Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/66—Non-ionic compounds
  • C11D1/825—Mixtures of compounds all of which are non-ionic
• • 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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0004—Non aqueous liquid compositions comprising insoluble particles
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
  • C11D17/041—Compositions releasably affixed on a substrate or incorporated into a dispensing means
  • C11D17/042—Water soluble or water disintegrable containers or substrates containing cleaning compositions or additives for cleaning compositions
  • C11D17/043—Liquid or thixotropic (gel) 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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
  • C11D17/041—Compositions releasably affixed on a substrate or incorporated into a dispensing means
  • C11D17/042—Water soluble or water disintegrable containers or substrates containing cleaning compositions or additives for cleaning compositions
  • C11D17/044—Solid compositions

Definitions

• the within disclosed invention relates to detergent mull compositions and delivery means therefor.
• nonionic surfactants are useful in formulating laundry detergents for use in low water temperature washes. It is further known that nonionic surfactants are particularly efficient at removing oily soils from synthetic fabrics but that they are not as efficient at removing particulate soils as anionic surfactants. As a result it is desirable to include detergent builders in detergent formulations containing nonionic surfactants to improve performance on particulate soils and provide good overall cleaning performance. However, the amount of nonionic surfactant that can be included in powder detergents is limited by the amount that can be absorbed into or adsorbed onto the solid components.
• Agglomeration techniques usually produce dense particles that have little capacity for absorbing nonionic surfactants and the final compositions usually have poor solubility rates and flowability.
• Spray-drying techniques produce more porous particles that can sorb more nonionic surfactant.
• the temperatures involved in spray-drying can cause oxidation of the nonionic surfactant and it is desirable to add the nonionic surfactant in a second step if a high concentration is desired. Since the spray-drying process is energy and capital intensive, this approach results in high manufacturing costs.
• the spray-drying process itself can lead to the formation of insoluble particles that deposit on clothes during the washing process.
• pouches constructed of water soluble films to deliver unit dosages of laundry additives is well documented.
• US-A-4115292 issued to Richardson et al, shows compositions with low amounts of very high pour point nonionic surfactants and relatively high amounts of water in water-soluble polyvinyl alcohol pouches.
• This invention seeks to provide detergent mull compositions containing high amounts of nonionic surfactants which are not produced by such energy consumptive processes.
• This invention seeks to provide detergent compositions in the form of mulls which have excellent solubility or dispersability in cool and cold water and which efficiently remove both particulate and oily soils.
• This invention can provide detergent compositions in the form of mulls which have excellent rates of dispersion/dissolution in cool and cold water and which have good phase stability without the addition of clays or other costly phase-stabilizing ingredients and without the requirement of an extremely small average particle size for the solid components of the mulls.
• this invention seeks to provide a method for conveniently packing, storing and delivering these detergent compositions to washing machines.
• a detergent mull composition comprising:
• novel detergent mull compositions are rapidly soluble/dispersible in cold water and yet surprisingly provide good removal of oily and particulate soils from both natural and synthetic fibres, even though the HLB values of the surfactant systems of these compositions may be lower than is considered optimum for good detergency.
• a low-temperature-effective-detergent mull composition comprising:
• the viscosity range of 10,000-100,000 centipoise (mPa - s) specified above is measured at 25°C and at 6.25 revolutions per minute as measured on a Haake Rotoviscometer with an MVII sensor.
• compositions of this embodiment have an average viscosity of 20,000-60,000 mPa - s, and most preferably 30,000-50,000 mPa - s under the same rheological test conditions.
• the pour point of the mull compositions according to the invention is preferably less than 19°C (65°F) and most preferably less than 5°C (40°F); when water is present in the detergent mull compositions according to the invention in an amount of 0.1 to 5.0% by weight of the composition (unless otherwise specified, all further measures herein are by percent by weight of the composition) phase separation tends to be eliminated. This eliminates the need for the addition of more expensive materials, such as clays, and reduces the phase separation without significantly reducing the cold water solubility of the composition.
• the invention provides a premeasured, low-temperature-effective delivery system comprising:
• any of the inventive detergent mull compositions or into the low temperature effective detergent delivery system described above there may be added further surfactant which do not render detergent solubility/dispersibility unacceptable, fluorescent whitening agents, bleaches, corrosion inhibiting agents (i.e. anti-corrosion agents), anti-redeposition agents, enzymes, dyes, pigments, fabric softeners, fragrances and other adjuncts.
