WO2019213890A1 - Granulé détergent - Google Patents

Granulé détergent Download PDF

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Publication number
WO2019213890A1
WO2019213890A1 PCT/CN2018/086291 CN2018086291W WO2019213890A1 WO 2019213890 A1 WO2019213890 A1 WO 2019213890A1 CN 2018086291 W CN2018086291 W CN 2018086291W WO 2019213890 A1 WO2019213890 A1 WO 2019213890A1
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Prior art keywords
detergent granule
detergent
cleaning composition
water
present
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PCT/CN2018/086291
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English (en)
Inventor
Dan Xu
Rui Shen
Xiao Tian
Zhe Guan
Xu Huang
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The Procter & Gamble Company
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Publication date
Application filed by The Procter & Gamble Company filed Critical The Procter & Gamble Company
Priority to EP18917802.3A priority Critical patent/EP3790950B1/fr
Priority to PCT/CN2018/086291 priority patent/WO2019213890A1/fr
Priority to CN201880092648.2A priority patent/CN112041417B/zh
Priority to MX2020011976A priority patent/MX2020011976A/es
Publication of WO2019213890A1 publication Critical patent/WO2019213890A1/fr

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    • 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
    • C11D3/04—Water-soluble compounds
    • C11D3/10—Carbonates ; Bicarbonates
    • 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
    • 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
    • C11D3/04—Water-soluble compounds
    • C11D3/046—Salts
    • 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
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates
    • 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
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/12—Soft surfaces, e.g. textile

