US3887614A - Detergent composed of hollow spherical pellets, and process for manufacturing the same - Google Patents

Detergent composed of hollow spherical pellets, and process for manufacturing the same Download PDF

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Publication number
US3887614A
US3887614A US371987A US37198773A US3887614A US 3887614 A US3887614 A US 3887614A US 371987 A US371987 A US 371987A US 37198773 A US37198773 A US 37198773A US 3887614 A US3887614 A US 3887614A
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United States
Prior art keywords
pellets
percent
weight
detergent
sodium silicate
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Expired - Lifetime
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US371987A
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English (en)
Inventor
Rinnosuke Susuki
Hiroshi Hoshi
Minoru Yoshida
Toshisaburo Toyoda
Masayoshi Nakamura
Susumu Ando
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Lion Fat and Oil Co Ltd
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Lion Fat and Oil Co Ltd
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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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/04—Filters with filtering elements which move during the filtering operation with filtering bands or the like supported on cylinders which are impervious for filtering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/44—Regenerating the filter material in the filter
    • B01D33/46—Regenerating the filter material in the filter by scrapers, brushes nozzles or the like acting on the cake-side of the filtering element
    • B01D33/463—Regenerating the filter material in the filter by scrapers, brushes nozzles or the like acting on the cake-side of the filtering element nozzles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/58—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element
    • B01D33/62—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying
    • B01D33/64—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying by compression
    • B01D33/642—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying by compression by pressure belts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/70—Filters with filtering elements which move during the filtering operation having feed or discharge devices
    • B01D33/72—Filters with filtering elements which move during the filtering operation having feed or discharge devices for feeding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
    • 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

Definitions

  • This invention relates to detergents composed of hollow spherical pellets, and particularly to synthetic detergents consisting of hollow spherical pellets which comprise a matrix of sodium silicate. surface active agent(s), and water. and dispersoid material(s) such as Glaubers salt, sodium tripolyphosphate or other inorganic materials evenly distributed throughout said matrix in a suspended state, and to a process for manufacturing said detergents.
  • the conventional detergents due to their granular shapes, were apt to agglomerate upon being thrown into water, and were not so easily dissolved in water. In addition, they had so high moisture permiability as to coagulate at a high temperature and humidity.
  • the conventionally prevailing method comprised a spray-drying process of forming synthetic detergents which consisted of steps by spraydrying in a hot air stream heated by combustion a slurry of a detergent composition containing a surface active agent such as sulfate esters of a higher alcohol or alkylbenzenesulfonates, builders such as sodium phosphate, sodium carbonate. and sodium sulfate and/or other additives, and 40 60 percent by weight of water.
  • a surface active agent such as sulfate esters of a higher alcohol or alkylbenzenesulfonates
  • builders such as sodium phosphate, sodium carbonate. and sodium sulfate and/or other additives
  • Another disadvantage is that the proportion of sodium silicate to be incorporated in the slurry is required to be limited despite the fact that sodium silicate is useful for decreasing the production cost as well as increasing the detergency; when the slurry is spray-dried, the sodium silicate contained in the slurry reacts with CO in the combustion gas, thereby producing waterinsoluble silicate which makes washing water muddy.
  • This invention aims to provide a new type of detergents which are composed of hollow spherical pellets instead of granules, and therefore are free from the above-mentioned disadvantages possessed by the conventional type of detergents.
  • Another object of this invention is to provide detergents composed of hollow spherical pellets which are uniform in diameter, high in mechanical strength as well as in modulus of elasticity so that they can have high measurability but show little subsidence or reduction in apparent volume during storage or transit.
  • a further object of this invention is to provide detergents composed of hollow spherical pellets which are low in apparent specific gravity, and high watersolubility so that they disperse immediately upon being thrown in washing water without floating over the water surface in an agglomerated state for a long time.
  • Still another object of this invention is to provide detergents composed of hollow spherical pellets which exhibit moderate congeability even at a high temperature and humidity, and accordingly has little viscosity and high fluidity.
  • the above-mentioned objects are obtained by mixing and kneading at a temperature of between 40 C a detergent composition essentially consisting of a matrix of sodium silicate, surface active agent(s), and water, and dispersoid materials such as inorganic builders of known types, into a plastic mass, and then pelletizing said mass by mechanical means, followed by thermally foaming the pellets thus obtained at a temperature of between 300C in a drying device.
  • the matrix serves as a dispersion medium, while the dispersoid materials as inorganic substances being suspended in said matrix and adapted for use as builders in the detergent composition.