• the invention further provides a method of laundering fabrics by contacting the fabrics with the foregoing detergent mull compositions or with water into which the compositions has been dissolved or dispersed, or by contacting the fabric with water to which the low temperature delivery system has been added.
• HLB hydrophile-lipophile balance
• a further potential problem with mulls containing surfactants with low pour points is that the surfactants are too fluid at room temperature, and as a result, have more tendency to separate from the solids in the mulls. This leads to phase separation upon storage of the detergent composition. It has been surprisingly found that the addition of very small amounts of water to the surfactant system will essentially eliminate phase separation in the final detergent mull composition. Water added in the range of 0.1 to 5.0%, based on the weight of the composition, will adequately control phase separation without significantly reducing detergent solubility or dispersibility. Although not wishing to be bound to any one particular theory, applicants speculate that this effect results from flocculation of the solids in the mull which further increases their capacity to adsorb and absorb the surfactant.
• the amounts of builders and surfactants that can be included in the formulations disclosed herein can vary considerably depending on the nature of the builders, the final desired viscosity and the amount of water added to the surfactant system.
• other additives commonly found in detergent compositions can also be included in the formulations described herein. These include but are not limited to further surfactants which do not render detergent dissolution/dispersion rates unacceptable, fluorescent whitening agents, bleaches, corrosion-inhibiting agents, anti-redeposition agents, enzymes, fabric softeners, perfumes, dyes and pigments.
• the amount of builder should desirably be in the range of 30 to 90% by weight of the total composition, with the surfactant system comprising 10 to 70% by weight of the composition and the additional optional ingredients comprising 0 to 60% by weight of the composition.
• the ratio of these ingredients should be further adjusted along with the level of water, which increases the viscosity when added to the formulation, to provide a mull composition with a viscosity preferably in the range of 10,000 to 100,000 centipoise (mPa s) at 25°C and 6.25 revolutions per minute as measured on a Haake Rotoviscometer with an MVII sensor, and more preferably in the range of 20,000 to 60,000 mPa - s and still more preferably in the range of 30,000 to 50,000 mPa - s.
• mPa s centipoise
• the invention disclosed herein provides for mull detergent compositions that can be manufactured economically, will dissolve or disperse at acceptable rates in cool and cold water, have good overall cleaning performance and have controllable phase separation.
• Suitable, and preferred, materials for the individual constituents of the novel compositions of this invention are described as follows:
• the surfactants of choice in the nonionic surfactant system have been selected from the nonionic surfactants including linear and branched, primary and secondary ethoxylated alcohols with an average chain length of 6 to 16 carbon atoms and averaging 2 to 10 moles of ethylene oxide per mole of alcohol; linear and branched, primary and secondary ethoxylated, propoxylated alcohols with an average chain length of 6 to 16 carbon atoms and averaging 0 to 10 moles of ethylene oxide and 1 to 10 moles of propylene oxide per mole of alcohol; linear and branched alkylphenoxy (polyethoxy) alcohols, otherwise known as ethoxylated alkyl phenols, with an average chain length of 8 to 16 carbon atoms and averaging 1.5 to 30 moles of ethylene oxide per mole of alcohol; and mixtures thereof.
• nonionic surfactants are those containing 6 to 10 moles of ethylene oxide per mole of alcohol. While the invention encompasses branched chain nonionic surfactants, it is well known that for commercial purposes linear nonionics are preferred due to their better biodegradability. Exemplary of such surfactants are the Neodol O (trade name of Shell Chemical Company) ethoxylate series.
• preferred surfactants include alcohol ethoxylates such as Neodol 91-6, which is a linear ethoxylated alchol with a predominant chain length of 9 to 11 carbons and average 6 moles of ethylene oxide per mole of alcohol, with a pour point of 7°C (45°F); Neodol 91-8, having the same predominant carbon chain length as Neodol 91-6 averaging 8.4 moles of ethylene oxide per mole of alcohol, with a pour point of 15.5°C (60°F); Neodol 23-6.5, which is a linear ethoxylated alcohol with a predominant chain length of 12 to 13 carbons averaging 6.5 moles of ethylene oxide per mole of alcohol with a pour point of 15.5°C (60°F); Neodol 25-7, which is a linear ethoxylated alcohol with a predominant chain length of 12 to 15 carbons averaging 7.2 moles of ethylene oxide per mole of alcohol, with a pour point of 21°C (70°)
• Neodol ethoxylate series containing 1-5 moles of ethylene oxide per mole of alcohol.