Definitions

  • the present invention relates to a detergent granule that can be used to make cleaning products, especially granular detergent products.
  • Mid-cut alkyl sulfate (MCAS or AS) with a C 6 -C 16 branched or unbranched unalkoxylated alkyl group has been discovered effective for suds-boosting when it is used as a co-surfactant with linear alkylbenzene sulphonate (LAS) in cleaning compositions, particularly laundry detergent compositions.
  • MCAS Mid-cut alkyl sulfate
  • LAS linear alkylbenzene sulphonate
  • WO2009010911 discloses the use of MCAS for boosting suds in a LAS-based surfactant system and forming a detergent composition with a reduced total surfactant level, but without apparently deteriorating the sudsing profile of the detergent composition.
  • MCAS raw materials are available in elongated needle form, which are formed by an extrusion process.
  • This extruded needle form of MCAS material is easy to process, with little or no risk of caking, clumping or clogging up the processing lines.
  • the extruded MCAS needles have limited suds-boosting effect when used in combination with LAS in cleaning compositions, probably due to its relatively large size and corresponding poor dissolution profile.
  • the MCAS raw materials are available in fine powder form with a medium particle size ranging from 200 ⁇ m to 1000 ⁇ m, which has exhibited good suds-boosting effect when used as a co-surfactant for LAS.
  • fine MCAS powder is prone to caking to clumping at a temperature higher than 35-37°C due to MCAS surfactant phase change as well as its tendency to absorb ambient water when placed in humid environment, and may cause significant processing challenges during shipping and manufacturing.
  • MCAS particles with physical characteristics and chemical compositions that can strike an improved balance between good dissolution profile and satisfactory suds-boosting effect on one hand, and reduced risk of caking and clumping and easy of processing/handling on the other hand.
  • the present invention has discovered, surprisingly and unexpectedly, that by making a detergent granule of a relatively small particle size and a relatively low aspect ratio (i.e., its shape is closer to sphere rather than needle) , the dissolution profile of such detergent granule can be improved, and the suds-boosting effect is enhanced correspondingly. Further, when such detergent granule contains MCAS at a very high level (e.g., from about 85%to about 95%by weight) in combination with a sufficient amount (e.g., from about 4%to about 14%by weight) of a water-soluble salt, it is less likely to absorb ambient water and therefore less like to cake or form clumps during shipping or storage.
  • MCAS very high level
  • a sufficient amount e.g., from about 4%to about 14%by weight
  • the present invention relates to detergent granule comprising:
  • AS alkyl sulfate
  • the detergent granule is characterized by a Medium Particle Size ranging from about 200 ⁇ m to about 1000 ⁇ m and an aspect ratio of no more than about 2.
  • the present invention relates to a cleaning composition
  • a cleaning composition comprising from about 0.1%to about 10%, by weight of such cleaning composition, of the above-mentioned detergent granule.
  • the present invention relates to the use of the above-mentioned cleaning composition for hand-washing fabrics.
  • FIG. 1 is a graph showing the dynamic vapor absorption data of an inventive detergent granule according to an embodiment of the present invention, in comparison with that of a comparative detergent granule outside of the scope of the present invention.
  • detergent granule refers to particles containing one or more detersive actives, including but not limited to surfactants, bleaching agents, enzymes, polymers, chelants, and combinations the “reof.
  • the term “cleaning composition” includes, unless otherwise indicated, granular or powder-form all-purpose or “heavy-duty” washing agents, especially cleaning detergents, for fabrics, as well as cleaning auxiliaries such as bleach, rinse aids, additives, or pre-treat types; hand dishwashing agents or light duty dishwashing agents, especially those of the high-foaming type; machine dishwashing agents; mouthwashes, denture cleaners, car or carpet shampoos, bathroom cleaners; hair shampoos and hair-rinses; shower gels and foam baths and metal cleaners; as well as cleaning auxiliaries such as bleach additives or pre-treat types.
  • the cleaning composition is a solid laundry detergent composition, and more preferably a free-flowing particulate laundry detergent composition (i.e., a granular laundry detergent product) .
  • Median Particle Size refers to the mid-point of the distribution of the particle sizes of the detergent granule, as measured by the Sieve Test as disclosed herein.
  • the term “aspect ratio” refers to the ratio of the largest diameter of an article over the smallest diameter of such article orthogonal to the largest diameter.
  • water-soluble refers to a solubility of more than about 30 grams per liter (g/L) of deionized water measured at 20°C and under the atmospheric pressure.
  • composition contains less than about 1%, preferably less than about 0.5%, of ingredients other than those listed.