  • the compounding ratio of the individual ingredients which constitute the matrix of the plastic detergent composition is as follows: 30 50 percent by weight of sodium silicate, l5 30 percent by weight of surface active agent(s and 30 50 percent by weight of water.
  • the plastic detergent composition is obtained by mixing 40 75 percent by weight of said matrix incorporated with 60 25 percent by weight of said dispersoid materials.
  • metalsilicate is useful, and more specifically such metalsilicate is preferable as contains a metal oxide consisting of alkali metals like sodium or potasium, Particularly out of these alkali metals, sodium oxides are most preferable from the viewpoint of the quality of the final products and for economical advantage. Further, in this case, the most preferable ratio of Na O to SiO in sodium silicate should be 1 2.1 3.1.
  • the surface active agents in this invention can be organic ester sulfonate of higher alcohols such as coconut oil reduction alcohol or sperm oil. or various organic sulfonate such as alkyl aryl sulfonate (those of which the alkyl group has 8 l6 molecules of carbon), alkane sulfonate (those of which the alkane group has 8 24 molecules of carbon), or alkene sulfonate (those of which the alkene group has 8 24 molecules of carbon).
  • organic sulfonate such as alkyl aryl sulfonate (those of which the alkyl group has 8 l6 molecules of carbon), alkane sulfonate (those of which the alkane group has 8 24 molecules of carbon), or alkene sulfonate (those of which the alkene group has 8 24 molecules of carbon).
  • the above-mentioned dispersoid materials may be inorganic builders such as sodium tripolyphosphate, sodium sulfate, or sodium carbonate.
  • foaming agent(s) may be added.
  • the foaming agents available are generally toluenesulfonylhydrazide, azocarbonyl acid amide and other nitrogen supplying foaming agents and are most effective when used in the range between 0.1 and percent. Further.
  • various additives can be added to the above detergent composition such as bactericide, fungicide, anti-discolouring agent, dye, optical bleaching agent, perfume, lathering agent (ethanolamine), anti-dirt absorption agent (carboxymethylcellulose, polyvinyl alcohol, etc.), lather restrainer, skin protection agent,
  • the above-described plastic detergent composition is useful for producing damp pellets of any size ranging between 0.6 and 3.0 mm diameter when the detergent composition is mixed in a Henschel mixer which is provided with a jacket type cooling tower or other appropriate cooling device on the outer part thereof, and is thrown into a pelletizing device. Then, a pelletized detergent of hollow spherical pellets is obtained by thermally drying said damp pellets with the appropriate thermal drying device available.
  • FIG. 1 shows illustratively an example of the apparatus for producing the detergent consisting of hollow spherical pellets.
  • FIG. 2 shows an example of the drying device for continuously drying the damp pellets of the detergent.
  • FIG. 3 shows a cross sectional view taken along the line 20 20 in the drying device of FIG. 2,
  • FIG. 4 shows a plan view viewed from the arrow B in FIG. 3, and
  • FIG. 5 shows a pellet of the detergent according to the invention, partly broken away.
  • FIG. 1 shows diagrammatically an example of the apparatus for producing the detergent of hollow spherical pellets from the slurry.
  • the steps for obtaining a damp pelletized detergent from the slurry are as follows:
  • Numeral l designates a measuring means for measuring the volumes of sodium silicate, surface active agent(s), water, and inorganic builders, etc. being components for the plastic detergent composition, and the delivering these components into a mixer 2.
  • a detergent composition comprising 40 75 percent by weight of the matrix ingredients consisting of sodium silicate, surface active agent(s), and water, and 60 percent by weight of other ingredients consisting of inorganic builders and or additives.
  • said kneaded components are changed into a plastic mass.
  • the temperature in the mixer should be adjusted within the above range since the plastic mass or detergent composition would be liable to be foamed at higher than C while it would easily change into flakes at lower than 40C.
  • the plastic mass is fed into a pelletizer 3 comprising an extruder 4 and a rotary cutter 5.
  • a cutting plate having a plurality of bores arranged over the surface thereof like a honeycomb, through which bores are extruded out the kneaded plastic mass under a pressure ranging between 30 6O kgs/cm and at a temperature of 40 80C. Then, the plastic mass extruded out through the bores is cut by the rotary cutter 5 to a desired length.
  • the cutting plate may be cooled to lower than 40C in order to effectively prevent the pellets from agglomerating into a mass.
  • the pellets thus obtained are moderately congealed, fully plastic, and completely free from agglomerating nor agglutinating with one another.
  • pellets thus formed are thrown into a drying device 6 where they are thermally foamed into hollow spherical shapes respectively as featured by the present invention.