• exemplary of these particular surfactants are Neodol 91-2.5, which is a linear ethoxylated alcohol with a predominant chain length of 9 to 11 carbons, averaging 2.5 moles of ethylene oxide per mole of alcohol, with a pour point of -15°C (5°F), and an HLB value of 8.1; and Neodol 25-3, which is a linear ethoxylated alcohol with a predominant chain length of 12 to 15 carbons, averaging 3 moles of ethylene oxide per mole of alcohol, with a pour point of 4.5°C (40°F), and an HLB value of 7.9.
• Surfonic @ JL-80X is an ethoxylated, propoxylated alcohol with an average chain length of 10 carbon atoms and averaging 9 moles of ethylene oxide and 1.5 moles of propylene oxide per mole of alcohol, with a pour point of -9.5C (15°F), and an HLB value of 13, available from Texaco Chemical Company.
• Suitable alkylphenoxy (polyethoxy) alcohols include nonyl- and octylphenoxypoly (ethyleneoxy) alcohols, such as the Igepal series manufactured by GAF Corporation, e.g., lgepal o CO-210, a nonylphenol average 1.5 moles of ethylene oxide per mole of alcohol, and the Triton@ series, manufactured by Rohm and Haas Company, e.g. Triton N-57, an ethoxylated nonylphenol averaging 5 moles of ethylene oxide per mole of alcohol.
• nonyl- and octylphenoxypoly (ethyleneoxy) alcohols such as the Igepal series manufactured by GAF Corporation, e.g., lgepal o CO-210, a nonylphenol average 1.5 moles of ethylene oxide per mole of alcohol, and the Triton@ series, manufactured by Rohm and Haas Company, e.g. Triton N-57, an ethoxylated
• the mulls of this invention have nonionic surfactant systems with pour points below 24°C (75°F), more preferably below 19°C (65°F), and most preferably below 5°C (40°F).
• Combinations of these surfactants may be used in the detergent mulls of this invention.
• Preferred combinations include those which combine a surfactant with a pour point of at least 15.5°C (60°F) with a surfactant with a much lower pour point such that the pour point of the combination is less than 24°C (75°F), more preferably less than 19°C (65°F), and most preferably less than 5°C (40°F).
• the pour point of combinations of these surfactants is usually between the pour points of each individual surfactant, but is not necessarily a weighted average of the pour points of each individual surfactant.
• the predominant criterion for choosing the surfactants with particular pour points is the temperature of the cold water wash into which the mulls of this invention will be placed.
• Cold water wash temperatures in the United States vary greatly depending on both location and time of the year. As mentioned above, the average cold water wash has been determined to be 18-19°C (65°F). However, the cold water wash temperatures can actually range from 32°C (90°F) to 4-5°C (40°F).
• the mulls of this invention are intended to be soluble in such wash temperatures.
• the pour points of the nonionic surfactant systems within the mulls should be at least lower, more preferably 2.7 Celsius degrees (5 Fahrenheit degrees) lower, most preferably 5.5 Celsius degrees (10 Fahrenheit degrees) lower than the temperature of the wash water into which they are placed.
• Suitable builders can be selected in this invention from the inorganic builders such as polyphosphates, orthophosphates, metaphosphates, tetraphosphates, tripolyphosphates, phosphates, pyrophosphates, carbonates, bicarbonates, borates, metasilicates, silicates, polysilicates, aluminosilicates (zeolites) and the alkali metal and ammonium salts of any of the foregoing.
• the inorganic builders such as polyphosphates, orthophosphates, metaphosphates, tetraphosphates, tripolyphosphates, phosphates, pyrophosphates, carbonates, bicarbonates, borates, metasilicates, silicates, polysilicates, aluminosilicates (zeolites) and the alkali metal and ammonium salts of any of the foregoing.
• Further builders can be selected from such organic builders as nitrilotriacetic acid (NTA) polycarboxylates, polyhydroxysulfonates, citrates, succinates, oxydisuccinates, polyacrylic acid, ethylenediaminetetraacetic acid (EDTA) and the alkali metal and ammonium salts of the foregoing. Mixtures of any of the builders can be used. Two particularly preferred builders are sodium carbonate and sodium tripolyphosphate. An additional preferred builder is sodium polysilicate manufactured by PQ Corporation of Valley Forge, Pennsylvania, under the trademark Britesil @.
• the combination of at least one bulider and the nonionic surfactant system should be readily soluble and/or dispersible in the wash water to which it is added.
• the concept of dispersibility includes solubility.