  • the terms “essentially free of, ” “substantially free of” or “substantially free from” means that the indicated material is present in the amount of from 0 wt%to about 0.5 wt%, or preferably from 0 wt%to about 0.1 wt%, or more preferably from 0 wt%to about 0.01 wt%, and most preferably it is not present at analytically detectable levels.
  • substantially pure or “essentially pure” means that the indicated material is present in the amount of from about 99.5 wt%to about 100 wt%, preferably from about 99.9 wt%to about 100 wt%, and more preferably from 99.99 wt%to about 100 wt%, and most preferably all other materials are present only as impurities below analytically detectable levels.
  • the AS surfactant used in the detergent granule of the present invention contains a branched or linear unalkoxylated alkyl group containing from about 6 to about 16 carbon atoms, and is therefore also referred to as Mid-Cut AS or MCAS.
  • the AS has the generic formula of R-O-SO 3 - M + , while R is branched or linear unalkoxylated C 6 -C 16 alkyl group, and M is a cation of alkali metal, alkaline earth metal or ammonium. More preferably, the R group of the AS surfactant contains from about 8 to about 14 carbon atoms, more preferably from about 10 to about 14 carbon atoms, most preferably from about 12 to about 14 carbon atoms. R can be substituted or unsubstituted, and is preferably unsubstituted. R is substantially free of any alkoxylation. M is preferably a cationic of sodium, potassium, or magnesium, and more preferably M is a sodium cation.
  • the detergent granule of the present invention contains a mixture of C 6 -C 16 AS surfactants, in which C 8 -C 14 AS surfactants are present in an amount ranging from about 85%to about 100%by total weight of the mixture.
  • This mixture can be referred to as a “C 8 -C 14 -rich AS mixture. ” More preferably, such C 8 -C 14 -rich AS mixture contains from about 90 wt%to about 100 wt%, or from 92 wt%to about 98 wt%, or from about 94 wt%to about 96 wt%, or 100 wt% (i.e., pure) , of C 8 -C 14 AS.
  • the detergent granule contains a mixture of C 6 -C 16 AS surfactants with from about 30 wt%to about 100 wt%or from about 50 wt%to about 99 wt%, preferably from about 60 wt%to about 95 wt%, more preferably from about 65 wt%to about 90 wt%, and most preferably from about 70 wt%to about 80 wt%of C 12 AS.
  • such mixture of C 6 -C 16 AS surfactants may contain from about 10 wt%to about 100 wt%, preferably from 15 wt%to about 50 wt%, and more preferably from 20 wt%to about 30 wt%of C 14 AS. This mixture can be referred to as a “C 12 -C 14 -rich AS mixture. ”
  • the detergent granule contains a mixture of AS surfactants that consists essentially of C 12 and/or C 14 AS surfactants.
  • AS surfactants may consist essentially of from about 70 wt%to about 80 wt%of C 12 AS and from 20 wt%to about 30 wt%of C 14 AS, with little or no other AS surfactants therein.
  • Such mixture may also consist of substantially pure C 12 AS, or alternatively, substantially pure C 14 AS.
  • a commercially available AS mixture particularly suitable for practice of the present invention is V95 G from Cognis (Monheim, Germany) .
  • the detergent granule of the present invention may contain a mixture of C 6 -C 16 AS surfactants comprising more than about 50 wt%, preferably more than about 60 wt%, more preferably more than 70 wt%or 80 wt%, and most preferably more than 90 wt%or even at 100 wt% (i.e., substantially pure) , of linear AS surfactants having an even number of carbon atoms, including, for example, C 6 , C 8 , C 10 , C 12 , C 14 , and C 16 AS surfactants.
  • the mixture of C 6 -C 16 AS surfactants as described can be readily obtained by sulphonation of alcohol (s) with the corresponding numbers of carbon atoms.
  • the required carbon chain length distribution can be obtained by using alcohols with the corresponding chain length distribution prepared either synthetically or extracted/purified from natural raw materials or formed by mixing corresponding pure starting materials.
  • the mixture of C 6 -C 16 AS surfactants may be derived from naturally occurring triglycerides, such as those contained in palm kernel oil or coconut oil, by chemically processing such triglycerides to form a mixture of long chain alcohols and then sulphonating such alcohols to form AS surfactants.
  • the mixture of alcohols derived from the naturally occurring triglycerides typically contain more than about 20 wt%of C 16 -C 16 alcohols.
  • a mixture containing a lower proportion of C 16 -C 16 alcohols may be separated from the original mixture before the sulphonation step, in order to form the desired mixture of C 6 -C 16 AS surfactants as described hereinabove.
  • the desired mixture of C 6 -C 16 AS surfactants can be readily obtained by separating and purifying the already formed AS mixtures. Suitable separation and purification methods include, but are not limited to: distillation, centrifugation, recrystallization and chromatographic separation.
  • the amount of AS surfactant (s) present in the detergent granule of the present invention may range from about 85 wt%to about 95 wt%, and preferably from about 88 wt%to about 92 wt%by total weight of the composition. With such a high level of AS surfactant (s) , the detergent granule of the present invention exhibits a high detersive activity and a very good dissolution profile.