  • the preferred drying device in this invention is shown in FIGS. 2, 3 and 4 andthe entire device is in the form of a hollow pillar-like drying tower which is vertically arranged as shown in FIG. 2.
  • the drying tower comprises an indefinite number of unit drying chambers (in FIG. 2, three chambers 1010, 1020, 1030 supported by a supporting device 80 loaded with a coiledspring) which are interconnected by a flange 40 provided in each unit drying chamber.
  • This drying tower is mounted through a coil-springlike supporting device 80.
  • a vibrator 60 designed to rotate an eccentric weight
  • a blast pipe is connectedly provided through a valve V
  • a blast pipe is provided through a valve V
  • a blast pipe is connected through a valve V
  • a blast pipe is connected through a valve V
  • Drying hot air is carried to the blast pipes from the direction of the Arrow A.
  • Numeral designates a pressure gauge.
  • the interior of the drying tower is shown in crosssection in FIG. 3.
  • sieves having a number of small holes are mounted through hinges on the interior of the drying tower, being inclined downward respectively and arranged alternately on the opposite inner walls of the drying tower in a descending manner.
  • This incline is designed to be moved wholly by the rod (not shown) connected to each sieve and to be adjusted freely. In the examples to be described hereafter. it is preferable to adjust the area ratio of holes 140 in the sieve 130 within the range of 10 to 50 percent and adjust the incline angle within the range of 10 to 40.
  • Numeral 30 shows a hopper which is the in-feed station for the pellets, numeral 70 the out-feed station and numeral 50 a window for observation provided in each unit drying chamber.
  • pellets to be dried is continuously supplied from the infeed station 30.
  • the pellets move downward with their own gravity, while rolling on the sieves 130.
  • the vibration actuated by the vibrator 60 is effective in causing a movement of the rolling. While the pellets are rolling and moving downward, each pellet becomes round, less angular and uniform in grain size. 1
  • the hot blast for drying is usually employed at a temperature of 150 and 400C, being supplied from the direction of the arrow A.
  • the valve V opens, while the valves V and V close, the hot air streams from upward to downward in the same direction as the downward movement of the objects to be driedQ
  • the valve V opens, while the valves V V close, the hot air streams in an opposite direction to the downward movement of these objects to be dried.
  • the intermediate valve V opens while either valve V or V;, closes, the hot air is a combination of these two procedures.
  • the different methods of effectuating blasts of the hot air are characterized by the fact that the same direction stream dries the pellets quickly, thereby obtaining pelletized detergents with a smaller apparent specific gravity, a thinner film surface and an excellent water-solubility.
  • the opposing direction stream dries the pellets slowly, thereby obtaining pelletized detergents with a smoother surface and a larger apparent specific density.
  • the combination type of stream obtains a desired apparent specific gravity and allows free control of the drying speed of the pellets.
  • the process and apparatus in accordance with this invention easily allows the sieves to be adjusted in an incline angle thereof and can easily change the number of connecting unit drying chambers thereby adjusting the hours of retention of the pellets in the drying tower.
  • the best drying may be selected according to the starting water content in the pellets.
  • a further advantage is that the drying state of the pellets can be conveniently observed through the observation window 50, thereby easily meeting any unexpected situation.
  • the matrix of this invention which contains sodium silicate, surface active agent(s), and water, due to its air-impermeability, is gradually foamed in the drying device by evaporation of water contained therein, so that the pellets soften to become spherical. As they are further foamed, the individual gassed cells in each pellet get larger so that they cojoin one another to form a single large cell. Simultaneously, the pellets are dried faster towards the outer portions thereof to become hollow spherical pellets which compose the detergent of this invention as shown in FIG. 5.
  • the size of the pellets according to this invention can be freely selected within the range betweenl and 5mm, and the most preferable size is 1.5 2.5mm which is appropriate for practical use. Particularly, those pellets obtained by extruding througha single cutting plate are extremely uniform in diameter.
  • the thickness of the shells of the individual pellets ranges between 2 50 percent of the radius of the pellets. of which the most preferable percentage is l0 30 percent.
  • the hollow pellets have a rather small specific gravity ranging between 0.1 0.4, preferably between 0.15 0.3.
  • the pellets of this invention are incorporated with a larger proportion of sodium silicate towards the outer portions of the shells thereof while a larger proportion of surface active agents towards the inner portions thereof, so that they can have a high modulus of elasticity; their restitution coefficient ranges between 0.1 0.6.
  • a" test on the breaking load value of the pellets found that they could have a mechanical strength of 5 200gr. per piece, which value is most desirable for the handling purpose.
