 130 rpm
• the cutter speed was 2000 rpm
• the residence time was 10 minutes.
• the resulting densified granulate had a bulk density of about 830 g/litre. It was free-flowing and showed no tendency to cake. It was of very attractive appearance, being composed of relatively large substantially spherical granules with a very narrow particle size distribution.
• the enzyme granules were admixed with the densified granulate, and the perfume then sprayed on, to give an enzymatic detergent composition (Composition 1).
• composition A For comparison (Comparative Composition A), the same postdosed ingredients were admixed in the same proportions with an undensified sample of the base powder.
• composition B a sample of a high bulk density detergent powder commercially available in the United Kingdom and containing 9 wt% of non-soap anionic surfactants, 8 wt% nonionic surfactant, 0.5 wt% soap and 18.5 wt% zeolite, were as follows: 1 A B Bulk density (g/l) 827 550 763 Dynamic flow rate (ml/s) 142 80 63 Average particle size ( ⁇ m) 768 500 407 Particle size distribution n 2.6 1.9 1.6 Fines ( ⁇ 180 ⁇ m) 2.2 16 23 Compressibility (v/v) 12 16 13
• Dispenser residues were as follows: 1 A B Residue at 20°C (wt%) 1.1 1.2 70 Residue at 10°C (wt%) 1.2 2.4 70
• a densified base powder of the formulation given in Example 1 was prepared using a slightly different method according to which the coconut alcohol 6.5EO was sprayed into the Fukae mixer during the densification step rather than sprayed onto the powder prior to densification. A similar product, of very attractive appearance, was obtained.
• the densified base powder had the following properties: Bulk density (g/l) 810 Dynamic flow rate (ml/s) 148 Fines (wt% ⁇ 180 ⁇ m) 2.5 Compressibility (% v/v) 13 Dispenser residue (wt%) (20°C) ⁇ 1
• Base powders were prepared to the formulations shown in Table 1, and were densified, as described in Example 1, using the Fukae mixer.
• a spray-dried powder was prepared to the following formulation: parts % (base) Sodium soap (as Example 1) 13.00 13.77 Nonionic surfactant: Tallow alcohol 8EO 3.80 4.03 Zeolite 4A (anhydrous basis) 44.00 46.61 Sodium citrate 6.30 6.67 Sodium carbonate 6.30 6.67 Sodium succinate 2.61 2.76 Sodium silicate 0.90 0.95 Minor ingredients 0.50 0.53 Water 12.00 12.71 89.41 94.70
• Nonionic surfactant coconut alcohol 6.5EO 5.00 5.30 94.51 100.00
• a cooling/drying step was then carried out in a fluid bed.
• Example 8a The properties of the densified base powder leaving the Lödige Recycler (Example 8a), on leaving the fluid bed (Example 8b) and of a sample of the spray-dried powder prior to densification (Comparative Example C) were as follows: C 8a 8b Bulk density (g/l) 360 738 755 Average particle size ( ⁇ m) 460 730 740 Moisture content (wt%) 11.9 11.8 11.2
• a base powder of the formulation given in Example 1 was densified continuously using a Lödige Recycler as described previously, and the densified product emerging from the Recycler was sampled at four different times.
• This Example describes a light-duty bleaching enzymatic detergent composition in accordance with the present invention.
• the detergent base composition was that of Example 1, and was densified in the Fukae mixer as described in that Example: % (final) % (base) Sodium soap 11.98 13.26
• Nonionic surfactant Tallow alcohol 8EO 3.43 3.80
• Postdosed ingredients were added as follows: % (final) Enzyme (Maxatase) granules 0.40 Perfume 0.28 Sodium perborate monohydrate 6.00 TAED granules 3.00 100.00
• the sodium perborate monohydrate, TAED granules and enzyme granules were admixed with the densified granulate, and the perfume sprayed on, to give a high-bulk-density enzymatic bleaching detergent composition.
• Powder properties of the final product were as follows: Bulk density (g/l) 780-800 Dynamic flow rate (ml/s) 140 Compressibility (% v/v) 5 Dispenser residue (wt%) (20°C) ⁇ 1
• a composition similar to that of Example 13 but intended for heavy duty laundry use could be formulated as follows: % (final) Densified base powder of Example 1 81.12 Enzyme granules 0.60 Perfume 0.28 Sodium perborate monohydrate 13.00 TAED granules 5.00 100.00
• composition of this Example contained fabric softening granules of clay carrying adsorbed nonionic surfactant (3EO).
• Example 15 The detergency of the product of Example 15 in a 60°C machine wash on various test cloths carrying standard soils was compared with those of three products (Comparative Examples D, E and F) containing anionic non-soap surfactants.
• the formulations of the three comparative products are shown below.
• Stain removal results (percentage stain removal) in the 60°C wash were as follows: Stain 15 D E F Blackberry 5.0 4.0 2.5 1.7 Blood 3.6 4.5 2.7 1.6 Gravy 3.9 4.1 3.4 2.3
• Example 15 It is evident that the product of Example 15 generally performed at least as well as the comparative products.

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• 1989
  • 1989-10-27 GB GB898924294A patent/GB8924294D0/en active Pending
• 1990
  • 1990-10-22 CA CA002028204A patent/CA2028204A1/fr not_active Abandoned
  • 1990-10-24 EP EP19900311672 patent/EP0425277A3/en not_active Withdrawn
  • 1990-10-24 AU AU64914/90A patent/AU6491490A/en not_active Abandoned
  • 1990-10-26 KR KR1019900017179A patent/KR930005063B1/ko not_active IP Right Cessation
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  • 1990-10-26 JP JP2290587A patent/JPH0762159B2/ja not_active Expired - Lifetime

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