  • the cleaning composition contains from about 85 wt%to about 95 wt%, preferably from about 88 wt%to about 92 wt%, of an AS mixture consisting essentially of from about 70 wt%to about 80 wt%of C 12 AS and from 20 wt%to about 30 wt%of C 14 AS.
  • Detergent granules with higher surfactant levels are typically expected to be more difficult to handle due to their tendency to absorb more water. Therefore, it is a surprising and unexpected discovery of the present invention that the detergent granule of the present invention, while containing such a high level of AS surfactant (s) , actually absorbs less water across different relative humidity (RH) ranging from 40%to 80%, in comparison with detergent granules containing lower amounts of AS surfactants, e.g., less than about 85 wt%. Correspondingly, the detergent granule of the present invention is less likely to cake or clump and is easier to handle during storage or shipment.
  • RH relative humidity
  • the water-soluble salt used in the detergent granule of the present invention can be selected from the group consisting of sodium sulfate, sodium carbonate, magnesium chloride, magnesium sulfate, sodium silicate, and combinations thereof.
  • the water-soluble salt is selected from sodium sulfate, sodium carbonate, or a combination thereof.
  • the amount of water-soluble salt present in the detergent granule of the present invention may range from about 4 wt%to about 14 wt%, preferably from about 5 wt%to about 12 wt%, and more preferably from about 6 wt%to about 10 wt%. If the detergent granule contains less than about 4 wt%of the water-soluble salt, it exhibits poorer flowability and is therefore more difficult to handle during storage, shipping and manufacturing. If the detergent granule contains more than about 14 wt%of the water-soluble salt, the amount of AS surfactant in such detergent granule likely must be reduced to less than about 85 wt%, which is undesirable for reasons stated hereinabove.
  • the detergent granule of the present invention may contain from about 1 wt%to about 5 wt%of water, preferably from about 1.5 wt%to about 4 wt%, more preferably from about 2 wt%to about 3 wt%. Too much water in the detergent granule may adversely affect its flowability and handability.
  • the detergent granule of the present invention may contain one or more other ingredients, such as silica, zeolite, other surfactants, enzymes, bleach actives, chelants, perfumes, dyes, fluorescent materials, and the like.
  • the detergent granule of the present invention consists essentially of the above-mentioned MCAS, water-soluble salt, and water. More preferably, the detergent granule of the present invention is essentially free of other ingredients.
  • the detergent granule of the present invention may be characterized by a Medium Particle Size ranging from about 200 ⁇ m to about 1000 ⁇ m, preferably from about 250 ⁇ m to about 600 ⁇ m, more preferably from about 300 ⁇ m to about 425 ⁇ m.
  • the detergent granule of the present invention preferably has a spherical or substantially spherical shape, which functions to further improve its flowability and handability during storage and shipment.
  • the detergent granule of the present invention may be used alone for cleaning, but preferably it is combined with other particles to form a cleaning composition, such as a granular laundry detergent product.
  • the detergent granule is typically added to the cleaning composition at a level of from about 0.1 wt%to about 10 wt%, preferably from about 0.2 wt%to about 8 wt%, more preferably from about 0.5 wt%to about 5 wt%, by weight of the cleaning composition.
  • the cleaning composition is a granular detergent composition.
  • the detergent granule of the present invention may be combined with other particles such as, for example: surfactant particles, such as anionic detersive surfactant particles (especially those containing LAS) including agglomerates and extrudates, non-ionic detersive surfactant particles including agglomerates or extrudates, and cationic detersive surfactant particles including agglomerates and extrudates; enzyme particles; perfume particles including agglomerates or extrudates of perfume microcapsules, and perfume encapsulates such as starch encapsulated perfume accord particles; polymer particles including soil release polymer particles, cellulosic polymer particles; buffer particles including carbonate salt and/or silicate salt particles, preferably a particle comprising carbonate salt and silicate salt such as a sodium carbonate and sodium silicate co-particle, and particles and sodium bicarbonate; other spray-dried particles; fluorescent whitening particles; aesthetic particles such as coloured noodles or needles or lamellae particles; bleaching particles such as percarbonate particles
  • the cleaning composition of the present invention comprises, in addition to the detergent granule described hereinabove, a C 10 -C 20 linear alkylbenzene sulphonate (LAS) , and more preferably such cleaning composition further comprises a fatty acid or salt thereof.