  • another test was made on the powdering property of the pellets which comprised steps of bottling them, and then vertically vibrating the bottle for 30 minutes at 300 reciprocations per minute and with a stroke of mm, with the result that just few pellets got powdered.
  • the uniformity in diameter of the individual pellets brings about further advantages such as almost little subsidence or reduction in apparent volume of the pellets in reduction high measurability, and excellent flow characteristics due to their small viscosity (A test has shown that they have an angle of repose between 3 20).
  • Such pelletized detergent according to this invention once thrown in water, will exhibit much higher watersolubility, smaller specific gravity compared with conventional granular detergents, as well as uniform thickness of the pellet shells. Further, the characteristics of the detergent exhibits a high temporary dispersibility (i.e. the extent of water-solution of the detergent floating over the water-surface without being agitated.) completely prevents the detergent from floating in lumps over the surface of water for a long time after being thrown in water or agglomerating to be precipitated downto the washer bottom. Still further, the use of not only sodium silicate but also Glaubers salt. sodium tripolyphosphate, and the like contained in the detergent as detergent builders enables the detergent to have detergency substantially equivalent to the conventional detergents.
  • the detergent of this invention has a fine appearance, and also that it will not irritate the users eyes or nose.
  • the above ingredients were evenly mixed and kneaded at 80C to form a plastic mass which in turn was thrown into the pelletizer to be extruded out through the bores of the cutting plate (the bore diameter 1.8mm) under an extruding pressure of SOkg/cm", followed by cutting the extruded slurry with the rotary cutter, thus to obtain pellets each with a diameter of 2.0mm.
  • the pellets thus obtained were thrown into the drying device to be subjected, for one minute, to counter air current flowing in said device and having a temperature of 350C to be foamed and dried.
  • Pellet size 3 3.5mm Thickness of Shell (Average) 0.7mm Mechanical Strength of Pellet (Average) 60gr/pce.
  • Acid Water 30.0 16.0 36.0 28.8 25.2 21.6 Inorganic Builders 25.0 60.0 28.0 28.0 28.0
  • Example Example Example Condition 1 1 1 1 1 1 1 1 1 1 Moisture Contents 9 5 1 1 8 7 7 Pellet Size(mm) 3-3.5 33.5 33.5 33.5 33.5 33.5 33.5 Thickness of 0.7 0.9 0.6 0.7 0.8 0.8 Shell(mm) Apparent Speci- Shapes fic Gravity 0.27 0.33 0.25 0.28 0.29 0.30 and Proper- Restitution ties Coefficient 0.5 0.4 0.3 (1.5 0.6 0.6
  • EXAMPLE 8 In this example. was followed the same process under the same operating condition as in Example 1 except that here Sodium silicate consisting of Na- O and SiO in the mol ratio of l to 2.5. and Olefin Sulfonic Acid having 15 l8 carbon atoms were used in place of Sodium silicate having a l to 2.1 mol proportion of Na O to SiO and Sodium Dodecylbenzene Sulfonic Acid. respectively, thus to obtain products substantially equivalent to those obtained in Example 1.
  • EXAMPLE 9 In this example, was followed the same process under the same operating condition as in Example 1 except that Sodium silicate consisting of M1 and SiO in the mol ratio of l to 3.0 was used instead of that in Example 1, thus to obtain products substantially equivalent to those obtained in Example 8.
  • EXAMPLE 10 In this example, was followed the same process under the same operating condition as in Example 1 except that here Ester of Coconut Reduction Alcohol Sulfonate was used in place of Sodium Dodecylbenzen Sulfonic Acid in Example 1. thus to obtain products substantially equivalent to those obtained Example 1.
  • a process for manufacturing a detergent composed of hollow spherical pellets comprising the steps of mixing and kneading a. 40 75 percent by weight of a matrix consisting of 30 50 percent by weight of sodium silicate (Na O SiO l 2.1 3.1), 30 percent by weight of a surface active agent selected from the group of organic sulfate esters and organic sulfonates, and 30 50 percent by weight of water, with b. 60 percent by weight of a dispersoid material consisting substantially of inorganic builders into the form ofa detergent composition having plastic- 10 ity:
  • plastic detergent composition further includes 0.1 5 percent by weight of a nitrogenous foaming agent consisting of either or both of toluensulfonyl hydrazide and azocarbonyl acid amide.