• satisfactory dispersibility is obtained when an observer is unable to visually discern any localised blue residue on fabrics washed with a mull composition containing a blue dye or pigment, or in the washing machine in which these fabrics were washed.
• an additional concept which is relevant to the invention is rate of dissolution/dispersion. Over time, many solid particulates will disperse in water. However, to be acceptable for use in this invention, the mulls should dissolve/disperse in the water at 18-19°C (65°F) within at least 25 minutes with gentle agitation, more preferably within 15 minutes, and most preferably within 10 minutes.
• the particle size of the builders is not critical if the viscosity of the composition is adjusted to be in the range of 10,000 to 100,000 mPa - s.
• the builder used in this composition can thus be generally used as received from the supplier without an extra processing step to mill the particles to a desired size as required in US-A--4316812.
• the average particle size of the solid components of the mull compositions of this invention is preferably between 10 to 500 ⁇ m, more preferably 50 to 250 ⁇ m, and most preferably 50 to 175 pm.
• the average particle size of one of the preferred builders, sodium tripolyphosphate (STPP)-which, in the Examples following, constitutes a major portion of the solids in the mull compositions- was determined by screening and is set forth in Table I:
• the viscosity should be in the range of 10,000 to 100,000 centipoise (mPa - s) at 25°C and at 6.25 revolutions per minute (rpm) as measured with a Haake Rotoviscometer with an MVII sensor, more preferably 20,000 to 60,000 mPa - s.
• the inventive mull compositions comprise preferably 30 to 90% by weight of at least one builder, 10 to 70% by weight surfactant system, and 0 to 60% by weight adjuncts (as described below); more preferably 40 to 80% by weight of at least one builder, 20 to 60% by weight surfactant system, and 0 to 40% by weight adjuncts; and most preferably 50 to 75% by weight of at least one builder, 25 to 50% by weight surfactant system, and 0 to 25% by weight adjuncts.
• Water has been used in Examples 12-14 below as a phase stabiliser and for viscosity control. In fact, in these particular uses, a clay or other thickener is not utilized. While it is not entirely understood why water may act as a thickener in this invention, it is believed that it may cause flocculation of the solids in the compositions of this invention which leads to further adsorption or absorption of the surfactants.
• the amount of water required to produce the desired viscosity and adequate phase stability appears to show a critical range. This amount ranges from 0.1% to 5%, more preferably 0.4% to 2% by weight of the composition.
• deionized water is especially preferred for use, although from a commercial standpoint, tap water appears acceptable.
• fluorescent whitening agents or brighteners are preferably added to improve whitening of fabrics.
• fluorescent brighteners can be selected from stilbene brighteners, and their derivatives; styrylnaphthalene brighteners and their derivatives; and styrene brighteners and their derivatives.
• Exemplary of the derivatives used is the preferred brightener Tinopal° 5BM-XC, produced by Ciba-Geigy A.G., Switzerland.
• Other brigheners include those disclosed in UK patents 1298577, 2076011, 2026054, 2026566, 1393042; and US patents 3951960, 4298290, 3993659, 3980713 and 3627758.
• nonionic, anionic, cationic and amphoteric surfactants may be combined with the detergent mulls of this invention in a manner to impart greater cleaning where desired, with the proviso that such added surfactants do not render detergent solubility or dispersibility unacceptable, especially in cool or cold water up to 24°C (75°F).
• anionic surfactants may be added to increase cleaning of particulate soils.
• anionic surfactants include the ammonium, substituted ammonium (e.g., mono- di- and triethanolammonium), alkali metal, and alkaline earth metal salts of C a -C 2o fatty acids and rosin acids, linear and branched alkylbenzenesulfonates, alkyl sulfates, alkyl ether sulfates, alkanesulfonates, olefin sulfonates, hydroxyalkanesulfonates, fatty acid monoglyceride sulfates, alkyl glyceryl ether sulfates, acyl sarcosinates, and acyl N-methyl taurides.
• nonionic surfactants include polyoxyethylene carboxylic acid esters, fatty acid glycerol esters, fatty acid and ethoxylated fatty acid alkanolamides, certain block copolymers of propylene oxide and ethylene oxide, and block polymers of propylene oxide and ethylene oxide with propoxylated ethylenediamine. Also included are such semi-polar nonionic surfactants like amine oxides, phosphine oxides, sulfoxides, and their ethoxylated derivatives.