  • LAS linear alkylbenzene sulphonate
  • the MCAS-containing detergent granule of the present invention may interact with such LAS and fatty acid/salt to provide an improved sudsing profile.
  • the cleaning composition may also be especially preferred for the cleaning composition to comprise low levels, or even be substantially free, of builder.
  • the cleaning composition comprises no builder.
  • the cleaning composition is typically used for cleaning and /or treating a situs inter alia a surface or fabric.
  • surface may include such surfaces such as dishes, glasses, and other cooking surfaces, hard surfaces, hair or skin.
  • Such method includes the steps of contacting an embodiment of the cleaning composition, in neat form or diluted in a wash liquor, with at least a portion of a surface or fabric, then optionally rinsing such surface or fabric.
  • the surface or fabric may be subjected to a washing step prior to the aforementioned rinsing step.
  • washing includes but is not limited to, scrubbing, wiping, and mechanical agitation.
  • composition solution pH is chosen to be the most complimentary to a target surface to be cleaned spanning broad range of pH, from about 5 to about 11.
  • For personal care such as skin and hair cleaning pH of such composition preferably has a pH from about 5 to about 8 for laundry cleaning compositions pH of from about 8 to about 10.
  • the compositions are preferably employed at concentrations of from about 200 ppm to about 10,000 ppm in solution.
  • the water temperatures preferably range from about 5 °C to about 100 °C.
  • a method of laundering fabrics using the cleaning composition of the present invention may comprise the steps of contacting a fabric to be laundered with the cleaning composition or a wash liquor formed thereby.
  • the fabric may comprise most any fabric capable of being laundered in normal consumer use conditions.
  • the cleaning composition herein is especially well-suited for use in a hand-washing context. It can also be used in automatic mashing washing using a top-loading or front-loading automatic washing machine.
  • the cleaning composition may be employed at concentrations of from about 500 ppm to about 15,000 ppm in solution, and optionally, more dilute wash conditions can be used.
  • 50 g or less, or 45 g or less, or 40 g or less, or 35 g or less, or 30 g or less, or 25 g or less, or 20 g or less, or even 15 g or less, or even 10 g or less of the cleaning composition is dissolved into water to form a wash liquor.
  • the wash liquor preferably has a pH of from about 8 to about 10.5.
  • the wash liquor may comprise 40 litres or less of water, or 30 litres or less, or 20 litres or less, or 10 litres or less, or 8 litres or less, or even 6 litres or less of water.
  • the wash liquor may comprise from above 0 to 15 litres, or from 2 litres, and to 12 litres, or even to 8 litres of water.
  • the wash liquor may comprise 150 litres or less of water, 100 litres or less of water, 60 litres or less of water, or 50 litres or less of water, especially for hand washing conditions, and can depend on the number of rinses.
  • the water to fabric ratio is typically from about 1: 1 to about 30: 1. Typically, from 0.01 Kg to 2 Kg of fabric per litre of wash liquor is dosed into the wash liquor.
  • the cleaning composition can be used in hard water conditions where the water hardness is between about 17 ppm to about 600 ppm; or from about 34 ppm to about 340 ppm; or from about 51 ppm to about 300 ppm of hard water ions such as Ca 2+ , Mg + , etc., or such as Ca 2+ and Mg 2+ .
  • the cleaning composition can be used in cold water temperature, where the temperature is from about 5 °C to about 40 °C, or from about 20 °C to about 30 °C, or from about 15 °C to about 25 °C, as well as all other combinations within the range of about 15 °C to about 35 °C, and all ranges within 10 °C to 40 °C.
  • This test method can be used to determine the Median Particle Size of the detergent granules of the present invention.
  • the particle size distribution of the detergent granules is measured by sieving the granules through a succession of sieves with gradually smaller dimensions. The weight of material retained on each sieve is then used to calculate a particle size distribution and Median Particle Size.
  • the prescribed Machine-Sieving Method is used with the above sieve nest.
  • the detergent granule of interest is used as the sample.
  • a suitable sieve-shaking machine can be obtained from W.S. Tyler Company of Mentor, Ohio, U.S.A.
  • the data are plotted on a semi-log plot with the micron size opening of each sieve plotted against the logarithmic abscissa and the cumulative mass percent (Q3) plotted against the linear ordinate.
  • the Median Particle Size (D 50 ) is defined as the abscissa value at the point where the cumulative mass percent is equal to 50 percent, and is calculated by a straight-line interpolation between the data points directly above (a50) and below (b50) the 50%value using the following equation:
  • Q a50 and Q b50 are the cumulative mass percentile values of the data immediately above and below the 50 th percentile, respectively; and D a50 and D b50 are the micron sieve size values corresponding to these data.