  • the detergent as claimed in claim 4 comprising sodium silicate and a surface active agent, whereby a larger proportion of said sodium silicate and a smaller proportion of said surface active agent are distributed towards the outer portion of the shell of each pellet, while a smaller proportion of said sodium silicate and a larger proportion of said surface active agent are distributed towards the inner portions of the shell of each pellet.

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  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
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US371987A 1969-12-03 1973-06-21 Detergent composed of hollow spherical pellets, and process for manufacturing the same Expired - Lifetime US3887614A (en)

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Cited By (28)

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US4111853A (en) * 1976-03-08 1978-09-05 Stepan Chemical Company Particulate composition of sodium alpha olefin sulfonate and sodium silicate
US4133857A (en) * 1975-09-16 1979-01-09 Chisso Corporation Method for producing a granular sorbic acid
EP0651050A1 (fr) * 1993-11-03 1995-05-03 The Procter & Gamble Company Agglomérat de tensioactifs en forme de particule
EP0663439A1 (fr) * 1994-01-17 1995-07-19 The Procter & Gamble Company Procédé pour la préparation de granules de détergent
USD419262S (en) * 1999-03-12 2000-01-18 Ecolab Inc. Solid block detergent
US6124250A (en) * 1993-12-30 2000-09-26 Ecolab Inc. Method of making highly alkaline solid cleaning compositions
US6150324A (en) * 1997-01-13 2000-11-21 Ecolab, Inc. Alkaline detergent containing mixed organic and inorganic sequestrants resulting in improved soil removal
US6156715A (en) * 1997-01-13 2000-12-05 Ecolab Inc. Stable solid block metal protecting warewashing detergent composition
US6177392B1 (en) 1997-01-13 2001-01-23 Ecolab Inc. Stable solid block detergent composition
WO2001025390A2 (fr) * 1999-10-05 2001-04-12 The Procter & Gamble Company Composants alveolaires et compositions contenant lesdits composants
WO2001024990A1 (fr) * 1999-10-05 2001-04-12 The Procter & Gamble Company Procede de preparation de constituant de mousse
US6258765B1 (en) 1997-01-13 2001-07-10 Ecolab Inc. Binding agent for solid block functional material
US6376453B1 (en) * 1997-12-10 2002-04-23 Kao Corporation Detergent particles
US6632291B2 (en) 2001-03-23 2003-10-14 Ecolab Inc. Methods and compositions for cleaning, rinsing, and antimicrobial treatment of medical equipment
US6638902B2 (en) 2001-02-01 2003-10-28 Ecolab Inc. Stable solid enzyme compositions and methods employing them
US6645931B1 (en) * 1999-06-15 2003-11-11 Kao Corporation Solid-shaped detergent
US6706773B1 (en) 1999-10-05 2004-03-16 The Procter & Gamble Company Process for preparing a foam component
US20040259757A1 (en) * 1991-05-14 2004-12-23 Ecolab Inc. Two part chemical concentrate
US6943200B1 (en) 1999-10-05 2005-09-13 Procter & Gamble Company Water unstable foam compositions
US20130196892A1 (en) * 2010-10-14 2013-08-01 Judith Maria Bonsall Packaged particulate detergent composition
US20130269119A1 (en) * 2010-10-14 2013-10-17 Judith Maria Bonsall Packaged particulate detergent composition
US9062281B2 (en) 2010-10-14 2015-06-23 Conopco, Inc. Particulate detergent compositions comprising fluorescer
US9273271B2 (en) 2010-10-14 2016-03-01 Conopco Inc. Laundry detergent particles
US9284517B2 (en) 2010-10-14 2016-03-15 Conopco Inc. Laundry detergent particle
US9290723B2 (en) 2010-10-14 2016-03-22 Conopco Inc. Laundry detergent particles
US9290725B2 (en) 2010-10-14 2016-03-22 Conopco Inc. Laundry detergent particles
US9290724B2 (en) 2010-10-14 2016-03-22 Conopco, Inc. Laundry detergent particles
US9365811B2 (en) 2010-10-14 2016-06-14 Conopco Inc. Manufacture of coated particulate detergents

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US6835706B2 (en) 1997-01-13 2004-12-28 Ecolab Inc. Alkaline detergent containing mixed organic and inorganic sequestrants resulting in improved soil removal
US6831054B2 (en) 1997-01-13 2004-12-14 Ecolab Inc. Stable solid block detergent composition
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WO2001024990A1 (fr) * 1999-10-05 2001-04-12 The Procter & Gamble Company Procede de preparation de constituant de mousse
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WO2001025390A3 (fr) * 1999-10-05 2001-09-27 Procter & Gamble Composants alveolaires et compositions contenant lesdits composants
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