• Suitable cationic surfactants include the quaternary ammonium compounds in which typically one of the groups linked to the nitrogen atom is a C 12 ⁇ C 18 alkyl group and the other three groups are short-chain alkyl groups which may bear inert substituents such as phenyl groups.
• suitable amphoteric and zwitterionic surfactants which contain an anionic water-solubilizing group, a cationic group, and a hydrophobic organic group include aminocarboxylic acids and their salts, iminodicarboxylic acids and their salts, alkylbetaines, alkylamidopropylbetaines, sulfobetaines, alkylimidazolinium derivatives, certain quaternary ammonium compounds, certain quaternary phosphonium compounds and certain tertiary sulfonium compounds.
• suitable zwitterionic surfactants can be found described in US-A-4005029, issued to Jones, at Columns 11-15.
• anionic, nonionc, cationic and amphoteric surfactants which may be suitable for use in this invention are depicted in Kirk-Othmer, Encyclopedia of Chemical Technology, Third Edition, Vol. 22, pages 347-387, and McCutcheon's Detergents and Emulsifiers, North American Edition, 1983.
• Further cleaning adjuncts can include enzymes. Particularly preferred are amylases and proteases. Particularly preferred are proteases such as alkaline proteases, also denoted as subtilisins. Suitable examples include Savinase @ , Alcalase@, and Esperase @ , all from Novo Industri A/S, Denmark, and Maxacal ® and Maxatase @ from Gist Brocades, N.V., Netherlands.
• Bleaches can also be added to the compositions of this invention, preferably peroxygen bleaches such as percarbonate, perborate, and the salts thereof, e.g. sodium perborate monohydrate, and organic and inorganic peroxy compounds, such as peracids, e.g. perlauric acid, and potassium peroxymonosulfate (available from E.I. du Pont de Nemours, Delaware, under the trade mark Oxone @ ).
• bleach activators can be incorporated, such as tetraacetylethylenediamine (TAED), ketones or aldehydes.
• a delivery system comprising (a) a water-soluble delivery pouch, which comprises a film prepared from at least one film-forming polymer and (b) an effective amount of a low temperature detergent mull as described hereinbefore, which comprises a nonionic surfactant system and a builder.
• Particularly preferred films are castable, water-soluble films comprised of polyvinyl alcohols which have number average molecular weights from 5,000 to 250,000.
• the polyvinyl alcohols generally have 1 to 25% residual acetate groups, more preferably 5 to 20% residual acetate groups, and most preferably 10 to 15% residual acetate groups.
• polymers as polyvinyl pyrrolidone, methyl cellulose, polyethylene oxide, gelatin and other film formers can be utilized.
• Plasticizers such as trimethylolpropane, glycerol, polyethylene glycol and others known to those skilled in the art can be included in the film to provide the film strength and flexibility required for producing, filling, shipping and storing the pouches prepared from these films.
• other ingredients such as wetting agents, defoamers, and anti-blocking agents can be included in these films to aid in their manufacture and in the preparation of pouches made from these films.
• the films employed can have a thickness of from 25 to 127 pm with the thickness and film material being selected to provide the optimum balance of film strength and cold water solubility. It has been found that films with a thickness of 38 to 89 um produced from polyvinyl alcohol with about 12% residual acetate groups are preferred.
• a further embodiment of this invention comprises a delivery system comprising (a) a water-soluble delivery pouch, and (b) an effective amount of a low-temperature-effective detergent mull as described hereinbefore, which comprises a builder and a nonionic surfactant system and additionally 30% or less, based on the weight of the surfactant system, of at least one ingredient that is suitable for use as a film plasticizer for the film used to form the water-soluble pouch.
• a delivery system comprising (a) a water-soluble delivery pouch, and (b) an effective amount of a low-temperature-effective detergent mull as described hereinbefore, which comprises a builder and a nonionic surfactant system and additionally 30% or less, based on the weight of the surfactant system, of at least one ingredient that is suitable for use as a film plasticizer for the film used to form the water-soluble pouch.
• each of the 10 exemplified compositions in Table II were prepared by premixing the nonionic surfactants together and then mixing the surfactant system together with the remainder of the ingredients in a Hobart mixer. Relatively low shear mixing was used and a total mixing time of 15-30 minutes was sufficient to provide uniform distribution of the ingredients in the resulting mulls. The pour point of each surfactant mixture was measured using the basic procedure found in ASTM D97-66.
• the resulting pouches were then placed at 4.5°C (40°F) for 24-48 hours (to simulate storage by the consumer, such as in a garage), removed and their solubility in 4.5°C (40°F) water was evaluated.