  • the 50 th percentile value falls below the finest sieve size (150 ⁇ m) or above the coarsest sieve size (2360 ⁇ m)
  • additional sieves must be added to the nest following a geometric progression of not greater than 1.5, until the median falls between two measured sieve sizes.
  • Example 1 Comparative Test Showing Reduced Water Absorption by Inventive Detergent Granule
  • Two sample detergent granules are made, which include an inventive sample of detergent granule containing about 88%MCAS (containing about 65 wt%C12 species, 25 wt%C14 species, 7 wt%C16 species, and no more than 3 wt %other species) , 9.5%sodium sulfate, and 2.5%water 90%MCAS and 10%sodium sulfate by total dry weight of such detergent granule (within the scope of the present invention) and a comparative sample of detergent granule containing 78%MCAS (same composition as above) , 19.5%sodium sulfate, and 2.5%water by total dry weight of such detergent granule (outside the scope of the present invention) .
  • inventive sample of detergent granule containing about 88%MCAS containing about 65 wt%C12 species, 25 wt%C14 species, 7 wt%C16 species, and no more than 3 wt %other species
  • Each sample detergent granule is formed by adding a specific amount of sodium sulfate into a heated concentrated MCAS paste (containing 74 wt%MCAS in water) and then mixed at an elevated temperature ranging from 60-80°C in a temperature controlled reactor for 10 minutes. The mixture is then manually spread onto a flat surface to form a thin layer having a thickness of about 3-10 mm, which is dried in an oven for about 2 hours at an elevated temperature of 110°C. Once the dried mixture reaches a target moisture content of about 2-3%, it is removed from the oven and ground into a powder form by using a Fritsch Pulverisette 14 grinder (commercially available from Fritsch GmbH, Idar-Oberstein, Germany) at a speed setting of 6 and using a 1.5mm sieve. The powders so formed are further sieved to reach the same particle size distribution as follows:
  • the moisture sorption isotherms of both the inventive detergent granule and the comparative detergent granule are acquired using a SPS-11 moisture sorption analyzer (commercially available from ProUmid GmbH &Co. KG, Ulm, Germany) .
  • the measurement is started at a relative humidity (RH) of 0%and is gradually increased in steps of about 10%RH each to a final RH of about 80%.
  • the equilibrium condition for each step is set to a mass constancy of ⁇ 0.01%over 30 minutes.
  • Temperature of the test condition is set at 35 ⁇ 0.1°C.
  • the delta mass (dm) in %at each RH% which is an indicator of the percentage of water absorbed by the sample detergent granule at the respective RH%, is calculated by the equation below:
  • FIG. 1 is a dynamic vapor absorption graph plotting the delta mass (dm in %) of the inventive detergent granule as well as that of the comparative detergent granule across a RH range RH of from about 40%to about 80%. It is evident that the inventive detergent granule absorbs less water than the comparative detergent granule across at relatively high humidity conditions (e.g., with RH ranging from about 40%to about 80%) . Therefore, the inventive detergent granule is less likely to cake or clump when stored or shipped in countries or regions where humidity may present a challenge.
  • Example 2 Comparative Test Showing Reduced Caking of Inventive Detergent Granules in Big Bag Test
  • sample detergent granules with the following compositional makeups are made, which include four (4) inventive samples of detergent granules A-E within the scope of the present invention and one (1) comparative sample of detergent granule C1 outside the scope of the present invention:
  • Each sample detergent granule is formed by the same method described in Example 1.
  • Big bag test is used to probe and qualitatively evaluate potential issues with a material prior to shipping such material in a big bag, during which it may be exposed to elevated temperatures.
  • 100g+/-1g of a test material is first place into a plastic beaker and ensure that the top surface of the test material is level.
  • a second beaker is placed into the first beaker containing the test material, while the bottom of the top, second beaker rests upon the test material, without pushing or forcing the top, second beaker into the test material.
  • the two beakers are sealed together with a PVC tape.
  • a 3Kg mass is placed into the top, second beaker so that the top, second beaker acts as a load-bearing surface for the 3Kg mass upon the test material.
  • the beakers with the test material and the 3Kg mass are then placed in an oven at 35°C and 80%RH. After 20 hours under such test conditions, the 3kg mass is removed, and the test material is cooled down to ambient temperature (with a minimum cooling time of 1 hour) .
  • the bottom, first beaker containing the cooled test material is inverted to observe how easy/difficult the test material can flow out of the bottom, first beaker.
  • the flowability of the test material is graded using the following grading scales:
  • ⁇ 8 Caked, but breaks up with gentle shaking.

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Wood Science & Technology (AREA)
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Abstract

L'invention concerne un granulé détergent caractérisé par une taille moyenne de particule allant de 200 µm à 1 000 µm et un rapport de forme ne dépassant pas 2, et contenant de 85 % en poids à 95 % en poids d'un sulfate d'alkyle (AS) comprenant un groupe alkyle en C6-C16 non alcoxylé ramifié ou linéaire et de 4 % en poids à 14 % en poids d'un sel soluble dans l'eau, avec une teneur en eau ou en humidité comprise entre 1 % en poids et 5 % en poids.
PCT/CN2018/086291 2018-05-10 2018-05-10 Granulé détergent WO2019213890A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP18917802.3A EP3790950B1 (fr) 2018-05-10 2018-05-10 Granulé détergent
PCT/CN2018/086291 WO2019213890A1 (fr) 2018-05-10 2018-05-10 Granulé détergent
CN201880092648.2A CN112041417B (zh) 2018-05-10 2018-05-10 洗涤剂颗粒
MX2020011976A MX2020011976A (es) 2018-05-10 2018-05-10 Granulo de detergente.

Applications Claiming Priority (1)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022047604A1 (fr) * 2020-09-01 2022-03-10 The Procter & Gamble Company Granule de détergent
WO2024092723A1 (fr) * 2022-11-04 2024-05-10 The Procter & Gamble Company Procédé de préparation de granulés de détergent

Citations (8)

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Publication number Priority date Publication date Assignee Title
WO1993018123A1 (fr) * 1992-03-10 1993-09-16 The Procter & Gamble Company Pates detergentes tres actives
US6015784A (en) * 1996-03-08 2000-01-18 The Procter & Gamble Company Secondary alkyl sulfate particles with improved solubility by compaction/coating process
US20040058843A1 (en) * 2002-09-19 2004-03-25 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Detergent compositions
WO2009050026A2 (fr) * 2007-10-17 2009-04-23 Unilever Nv Compositions de blanchisserie
WO2013054624A1 (fr) * 2011-10-14 2013-04-18 花王株式会社 Composition détergente en poudre pour des vêtements et son procédé de fabrication
WO2014198128A1 (fr) * 2013-06-13 2014-12-18 The Procter & Gamble Company Detergent a lessive granulaire
WO2016015326A1 (fr) * 2014-08-01 2016-02-04 The Procter & Gamble Company Compositions de nettoyage contenant des acides gras à des niveaux élevés
WO2018014281A1 (fr) * 2016-07-21 2018-01-25 The Procter & Gamble Company Compositions de nettoyage contenant un azurant à base de diaminostilbène

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Publication number Priority date Publication date Assignee Title
GB9417356D0 (en) 1994-08-26 1994-10-19 Unilever Plc Detergent particles and process for their production
CN1384871A (zh) * 1999-06-21 2002-12-11 宝洁公司 涂敷的洗涤剂颗粒的制备方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1993018123A1 (fr) * 1992-03-10 1993-09-16 The Procter & Gamble Company Pates detergentes tres actives
US6015784A (en) * 1996-03-08 2000-01-18 The Procter & Gamble Company Secondary alkyl sulfate particles with improved solubility by compaction/coating process
US20040058843A1 (en) * 2002-09-19 2004-03-25 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Detergent compositions
WO2009050026A2 (fr) * 2007-10-17 2009-04-23 Unilever Nv Compositions de blanchisserie
WO2013054624A1 (fr) * 2011-10-14 2013-04-18 花王株式会社 Composition détergente en poudre pour des vêtements et son procédé de fabrication
WO2014198128A1 (fr) * 2013-06-13 2014-12-18 The Procter & Gamble Company Detergent a lessive granulaire
WO2016015326A1 (fr) * 2014-08-01 2016-02-04 The Procter & Gamble Company Compositions de nettoyage contenant des acides gras à des niveaux élevés
WO2018014281A1 (fr) * 2016-07-21 2018-01-25 The Procter & Gamble Company Compositions de nettoyage contenant un azurant à base de diaminostilbène

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022047604A1 (fr) * 2020-09-01 2022-03-10 The Procter & Gamble Company Granule de détergent
GB2612482A (en) * 2020-09-01 2023-05-03 Procter & Gamble Detergent granule
WO2024092723A1 (fr) * 2022-11-04 2024-05-10 The Procter & Gamble Company Procédé de préparation de granulés de détergent

Also Published As

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CN112041417B (zh) 2022-07-29
CN112041417A (zh) 2020-12-04
EP3790950B1 (fr) 2023-11-01
EP3790950A1 (fr) 2021-03-17
MX2020011976A (es) 2021-01-15

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