• This procedure involved placing the pouches in a washing machine containing 68 litres of water at 4.5°C (40°F) and initiating a wash cycle using the "delicate" setting to control agitation. After ten minutes, the agitation was terminated, and the machine was drained and inspected for residual detergent. Residual detergent is determined by whether any residue remains which is visually discernible in the washing machine. This is a measure of the dissolution/dispersion rates of the mull compositions. The results are shown in Table II below.
• Example 1 which contains two surfactants, Neodol 23-6.5 and Neodol 25-9, which are considered to be water soluble by their manufacturer, failed to completely dissolve at 4.5°C (40°F) under the test conditions. In addition when this composition was stored at 21°C (70°F) and added to wash water at 17°C (63°F), it again failed to completely dissolve under the test conditions described previously.
• Example 4 by comparison, which contains Neodol 91-2.5, dissolved/ dispersed completely in the cold, i.e. 4.5°C (40°F) water even after storage at 4.5° (40°F).
• compositions of this invention provide good cleaning as well as good solubility/dispersibility characteristics.
• the cleaning performance was evaluated by washing swatches treated with these soils in water at 38°C (100°F) containing 100 ppm water hardness (as CaC0 3 ) with a molar ratio of Ca2+: Mg2+ of 3:1 and a concentration of 0.08% of the appropriate detergent mull composition in a commercial washing machine.
• the reflectance values of the swatches were measured before and after washing, and the Kubelka-Munk equation was used to calculate % soil removal.
• Example 10 is a ternary system containing mixture of three nonionic surfactants, two of which have very low pour points (Neodol 91-2.5 and Surfonic JL-80X). On two fabrics, cotton and polyester, this ternary system had significantly better particulate (clay) soil removal, than the composition of Example 1, which was unexpected based on the HLB's of the surfactant systems.
• Example 12 50 kilogram quantities of mull detergent compositions were prepared using a ribbon blender and the formulas are summarized below. In Example 12, the water was added to the surfactant system before this system was mixed with the rest of the composition.
• Example 11 The composition of Example 11 was observed to have phase separation after storage at room temperature. The separation was quantified by placing 1000 grams of the composition in a one-litre graduated cylinder for one week at room temperature and then removing and weighing the separated liquid phase that appeared on top of the remainder of the composition. It was found that weight of the liquid totaled 4.8% of the total composition. When the detergent of composition 12 was evaluated under the same conditions, 0.1% or less liquid phase separation was observed.
• Example 12 Furthermore, 2 kilogram quantities of the detergent composition of Example 12 were prepared and tested for solubility as were Examples 1-10.
• the composition of Example 12 dissolved/dispersed completely in less than ten minutes in 4.5°C (40°F) water.
• mull detergent compositions 2 kilogram quantities were prepared using a Hobart mixer and their formulas are summarized below. Approximately 25 grams of each composition were placed in a 2x3 inch (5.08x7.62 cms) water-soluble pouch constructed from a 63 pm thick film comprised predominantly of polyvinyl alcohol (number average molecular weight of about 10,000 and about 12% residual acetate groups) with 5% glycerol and 4% trimethylolpropane as plasticizers. The pouches were stored for nine weeks at 21°C/50% relative humidity (70°F/50%).

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• 1985
  • 1985-03-20 EG EG18485A patent/EG16786A/xx active
  • 1985-03-21 EP EP19850301979 patent/EP0158464B1/en not_active Expired
  • 1985-03-21 CA CA000477113A patent/CA1284602C/en not_active Expired - Lifetime
  • 1985-03-21 DE DE8585301979T patent/DE3571643D1/de not_active Expired
  • 1985-03-22 JP JP5765285A patent/JPS60212495A/ja active Pending
  • 1985-03-22 TR TR1397685A patent/TR22756A/tr unknown
  • 1985-03-22 AR AR29983985A patent/AR241466A1/es active
  • 1985-03-22 BR BR8501303A patent/BR8501303A/pt not_active IP Right Cessation
  • 1985-03-22 ES ES542041A patent/ES8705022A1/es not_active Expired
  • 1985-03-22 AU AU40258/85A patent/AU575383B2/en not_active Ceased
  • 1985-03-22 ES ES542042A patent/ES8801714A1/es not_active Expired
  • 1985-03-22 MX MX20470585A patent/MX164019B/es unknown
• 1987
  • 1987-01-15 ES ES557352A patent/ES8801363A1/es not_active Expired

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